Anal. Chem. 1987, 59, 212R-252R (330) Roeder, P. L. Can. Mineral. W85, 2 3 , 263-271. (331) Severin, V. V. Zap. Vses. Mlneral. 0 - v a . 1984, 113, 98-105; CA 100(18)142416x. (332) Bastin, G. F.; Heijligers, H. J. M. Microbeam Anal. 1985, 1-6. (333) Patel, M. X-Ray Spectrom. 1985, 14, 20-22. (334) Velde, B. Clay Miner. 1984, 19, 243-247. (335) Armstrong, J. T. Microbeam Anal. 1984, 208-212. (336) Cliff; Larimer Proceedings of the 5th European Congress on Electron Microscopy, Institute of Physics, London 1972, 140-141. (337) Mellini, M.; Menichini, R. Rend. SOC.Ital. Mineral. Petrol. 1985, 40, 26 1-266. (338) Musashino, M. Bull. Kyoto Univ. Educ., Ser. B 1986, 68. 29-44. (339) Heinrich, K. F. J. Microbeam Anal. 1985, 79-81. (340) Markowicz, A.; Storms, H.; Van Grieken R. X-Ray Spectrom. 1986, 15. 115-119. (341) Heinrich, K. F. J. Microbeam Anal. 1986, 279-280. (342) Love, G.; Scott, V. D.; Sewell, D. A. Microbeam Anal. 1985, 82-84. (343) Schowengerdt, F. D.; Spottiswood, D. J.; Sen, R.; Yarar, B. Congr. Int. Mlneralurgie, 15th 1985, 1 , 49-56. (344) Mucci, A.: Morse, J. W. Am. J. Sci. 1985, 285, 306-317. (345) Hochella, M. F., Jr.; Harris, D. W.; Turner, A. M. Am. Mineral. 1988, 7 1 , 1247-1257. (346) Hofmann, S.; Frech, R. Anal. Chem. 1985, 5 7 , 716-719. (347) Doern, F. E.; Kover, L.; Mclntyre, N. S. S I A . Surf. Interface Anal. 1984, 6 , 282-285; CA 102:71982g. (348) Sfar, M.; Lacharme, J. P.; Lepeut. P.; Champion, P. J. Phys. Colloq. 1984, 375-378; CA 100(26)214351~. (349) Southon, M. J.; Harris, A.; Kohler, V.; Mullock, S. J.; Wallach. E. R. Microbeam Anal. 1985, 310-314. (350) Dennemont, J.; Landry, J. C. Microbeam Anal. 1985, 20th, 305-309. (351) Adams, F. C.; Akyuz, S.;Akyuz, T.; DeWaele, J. K. Hacettepe Bull. Nat. Sci. Eng. 1984, 13, 19-27; CA 102(4)38904k. (352) Sutter, J. F.; Hartung. J. B. Scanning Electron Microsc. 1984, 1525.-. 1529. .-. (353) Akyuz, S.; Waele, J. K.; Akyuz. T.; Adams, F. C.J. Inclusion Phenom. 1985. 3. 125-133. (354) ~M'usseiman,I:H.: Linton. R. W.; and Simons, D. S. Microbeam Anal. 1985, 337-341. (355) Marien, J.: DePauw, E. Anal. Chem. 1985, 5 7 , 361-362. (356) Jones, A. P.; Smith, J. V. Neues Jahrb. Mineral 1984, 5 , 228-240. (357) Reed, S. J. B. Mineral. Mag. 1986, 3-15. (358) Zinner, E.; Crozaz, G. Springer Ser. Chem. Phys., Second. Ion Mass Spectrom. 1986, 44, 444-446. (359) MacRae, N. D.; Metson, J. B. Chem. Geol. 1985, 53(3-4), 325-333. (360) Nesbitt, H. W.; Metson, J. B.; Bancroft, G. M. Chem. Geol. 1986, 55, 139-160. (361) Hoklaway, M. J.; Dutrow, B. L.; Borthwlck, J.; Shore, P.; Harmon, R. S.; Hinton, R. W. Am. Mineral. 1986, 7 1 , 1135-1141. (362) Steele, I.M. Neues Jahrb. Mineral. 1988, 5 , 193-202. (363) Summers, W. R.; Schweikert, E. A. Anal. Chem. 1988, 5 8 , 2 126-2 129. (364) Stevens, J. G.; Bowen, L. H.; Whatley, K. M. Anal. Chem. 1986, 5 8 , 250R-264R.
(365) Mysen, 8. 0.; Carmichael, I. S. E.; Virgo, D. Contrib. Mineral. Petro. 1985, 90, 101-106. (366) Vandenbergerghe, R. E.; De Grave, E.; De Geyter, G.; Landuydt, C. Clays Clay Minerals 1988, 34 275-280. (367) Dubrawski, J. V.; Warne, S . St. J. Thermochim. Acta 1988, 107, 51-59. (366) Sommer, M. A., 11; Yonover. R. N.; Bourcier, W. L.; Gibson, E. K. Anal. Chem. 1985, 5 7 , 449-453. (369) Wopenka, 8.; Pasteris, J. D. Appl. Spectrosc. 1986, 40, 144-151. (370) Haskell, R. J.; Wright, J. C. Anal. Chem. 1985, 5 7 , 332-336. (371) Baltrus, J. P.; Makovsky, L. E.; Stencel, J. M.; Hercules, D. M. Anal. Chem. 1985, 5 7 , 2500-2503. (372) Rucklidge, J. C.; Wilson, G. C.; Kiiius, L. R.; Litherland, A. E. Springer Ser. Chem. Phys. 1985, 44, 451-454. (373) Ingamelis, C. L.; Pitard, F. F. Applied Geochemical Analysis; Wiley: New York, 1986; 733 pp. (374) Wiilis, J. P. Colloquium Spectroscopicuum International XXIV; from Fresenius' Z . Anal. Chem. 1986, 324, 485-494. (375) Xie, X.; Yan, M.; Li, L.; Shen, H. Geostd. Newsi. 1985, 9 , 63-159. (376) Xie, X.; Yan, M.; Li, L.; Shen, H., Geostd. Newsl. 1985, 9 , 277-280. (377) Hansen, R. G., MINTEK Rept M190, 1965. (378) Scheutzhow, R.; Kuhn, G. Z . Angew. Geol. W85, 31, 305-307. (379) Burke, K. E. Geostd. Newsl. 1985, 9 , 69-78. (380) Steger, H. F.; Bowman, W. S.,CANMET ReDt 84-IE, 1985, 33 DD; CA 103(22j188599z. (381) Lister, B.; Cogger, N. Geostd. Newsl. 1986, 10, 33-59 (382) Flanagan, F. J. Geostd. Newsl. 1988, 10, 111-120. (383) Schwarz, L. J.; Dorrzapf, A. F., Jr.; Crandeil, W. G.; Flanagan, F. J. Geostd. Newsl. 1986, 10, 99-107. (384) Aly, M. M. Spectrochim. Acta 1986, 418, 837-845. (385) Govindaraju, K. Geostd. Newsi. 1884, 8 , 173-206. (386) Gladney, E. S.;Burns, C. E.; Roelandts, I.Geostd. Newsl. 1984, 8 , 119-154. (387) Gladney, E. S.;Burns, C. E.; Roelandts, I. Geostd. Newsl. W65, 9 , 35-68. (388) Abbey, S.; Gladney, E. S . Geostd. Newsl. 1986, 10, 3-11. (389) Lister, B. Geostd. Newsl. 1984, 8 , 171-172. (390) Lister, B. GeosM. Newsl. 1985, 9 , 263-273. (391) Lister, B. Geostd. Newsl. 19868 IO, 177-181. (392) Abbey, S.; Rousseau, R. M. Geosfd.Newsl. 1985, 9 , 1-16. (393) Colombo, A. Geostd. Newsi. 1986, 10, 61-86. (394) Colombo, A. Geostd. Newsl. 1988, 10, 163-189. (395) Dempir, J. Geostd. Newsl. 1988, 10, 87-91. (396) Abbey, S. Geostd. Newsl. 1988, 10, 159-168. (397) Filby, R. H.; Nguyen, S.;Grimm, C. A.; Markowski, G. R.; Ekambaram, V.; Tanaka, T.; Grossman, L. Anal. Chem. 1985, 5 7 , 551-555. (398) Scheutzhow, R. Z . Angew. Geol. 1985, 31, 212-214; CA 104(4)22218v. (399) Flanagan, F. J. U S . Geol. Surv. Bull. 1988, No. 1582, 70 pp. (400) Roelandts, I.Geostd. Newsl. 1984, 8 , 207-218. (401) Roelandts, I.Geostd. Newsi. 1985, 9 , 281-294. (402) Roelandts, I.Geostd. Newsi. 1986, 10, 265-281. I
Food Anthony F. Gross,* Peter S . Given, Jr., and Albert K. Athnasios Nabisco Brands, Inc., Corporate Technology, Box 1943, East Hanouer, New Jersey 07936-1943
This review covers the literature for approximately the period from October 1984 to October 1986. This is the first review by the present authors and we continue to use the basic format of the authors of the last review (23P),as well as the practice of citing domestic and more widely circulated foreign journals over the less accessible ones. This is a critical review and not an attempt to provide an all-inclusive bibliography. The chemical abstract reference is now included in most of the literature cited.
ADDITIVES Review articles pertaining to additives consist of the following: Arneth and Witzgall (3A) compiled thin-layer chromatography (TLC) methods for the analysis of all commonly used meat additivies; the chemistry and analysis of sulfite and sulfur dioxide in foods was reviewed by Barnett (4A);and Modderman (38A) reviewed the chemistry of sulfite, its reaction with food components and problems encountered during measurement. 212R
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Sulfite was oxidized to sulfate with sulfite oxidase producing peroxide which was then reduced by NADH in the presence of NADH peroxidase by Beutler (6A)with subsequent spectrophotometric measurement of NADH consumption. Residual sulfite in shrimp was determined by Cooper et al. (12A) using ion chromatography; result was 97% of AOAC Monier-Williams method finding. Damiani and Burini (14A) detected nitrite in milk by reaction with 2,3-diaminonaphthalene to form naphthotriazole which was measured fluorometrically. DeVries et al. (16A) combined selective distillation with selective redox titration to measure sulfite. Eek and Ferrer (18A) determined nitrate and nitrite in water and ham using ion exchange high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection, as did Eggers (19A)for cured meats. Grekas & Calokerinos (23A)described a continuous flow apparatus for the detection of sulfite and sulfur dioxide in beverages and air samples using molecular emission cavity analysis. Holak (27A) developed quantitative methods to extract and differentiate free and combined sulfite and
0 1987 American Chemical Society
FOOD Anlhony F. Oma. DkeCtw -6 Devel opment. Corpora@ Technokqy. NBbisci Bands. IN. (B.S. 1951. Cd@3 01 lha Ch 01 New Y a k ) . supavlsss lha memads de vetopment and problem SOking eff& 0 lha Scientilic Services Department. His work experience includes analysis 01 I d stutts. pesticide residue analysis. instrumen tal analysis, and me development 01 anaiyti CBI meihcds. ~e has served as an ~ S S O C C ate referee lor lha Association 01 Official i' L AnaMimI Chemists. Presentb he serves as 1 an ihustry advisor to U.S: L M & I ~ ~ 01 the c&x AiimntarlUS Camminee 01 ~naly'; $is and Sampling. He is a member of the ,*,: &I Aswcialion of Official Analytical Chemists and a member 01 the American chemical Smiely
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Pder S. Given, Jr.. F'h.D.. is Group L a d e in lha Fundamental Science Department 0 Nabirco Bands, Inc. (B.S. 1975. Syracusi Univershy. m.D. 1981, State Unkershy 0 Naw Y m ) . He io responsible tor fundsmn tal research programs on food ingredient! Which include Interacttons betwean macro molecules and tow moiecuiar weight corn pounds and the physical-chemical behavia 01 lipids. C m m t focus invokes hlgh-resoiu tion NMR appiicBttons. Prior activities WM the company include development 01 analytical methods whh emphasis on HPLC. investigative work on consumer inquiries. and chemmetric approaches to fingerprint analysis and discrimination.
date. Corporate Technology. Nabkc, Brands. Inc.. East HBnover. NJ [BSc (1956). Alexandria Univerrhy. Egypt; M.S (1962). North Carolina State lhkmhy, Ra leigh. NC]. manages the GCIMS and NMI groups 01 liw A n a W i Methods Dewiop &nt Deprtment and directs problem-Joiu ing ellais in nonroutine and crlllcai anab ses. His interests include anaMmi mthc& I devebpment and troubierh&ting and lha separation and elucidation 01 structure 01 chemical consliluenls 01 food and natural products by applying chemical. chromato. gaphic. and Specnometric IeChniqueS. He has sumOred several publications on lha analysis 01 myco1oxins. CBrbohydrates. and lipid9 in foods. on natural Iiavw consttnuents in tobacco. and on the irolatton and structural detminatton of medicinaiiy active chemical consliiwnts from natusi products and developed methW0gies lor intermediate process control and lor the analysis of a wide Spectrum 01 food chemical components including intense sweateners. emu1slfiws. antoxidants. and nace twd COntBminanlS. Organizational aC1ivlllBS include ACS. AOAC. and AOCS Were he is a member of the Mycotoxins and Uniform Msthcds Comminees.
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measured extract concentrations by using differential pulse polarography. The selectivity of malachite green for detecting the presence of sulfite in poultry was reevaluated hy Mallinson et al. (%A); some interferences were found. Extracted nitrate was utilized for quantitative nitration of benzene with subsequent GC-thermal energy analysis by Ross and Hotchkiss (43A). Schwedt and Baeurle (44A) compared photometry with p-rosaniline, HPLC, and enzymatic analyses of sulfite (as sulfur dioxide) in foods; the results varied widely according to food matrices. Schwedt (45A) describes the use of commercial test strips for simultaneous measurement of nitrite, nitrate, sulfur dioxide, ascorbic acid, and potassium. Color intensity was measured by reflectometry. Silva et al. (47A) developed a method for sequential analysis of nitrate and nitrite in a continuous flow/extraction system by formation of an organic copper complex with nitrate and atomic absorption spectrophotometric analysis of the complexed copper. Nitrite either was oxidized to nitrate with Ce(IV) and measured by copper complexation or was reduced to nitrogen with sulfamic acid and passed undetected. Sulfur dioxide was distilled into formaldehyde and then measured by use of ion exchange HPLC with Conductivity detection by Sullivan and Smith (5OA). Sullivan et al. (51A) detected sulfite by flow injection analysis where sulfur dioxide, isolated from the
flowing stream by gas diffusion, decolorizes malachite green. Simultaneous determination of benzoate, sorbate, and four p-hydroxyhenzoic acid esters in meat using reverse-phase HPLC was achieved by Ali (ZA). Similar work was reported by Garcia-Regueiro et al. ( Z A ) . Eichler and Rubach (ZOA) measured sorbate, benzoate, p-hydroxybenzoic acid esters, formate, and propionate in a single step using isotachophoresis. Matsunagi et al. (36A) reported the simultaneous determination of sorbate, benzoate, p-hydroxybenzoic acid esters and saccharine by ion-pair HPLC using hexadecyltrimethylamine. Ion-pair extraction with tri-n-octylamine was used by Puttemans et al. (40A) with reverse-phase HPLC to measure sorbate, benzoate, and saccharin in yogurt. Haddad and Jackson (24A) reported simultaneous determination of ascorbate, bromate, and metabisulfite in bread improver using ion exchange HPLC with both UV and conductivity detection. A similar technique was applied by Yamamoto et al. (54A) to measure potassium bromate in bread. Rao e t al. (41A) determined qunine in soft drinks by spectrophotometry of the complex formed between quinine and alizarin brilliant violet R a t 578 nm. Reijenga et al. (42A) measured quinine using isotachophoresis. Quinine, hydroquinine, saccharin, and sodium benzoate concentrations in soft drinks were measured by Valenti (53A) using direct injection into reverse-phase HPLC with UV detection at 254 nm. Chikamoto and Maitani (IOA) determined ethanol and propionic acid levels in baked products simultaneously by steam distillation followed by GC analysis. Yanai ( M A ) developed a test paper for ethanol by impregnating paper with Monascus red dye which reveals color in the presence of ethanol vapor. Argoudelis (ZA) developed a cation exchange HPLC method for the simultaneous determination of aspartame, caffeine, saccharin, and benzoate in soft drinks. Ammonium phosphate mobile phase and UV detection a t 214 nm were utilized. Aspartame and its degradation products were determined by using gradient elution reverse phase HPLC by Cross and Cunico (13A). A 0-cyclodextrin bonded phase HPLC column was used by Issaq et al. (3OA) to measure aspartame in soft drinks. Aspartame was also measured by TLC and ninhydrin visualization by Sherma et al. (46A). Limacher and Tanner (%A) measured cyclamate using GC separation of the reaction adduct of cyclamate with 20% sulfosalicyylic acid followed by treatment with hydrochloric acid and hydrogen peroxide. Yamauchi et al. (55A) . . constructed an amuerometric enzvme (L-glutamate oxidase) electrode to measure L-glutamic acid. determined the antioxidants, lndyk and Woollard ( 2 9 A ~ BHA, BHT, TBHQ, and tocopherols. in tallow and vegetable oil by normal-phase HPLC with UV detection a t 280 nm. BHA, BHT, and TBHQ in edible oils were measured by Kitada et al. (31A) using reverse-phase HPLC with amperometric detection. A specific spectrophotometric method for BHA was developed by Komaitis and Kapel(3ZA) by reacting BHA with NJV-dimethyl-p-phenylenediamine and measuring at 550 nm. Stoyke et al. (49A) developed an extraction technique and a GC method for ETDQ, the active component in the feed antioxidant XAX-M. A qualitative test for the presence of galactose-containing thickeners in meat was described by Bauer and Stachelberger (5A) where the meat is acid hydrolyzed and the liberated galactose measured enzymatically. Brumley et al. @ A ) discussed the limits and resolution of OH- negative ion chemical ionization mass spectrometry (MS) analysis of polysorbates (polyoxyethylated fatty acid esters of sorbitan). Resolution of fatty acid esters of sucrose on open tubular columns with supercritical carbon dioxide mobile phase was described by Chester et al. (SA). Mitsuhashi e t al. (37A) developed an enzymatic regimen to measure propylene glycol in a variety of foods using glycerol dehydrogenase and glycerol kinase. A GC method for simultaneous quantitative determination of methylated fatty acids and silylated sterols from orange juice was reported by Stack et al. (48A). Simultaneous determination of monensin, narasin, and salinomycin in feeds using reverse-phase HPLC and postcolumn reaction with vanillin was described by Blanchflower et al. (7A). DeVries et al. (15A) developed an automated headspace GC-ECD (electrochemical detection) method for methyl bromide in wheat, flour, cocoa, and peanuts. The fungicides biphenyl, 2-hydroxybiphenyl, and thiabendazole were detected by Gieger (ZZA) in fresh fruits using reversephase HPLC with fluorescence detection. Heikes (%A) imANALYTICAL CHEMISTRY, VOL. 59, NO. 12. JUNE 15, 1987
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proved a 1-h purge and Tenax-TA trap method for ethylene dibromide determination by GC-ECD. A microbiological method for systemic fungicide residue determination was adapted by Kovacs (33A)to incorporate several bacterium and yeast species to measure a variety of fungicides. Duncan et al. ( I 7A) compared HPLC-electrochemical detection with GC-MS-single ion monitoring (SIM) for the assay of salsolinol, dopamine, 3,4-dihydroxyphenylacetic acid, 3,4-dihydroxyphenylethanol, and norepinephrine in foods and beverages, and found GC-MS-SIM far superior. HobsonFrohock (26A)performed tissue residue studies of medicinal additives, amprolium, arprinocid, clopidol, dimetridazole, and sulfaquinoxaline, in broiler chickens and turkeys using GC and HPLC. The determination of tetracyclines and macrolide antibiotics in various meats was carried out by Hoshino et al. (28A) using a cyano column for HPLC analysis. Newsome (39A) developed an enzyme-linked immunoassay for triadimeton in fruits and vegetables and found good agreement with results from an established GC procedure. Cook et al. (11A) determined packaging headspace oxygen, nitrogen, and carbon dioxide distributions by developing a special sampling device, collection of gases in an evacuated sampling valve, and sample injection into a GC fitted with a thermal conductivity detector. Carbonation levels in beverages were measured by Szerenyi and Ringleib (52A)by passing the beverage over one side of a gas-permeable membrane and then measuring the carbon dioxide content in a diluent gas passed over the opposite side of the membrane continuously using either thermal conductivity or infrared.
ADULTERATION, CONTAMINATION, DEC OMPOSIT1ON Gilbert (9OB) published a book on The Analysis of Food
Contaminants, and wrote a review (91B)on the advantages and disadvantages of mass spectrometry in identification of food components. Folkes (79B) wrote a review on the determination of contaminants in food and the impact of developments in instrumental analysis on methodology and limits of determinations. Specific examples of contaminants discussed are As, Pb, Hg, Cd, organochlorine pesticides, polynuclear aromatic hydrocarbons, polychlorinated biphenyls, vinyl chloride monomer, styrene, and nitrosamines. Immunoassay techniques for measuring veterinary drug residues in farm animals, meat, and meat products were reviewed by Heitzman (115B).Horman (120B) published a review on mass spectrometry and food safety and the use of MS to determine natural toxiants and contaminants in foods. Reid published two reviews (ZIOB,211B) on the extraction and cleanup of contaminants and toxicants from food for mass spectrometric analysis. Contribution of Mass Spectrometry to Food Safety was the subject of a review by Stan (244B). Shepherd (288B) reviewed size exclusion and gel chromatography and applications to the cleanup of food samples for contaminant analysis. Adulteration of natural lime oils was detected by Alessandro et al. (3B) by glass capillary GC-MS. Brause et al. (27B) detected adulteration in apple juice and orange juice by a chemical matrix method combining isotope analysis, sugar profiles, UV absorbance, glucose fructose ratio, total sugars/Brix ratio, mineral, and trace e ements, and determination of trace organic compounds of beet sugar and invert sugar by GC/MS was used to detect adulteration of orange juice especially with water and pulp wash. Adulteration of apple juice can be determined by sugar profile, 13Cratio, chlorogenic acid, malic acid, proline, and sorbitol content. Bricout et al. (29B) used the isotopic ratios 13C/12Cad 2H/1H for detecting the addition of cane and beet sugars and high fructose corn syrup to orange juice in an effort to control its authenticity. Cohen et al. (46B) collected data on the composition of Israeli orange juice, grapefruit juice, orange peel, and grapefruit peel. Significant differences were found between the juice and peel in the content of isocitric acid, total flavonoids, chlorides, phosphates, chloramine T, and arginine. Significance of these findings in detecting juice adulteration with peel extract solids was discussed. Doner (66B) reported on carbon isotope ratios in natural and synthetic citric acid as indicators of lemon juice adulteration. Fang et al. (76B) reported the use of HPLC and ion chromatography for the analysis of citrus fruit juice and passion fruit juice of Taiwan for free amino acids. Fruit juice authenticity was inspected by amino acid distribution patterns.
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Galensa et al. (84B)used HPLC for detecting grape juice addition to orange juice by separating and determining naringin hydrolysis products. Adulteration in commercial cranberry juice drinks and concentrates was detected by Hong et al. (118B)by HPLC analyses for nonvolatile acids and anthocyanidine profiles. W-visible spectral measurements were used to measure pigment concentration, polymeric color, and percent polymeric color. Adulterated samples were detected by havin nonvolatile organic acid profile indicative of added malic and/or citric acid. Substantial levels of delphinidin and malvidin, neither of which are present in cranberries in significant amounts, were indicative that grape skin extract was the added colorant. Kauschus et al. (136B)found that analysis of the sugar components of water-soluble polysaccharides in orange juice by CGC showed the arabinose/galactose ratio to be remarkably constant, This value (0.50-0.53) offers an additional criterion for evaluating the authentic composition of orange juice. Siewek (235B)reported that adulteration of black currant juice by red currant juice may be detected by the fact that the red juice contains a flavonol glycoside that is absent in the black juice. HPLC, NMR, and spectrometric methods were used to characterize the structure of the compound. Siewek et al. (236B)detected the adulteration of grape juice and of alcoholic bever es from grape juice with fig juice by determining of flavone2-glycosides which do not occur in grapes using HPLC. An addition of 5% fig juice can be detected with certainty. Wald e t al. (283B) detected adulteration of black currant products with blackberry juice by determination of flavonoids by HPLC. Wallrauch (284B) wrote a review with 10 references on the use of amino acid content of fruit juices to detect adulteration by other juices, to detect dilution with water or other fluids, and to identify fruit varieties used for juice manufacturing. The variability of proline content in a number of juices was tabulated. Wrolstad (295B) analyzed apple juice samples from several countries for sugar and nonvolatile acid content and discussed the use of the results to detect adulteration of the juice. Stable C isotopes were also determined and recommendations were made for improving the analytical methods and broading the analysis data in the detection of juice adulteration. Zyren et al. (307B) reported on the interlaboratory variability of methods used for detection of economic adulteration of apple juice. The most important test for determining adulteration was the total malic acid/L-malic acid ratio. Fumaric acid, a minor contaminant in synthetically produced malic acid, shows promise as an indictor of economic adulteration. Volonterio et al. ( B I B )reported a sensitive method for determining nonbiogenic acetic acid in fermentation vinegar by radiochemical 14Ccounting. Frangipane et al. (82%) detected by GC isoglucose-adulterated honey by determining the isomaltose/maltose ratio. White et al. (293B)reported that the detection of beet sugar adulteration of honey by quantitation of oligosaccharide-bound galactose by galactose oxidase treatment of the higher sugar fraction is useful to screen honeys with normal stable C isotope ratio values. However, additional testing is required for confirmation of adulteration. Adulteration of durum wheat pasta with nondurum wheat gliaden proteins was detected by Burgoon et al. (34B) using aluminum lactate polyacrylamide gel electrophoresis a t pH 3.1. Pastas adulterated with as little as 5% hard red winter wheat flour could be detected with this method. Cow milk adulteration of buffalo milk and buffalo mozzarella cheese was detected by the mobility of casein by polyacrylamide gel electrophoresis as reported by Beghi et al. (14B). Farag et al. (77B) used GC for the qualitative and quantitative determination of fatty acids of authentic buffalo milk, cow milk, and buffalo milk adulterated with cow milk, and by application of a simple regression equation for particular acids, adulteration of buffalo milk with 5% cow milk could be detected. Krause et al. (143B) reported that the presence of cow milk in sheep, goat, or buffalo milk could be detected a t 1-2% by measuring the amount of y-2-casein in the mixture by isoelectric focusing. The presence of cow milk could also be detected in sheep, goat, or buffalo cheeses. The presence of cow milk whey in whey cheeses was detected by determining @-lactoglobulinsby isoelectric focusing. In ricotta cheese, where the whey proteins are heat denatured, addition of a strong reducing agent was necessary to resolubilize the proteins before isoelectric focusing. Pollman (203B) used
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calcium, phosphorus, magnesium, and lactose indexes to detect adulteration in grated cheese. Carnegie et al. (38B) used a new HPLC method to monitor the adulteration of cooked beef products with meat from other species. The ratio of the histidine dipeptides anserine and carnosine, which are present in skelectal muscle, are so different between sheep, cattle, horse, and kangaroo that detection of adulteration can be rapidly achieved by HPLC on Partisil SCS columns with 0.2 M lithium formate at pH 2.9 as mobile phase. T o obtain a definitive identification of the adulterant, it was necessary to also examine the electrophoretic mobility of myoglobin in SDS gels. Imre et al. (125B)reported that polyacrylamide gel disk electrophoresis of beef, horse, and donkey muscle proteins gave species-specificpatterns that can be used for identification. The method can be used to detect 5% adulteration of ground beef with horse or donkey meat. Kumudavally et al. (145B)employed TLC and GC to analyze free fatty acids from canned meat curries prepared from fresh and spoiled mutton and admixtures of the two. Analysis of the free fatty acid fraction revealed a 10-12-fold increase in palmitic, stearic, and oleic acids. Zitko (306B) pubIished a review with 98 references on organic contaminants in fish and shellfish and methods for their determination. Firestone et al. (78B) reported on the detection of adulterated or misbranded olive oil products that have been shipped to the United States during 1983-1984. Triscornia et al. (267B) reported on the possibility of verifying the genuineness of olive oils by determination of the alkanal content of edible virgin and lampante olive oils and solvent extracts of olive marc. Mariani et al. (158B)detected solvent extraded marc oil in virgin (pressed) olive oil by separating the wax constituents with silica gel column chromatography or TLC, followed by determining the wax esters by capillary GC. Statistical procedures for the discrimination between marc oils and virgin, lampante, or rectified oils were proposed on the basis of the C number (34-46) and amounts of wax esters present. Addition of 10% marc oil to pressed oil was detectable. Dirinck et al. (65B)reported that total aldehyde or hexanal as main contributor to aldehyde content when determined by dynamic headspace analysis may be used for objective measurement of rancidity intensity in oils. El-Sayed et al. (72B) detected lard in hydrogenated fat by the higher amount of palmitic acid in the 2-position of the trigycerides, and the saturated/unsaturated acid ratio in the 2-position also could be used to distinguish lard from hydrogenated oil and shortenings. Gomez et al. (95B) detected mineral oil in vegetable oil by TLC, and analysis of rape oil denatured with aniline and associated with toxic syndrome showed that two oils presented an anamolous hydrocarbon band with characteristics similar to those of mineral oils. Gopalakrishnan et al. (97B) described a method for detecting and estimating adulteration in coconut oil with palmolein by treatment of the oil with Carr-Price reagent. The presence of palmolein is indicated by the appearance of a blue-black color, which was determined at 700 nm. A simple method for detecting palmolein adulteration in peanut oil was described by Motghare et al. (172B). Grover (1OOB)reviewed the presence and detection of toxic substances, in argemone, castor, karanja, ambadj, and salseed oils, aflatoxin in peanut oil, and thiocyanate and thiosalidines in rape oil. Han et al. (107B) developed a reversed-phase HPLC method for quantitative determination of adulteration of sesame oil with soybean oil. The procedure could be extended to detect adulteration of sesame oil with oils other than or in addition to soybean oil, e.g., with rape oil. Detection of argemone oil adulteration of edible oils was reported by Madhyastha et ai. (153B)by extraction of sanquinarine from an edible oil adulterated at 1% by argemone oil followed by its analysis on an alumina-silica gel minicolumn where it was detected as a yellow fluorescent band in the silica layer. N a s i d a h et al. (179B) reported a comparative study of three methods available for the detection of argemone oil in edible vegetable oils, a wet method which depends on the formation of crystalline red-brown chelation compounds of sanquinarine and dihydrosanquinarine with ferric chloride could detect argemone at 1%, and two chromatographic methods (paper and TLC) could detect 0.02%. Sauter et al. (215B)determined adulteration of pumpkin seed oil by thin-layer chromatography of the unsaponifiable fraction and examining the pattern of unsaponifiable compounds. Manandhar et al. (156B) de-
tected and estimated the presence of linseed oil in rape oil. Mariani et al. (157B) developed a procedure to detect adulteration of oils and margarines by determination of their mono- and diglyceride content. The glyceride classes were separated by TLC on silica gel with hexane-ether-formic acid (100:100:3),and silylated glycerides were further fractionated by GC on a 5% SE 52 glass capillary column with temperature programming. Sheppard et al. (232B) applied various analytical methods for the detection, identification, and quantitation of vegetable oil adulteration in ice cream by determination of total fat content, sterols, short- and long-chain fatty acids, vitamin E, Reichert-Meissl values, and Polenske values. All methods, except total fat determination were capable of detecting vegetable oil adulteration. Sterol determination was the most effective and versatile measurement because it provided information not only on the detection and extent of adulteration but also on the possible identity of the adulterant. Chadha et al. (39B) used capillary GC-FID for detection and identification of brominated vegetable oils in soft drinks. Gubman et al. (101B) determined phosphatides in plant oils colorimetrically. Gibbrellic acid residues on fruits was determined by Cruces et al. (51B) by synchronous scanning derivative spectrofluorometry. L-Pyroglutamic acid as an indicator of decomposition or abuse of processed foods was determined spectrophotometrically in molasses, wastewater, and catsup by Ekstoem et al. (71B). Uranium was determined in commercial milk samples by Gamboa et al. (85B)by measuring the a particles emitted after irradiation, chemical etching, and electrochemical etching, and Luan (152B) determined traces of arsenic in soft drinks by oscillographic polarography. Skatole and indole were determined in the back fat of pigs by Garcia-Regueiro et al. (86B) using RP-HPLC. Gardiner et al. (87B) used an improved modification of an official AOAC method for extraction and detection of filth in hard and soft cheese. Hatanaka et al. (109B) described a rapid and simultaneous analysis of hippuric acid and benzoic acid in fermented milk or raw milk using RP-HPLC. Microbial growth in stored wheat was assessed by Kaminski et al. (134B) by GC of the formed volatiles like diacetyl, acetoin, 3-octanone, and 1-octanol. Carbonyls, as a measure of bacterial and fungal infection changes, were measured as their oximes by photometry, and ergosterol as a measure of fungus and yeast growth was measured by capillary GC or UV spectrometry. Uric acid, free fatty acids, and polar lipids were determined with HPLC by Wetzel et al. (291B) as an objective criteria for condition of stored wheat. Pentachlorophenol residues in chicken liver and fat were determined by Neidert et al. (180B)by GC-ECD and in gelatin by Yip (301B) by GC-ECD on a 1% SP-1240 DA column with methane in argon as carrier gas. The method for pentachlorophenol in gelatin was adopted official first action by AOAC. Phenol was determined in honey by Ogawa et al. (185B) using GC-FID. Page (194B) determined acrylonitrile (ACN) in foods by headspace GC with N/P selective detection. The method was studied collaboratively for ACN determination in cold pack cheese, peanut butter, honey butter, and margarine (in plastic containers). The method for (ACN) was modified by Page et al. (1938) to include packaged luncheon meats. Decomposition products of Usal (aspartame HCl), were determined by Prude1 et al. (205B) in model systems and dioxopiperazine determined in soft drinks by HPLC. Usal and its decomposition products aspartic acid, phenylalanine methyl ester, aspartylphenylalanine,phenylalanylaspartic acid, and dioxopiperazine were separated on Separon Si C-18 using phosphate buffer (pH 2.1)-methanol (85:15) as mobile phase with UV detection at 200 nm. Takarai et al. (%OB) determined foreign substances in foods and additives (plasticizers) in commercial plastic products by direct inlet mass spectrometry (DI-MS)with no pretreatment. Fibers of cigarette filters were found in commercial shiokara; ethyl palmitate and ethyl linoleate, and ergosterol were found in commercial bread. A method of cleanup by droplet countercurrent chromatography (DCC) for food contamination monitoring was developed by Onji et al. (188B, 189B). Yamazaki e t al. (299B) proposed a method for dibutyltin determination in food ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
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containers and packaging materials. Residual vulcanization accelerators (dialkyldithiocarbamates) in baby bottle rubber teats were analyzed by Yamazaki et al. (298B) by GC with N / P detection. Vanhaelen-Fastre et al. (279B) qualitatively and quantitatively determined the hallucinogenic components of Psilocybe mushrooms by reversed-phase HPLC. Mycotoxin analysis was the subject of several review articles. Briantais (28B) published a review with 38 references on analytical methods for determination of mycotoxins, regulatory aspects, and control of foods. Aflatoxin B1, aflatoxin M,, and patulin contaminations were emphasized. Campbell et al. (35B) presented a review with 38 references on sampling, sample preparation, and sampling plans of foodstuffs for mycotoxin analysis. Coker (49B) wrote a review with 138 references on HPLC and other chemical quantification methods used in the analysis of mycotoxins in foods. Crosby @OB),in a review with 27 references, discussed chemical methods of analysis, for the extraction, cleanup, and determination of aflatoxins from animal feeds and foods. The advantages and disadvantages of TLC and HPLC were discussed along with newer techniques such as immunoassay. Methods for determination of ochratoxin, patulin, and trichothecenes were also included as well as problems encountered during collaborative mycotoxin method evaluations. Park et al. (195B) published a review with 55 references on the official methods of analysis of mycotoxins in foods such as those approved by the AOAC, IUPAC, AACC, and AOCS. Ueno (274B) published a review with 37 references on development of immunoassay using monoclonal antibodies for the detection of mycotoxins in farm products; the principles of immunoassay, preparation of antigens and antibodies, and application of the immunoassay in detection of aflatoxins, trichothecenes, and ochratoxins were discussed. Candlish et al. (36B) reported on a monoclonal antibody to aflatoxin B, and the detection of the mycotoxin by an "ELISA" assay which had a sensitivity of 0.2 ppb with a working range up to 10 ppb for aflatoxin B,. Ram et al. (206B) screened naturally contaminated corn and cottonseed samples for aflatoxin B1 by a direct competitive ELISA. ELISA estimates for aflatoxin B1in corn were in good correlation with values obtained by TLC, and ELISA estimates for aflatoxin B1 in cottonseed were in good correlation with values obtained by HPLC. By use of this ELISA, 36 duplicate sample extracts can be screened for aflatoxin B1 in less than 2 h. The use of ELISA for determining mycotoxins in food was discussed by Terplan et al. (262B)who used an ELISA assay to determine aflatoxin B1, aflatoxin M1, ochratoxin A, and T-2 toxin in various foods (milk, dried milk, cheese, yogurt, wheat, corn, peanuts, and barley). The results correlated well with those obtained by a TLC method. Ueno (275B) developed a simple and improved ELISA method for quantitation of aflatoxin B, by utilization of second antibody bound to beads and filtration plates. Aflatoxin B1 as low as 1ppb in peanut meal and 0.1 ppb in human blood was detected by the immunoassay method with recoveries of >80%. Dimitrov et al. (64B) discussed the results of international collaborative studies on the analysis of aflatoxin B,, B,, G1, G2,and M in corn flour, peanut meal, and powdered milk. The use of one- and two-dimensional TLC and GC methods gave best results in terms of simplicity, precision, sensitivity, and reproducibility. The occurence of aflatoxins in food and the development of methods for their determination were reviewed. Gilbert et al. (92B) surveyed aflatoxins in peanut butters, nuts, and nut confectionary products by HPLC with fluorescence detection. Results showed that 31 of 32 samples of major national brand-name products contained less than 10 ppb aflatoxin B1. Gulyas (202B) determined aflatoxins B,, B2,G1, G2,and M1 in peanut meal, corn flour, and milk powder by overpressure TLC of purified extracts using silica gel plates and chloroform-ethyl acetate-THF (8:12:0.6) at a pressure of 0.5 MPa. Aflatoxins were quantitated by emmission fluorometry. Sensitivity of method for aflatoxins was approximately 0.25 ng and for MI approximately 0.5 ng. Huang et al. (124B) separated aflatoxin B1,B,, G1, and G, by RP-HPLC and determined them by using UV at 365 nm with detection limit of 3.2-3.9 ng. Kawamura et al. (137B) developed a sensitive method for the determination of aflatoxin B, as its water adduct AFB2a in peanuts, cassava, and corn. The method used normal-phase and reversed-phase 216R
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HPLC. Aflatoxins in vegetable oils were analyzed by Miller et al. (166B),the oil samples dissolved in hexane were applied to a silica column and washed with ether, toluene, and chloroform; aflatoxins were eluted from the column with chloroform-methanol (97:3) solvent mixture, and quantitated by TLC and HPLC. Recoveries of aflatoxin B, standards added to aflatoxin-free oils were between 89.5 and 93.5% with precision of 6.3-8.0%. Orbey et al. (191B)determined aflatoxins B,, B2, G1, and G2 in hexane defatted hazelnuts by chloroform extraction, followed by cleanup on a silica gel cartridge and HPLC analysis using coumarin as internal standard. Shepherd et al. (229B) carried out a systematic investigation of the conditions employed for the postcolumn iodination reaction used to enhance fluorescence sensitivity of aflatoxins B, and G1 in reversed-phase HPLC. The effects of postcolumn reaction coil tubing dimension, coil temperature, eluent, and reagent flow rates and reagent concentrations were examined, and the optimum choice of each was established. The maximum achievable sensitivity was 20 pg of B, injected on column. Spilmann (240B)studied a modification of the AOAC official method for screening aflatoxin in corn and the feasibility of using it as a quantitative method. Several different corn products were analyzed by using the modified method with an average savings of >1 h/sample vs. the CB method, with average recoveries of B, of 94% for the low-level spiked samples and 108% for the high level. Results obtained by analyzing naturally contaminated samples compared favorably with the CB method. Picogram amounts of aflatoxins in milk and cattle were determined by Veres et al. (BOB)using radioimmunological analysis. Wei et al. (289B) determined aflatoxins B,, B2,G1, and G2 in infant food by normal-phase HPLC. Whitaker et al. (292B)determined the amount of aflatoxins extracted from raw peanuts by using water-slurry modifications of AOAC method 11 for 49 combinations of methanol concentration and solvent/peanut ratio. The amount of aflatoxins B, and B2 extracted from raw peanuts was a function of both methanol concentration and solvent/peanut ratio; a cubic equation was developed, using regression techniques, to describe the combined effects. From the functional relation, the predicted methanol concentration and solvent/peanut ratio were computed to be 60% and 10.8 mL/g of peanuts, respectively. This combination extracted 12.1 % more aflatoxin than did AOAC method 11. Fremy et al. (83B) established protocols for detecting picogram quantities of aflatoxin M1 in milk, yogurt, brick cheddar, and ripened Brie cheese by ELISA. Good agreement was found for aflatoxin M, levels in several naturally contaminated milk samples analyzed by both ELISA and HPLC. Saito et al. (214B) developed a TLC method for determining aflatoxins Ml and M2 and aflatoxicols I and I1 in cereals, nuts, and their products. Comparison and critical evaluation of six published extraction and cleanup procedures for aflatoxin M1 in liquid milk were carried by Shepherd et al. (230B);a prepacked reversed-phase cartridge method was shown to be the most satisfactory in terms of speed, cost, and cleanliness of the final residue. Stubblefield et al. (247B)reported the results of a collaborative study on rapid HPLC method for determination of aflatoxin MI and M2 in artificially contaminated fluid milks. The reversed-phase LC method for M1 and M2 has been adopted official first action by AOAC. A new hydroxyaflatoxin B,: aflatoxin M, was separated by Lafont et al. (146B) from mycotoxin fractions isolated from liquid or powdered milk. Solvent extracts of milk were purified by column chromatography and purified aflatoxins were separated by TLC on silica gel. Aflatoxin M4 was quantitated by visual comparison with standards under UV light or by fluorodensitometry. Trichothecenes and methods for their determination were reviewed by Bonchev et al. (24B). Pohland et al. (202B) published a review with 29 references on the analytical chemistry of deoxynivalenol including GC, TLC, HPLC, and GC-MS determination of the mycotoxin in foods. Yoshizawa (303B) in a review with 17 references discussed the characteristics of mycotoxins, food contamination with trichothecenes, and assay methods for mycotoxin determination in foods and biological samples. Bata et al. ( I I B )recommended a transesterification method for rapid quantitation of trichothecene toxins in foods and feeds, using both HPTLC and a capillary GC method. Blaas
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et al. (19B)described a GC-MS method for determination of deoxynivalenol (DON) and nivalenol (NV) at the ppb concentration range. A liquid chromatographic cleanup step was followed by silylation of the extract and the resulting TMSethers were determined by GC-MS monitoring the characteristic ions in the negative chemical ionization mode. Chromatography was performed on a DB-5 fused silica capillary column at 80-280' with helium as carrier gas. Brumley et al. (32B) discussed negative ion (NI) mass spectrometry of DON under resonance electron capture conditions. Certain fragmentations were studied by collision-induced decompositionjmass-analyzed kinetic energy spectroscopy. The NI technique was applied to the identification of DON in extracts of grains and snack foods by using on-column injection capillary GC. The sample extract was obtained by extraction with acetonitrile-water and was subjected to TLC as a quantitative screening or isolation step. Cohen et al. (47B) described a comparative study between two Canadian methods on the analysis for vomitoxin in cereal grains and showed that the use of Sephadex LH-20 for purification of extract along with a GC capillary system gives better accuracy and sensitivity in analysis and prevents interference that occurs in packed column GC. A capillary GC-EC determination of T-2 toxin, HT-2 toxin, and diacetoxyscirpenol (DAS) in cereal grains at levels as low as 100 ppb for T-2 and DAS and 50 ppb for HT-2 was described by Cohen et al. (48B). The method was applied to wheat, oats, and barley with average recoveries ranging from a low of 65% for T-2 in barley to a high of 99% for DAS in oats. Eppley et al. (74B) reported on the results of a collaborative study on a TLC method for DON in winter wheat, the results of the study showed that false positives were not a problem and that all of the collaborators could detect DON at the 300 ppb level or higher. The method has been adopted official first action by AOAC. The application of online supercritical fluid extraction with chemical ionization (CI) mass spectrometry (with ammonia as the CI reagent), and collision induced dissociation (with argon as target gas) tandem mass spectrometry, for the rapid identification of ppm levels of several trichothecene mycotoxins in wheat samples was demonstrated by Kalinoski et al. (133B). Maycock et al. (164B) described the preparation of the p-nitrobenzoyl derivatives of the 4-trichothecenetoxins T-2, diacetoxyscirpenol (DAS), nivalenol (NV), and deoxynivelenol (DON) and their separation by HPLC with UV detection at 254 nm. Vomitoxin was determined in grains and feed samples by Noonpugdee et al. (182B) by a combination of semipreparative HPLC and capillary GC-ECD. The limit of detection was 50 ppb in corn. Levels found in corn, barley, oats, wheat, corn spoilage, and mixed feeds were given. Romer (213B) reported that small charcoal/alumina cleanup columns were effectively used to remove interfering materials from grain, feed, and food extracts prior to chromatographic determination of trichothecene mycotoxins. A TLC method (with ethyl acetate-methanol (20:l) as mobile phase) has been developed that can simultaneouslydetect ppb levels of DON, fusarenon X, nivalenol, T-2 toxin, HT-2 toxin, neosolanical, and diacetoxyscirpenol in food and feed samples. The use of charcoal alumina cleanup columns in conjunction with HPLC and G of trichothecenes was also discussed. A rapid method for detecting DON was developed by Shannon et al. (227B) who employed a C18 silica gel reversed-phase column to remove impurities from grain extracts prior to TLC screening of DON using aluminum chloride as spraying agent to develop the blue response characteristic of the mycotoxin. Total time involved was approximately 30 min and the method was applicable to corn, wheat, and barley at detection levels of 1ppm and oats at 1.5 ppm, as well as environmental samples at 0.75 ppm. Steinmeyer et al. (245B)described a method for determination of deoxynivalenol and nivalenol in cereals by capillary GC-ECD of their heptafluorobutyrate derivatives DON and its metabolite DON-1 were analyzed in milk by Swanson et al. (249E) using C18cartridges for purifying the analyte solution for subsequent preparation of the TMS-ether derivatives which were GC-ECD analyzed on an OV-17 column. Tanaka et al. (255B) developed a sensitive method for the simultaneous analysis of DON and nivalenol in cereals. The toxins were extracted with acetonitrile-H20 (3:1), defatted with hexane, and purified by a two-step chromatographic
(i
procedure using Florisil and Sep-PAK columns. DON and NIV in the column eluates were quantitated by GC-ECD and GC-MS (single ion monitoring). Terhune et al. (261B) described a GC-ECD method for quantitation of DON in wheat, corn, and feed a t levels as low as 20 ppb. Tiebach et al. (265B) determined DON and NIV in naturally contaminated cereal samples by using direct liquid introduction HPLC-mass spectrometry in a negative ion chemical ionization mode and selected ion monitoring. HPLC was performed on a column of Fine Si1 C18-10, with acetonitrilewater (1:l) mobile phase Cereal samples were extracted with methanol, defatted with hexane, and cleaned up on a Florisil column. Confirmation of DON and NIV was also performed by capillary GC-MS after silylation. Trenholm et al. (271B) evaluated different extraction procedures and equipment for the analysis of naturally contaminated grain products for vomitoxin analysis and reported on the merits of different techniques. Trucksess et al. (273B) reported a modification of their TLC method (1984) for determination of DON in high-sugar breakfast cereals, corn syrup, and beer. Moniliformin was determined by Jansen et al. (129B) in vegetable foods and feeds. The mycotoxin was extracted by Soxhlet extraction with methanol from moldy corn, rice, rye, oats, wheat, and barley samples and was determined by TLC using MBTH as a new derivatizing agent for moniliformin. The moniliformin derivative was assayed at 518 nm. Scott et al. (219B) developed a rapid method for determination of Fusarin C in cereal products by RP-HPLC on normal-phase HPLC with UV detection at 365 nm. TLC and solvent stability of moniliformin mycotoxin have also been investigated. Shepherd et al. (231B) determined moniliformin in maize using ion-pairing extraction and ion-pairing HPLC with UV detection. ' Carman et al. (37B) described a rapid method for the determination and confirmation of the plant toxin myristicin in fresh, frozen, and canned carrots by GC bf purified extracts on a nonpolar stationary phase (OV-101) using FID. Suspected positive findings were confirmed by using a second stationary phase of moderate polarity (OV-225). Kellert et al. (138B) determined Alternatia toxins in moldy tomatoes, apple preserves, fruit, and tomato juices, etc. by GC/MS. Stack et al. (243B) described a liquid chromatographicmethod for determining tenuazonic acid (TA) and alternariol methyl ether (AME) in tomatoes and tomato products, based on extraction of Alternaria metabolites from an aqueous slurry of the sample with chloroform, centrifugation, and fractionation on a silica gel column. Reversed-phase HPLC with UV detection for TA at 280 nm and fluorescence detection for AME were used for final separation and determination. Chu et al. (42%) developed an ELISA assay for the detection of saxitoxin in shellfish. PSP toxins in shellfish were determined by Jonas-Davies et al. (132B) using an automated analyzer continuous flow reaction system to oxidize toxins to derivatives which are detected by fluorescence, while Sullivan et al. (248B) used an HPLC procedure for determining the toxins. Kubacki (144B) published a review with 33 references on methods for the determination of patulin in apple juice. Special attention was paid to HPLC. Data on the occurrence of patulin in apple juice and a few other apple products were included. Experimental results on the role of technological processes in decreasing patulin contamination of apple juice and apple wine were presented. Acar et al. ( I B )reported on the occurrence and determination of patulin in commercial tomato pastes. Patulin was extracted from tomato paste with ethyl acetate, followed by cleanup on a Florisil column and two-dimensional TLC using Silica Gel F254. The solvent systems were benzene-methanol-acetic acid (90:5:5) and toluene-ethyl acetate-formic acid (54:l). Spot visualization was with 4 % dianisidme and chlorine gas. The detection limit was 40 ppb, and patulin was absent in 23 investigated tomato paste samples. A method for HPLC determination of patulin in fruit juices was reported by Ehlers (69B). Patulin was separated from hydroxymethylfurfural and determined by chromatography on a silica el 40 column with toluene-ethyl acetate (3:l) and then on a iep-PAK cartridge with the same solvent. Eluted patulin was concentrated, redissolved in methanol-ethyl acetate (9:1),and HPLC analyzed on a Lichrosorb RP-18 with gradient elution and UV detection at 280 nm. Limit of deANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987 * 217R
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tection was 1 ppb and recovery from apple juice containing 160 ppm was 80%. Eller et al. (73B)presented a procedure for the evaluation of patulin content of fruit and vegetable juices and purees: two-dimensional TLC using silufol plates with trichloroethane-acetone-80% formic acid (16:3:1) and toluene-ethyl acetate-86% formic acid (5:4:1), development with benzidine HC1, and detection at 365 nm. Patulin was found in apple powder (80 ppm), molded strawberry (32 ppb), and molded mandarin orange (10-80 ppb). Forbito et al. @OB) described a rapid method for the quantitative determination of patulin in apple juice. The mycotoxin was extracted from the sample with ethyl acetate and the extract was cleaned up by extraction with a sodium carbonate solution, and patulin was determined by RP-HPLC using a FBondapak CIScolumn and UV detection at 254 nm. Ogawa et al. (184B)published a method on the determination of penicillic acid and patulin in commercial fruit juice by GLC of their trimethylsilyl derivatives. TLC determination of sterigmatocystin in cheese was reported by Francis et al. (81B).Cheese was extracted with acetonitrile-4% potassium chloride, the extract was partitioned with aqueous calcium chloride, hexane, and methylene chloride, and passed through a column of copper carbonatediatomaceous earth (1:2) eluting with methylene chloride. The eluate was evaporated and sterigmatocystin determined by chromatography on Sil-G-25 HR plates with benzene-methanol-acetic acid (85:10:5) and was visualized by spraying the plate with AlCl,. The fluorescence of the spot was enhanced 10-fold by additional spraying with a silicon-ether mixture enabling detection and quantitation at 2 and 5 ppb, respectively. Average recoveries were 88.3% and 86.4% at the 10 and 25 ppb levels. Zearalenone and deoxynivalenolwere determined by Bennett et al. (15B) in corn, wheat, oats, rice, and barley. The toxins were extracted with aqueous methanol and partially purified by partitioning into ethyl acetate and then defatting with acetonitrile-petroleum ether. Toxins were then isolated by silica gel column chromatography. Interfering materials were removed from the column with benzene; zearalenone was eluted with benzene-acetone (95:5), and after a column wash with chloroform-methanol (98:2), deoxynivalenolwas eluted with chloroform-methanol (95:5) and zearalenone was quantitated by TLC and deoxynivalenol by gas chromatography of the TMS derivative. The detection limit for each toxin was about 0.02 ppm. Recoveries of added toxins varied with substrate and level of toxin. Bennett et al. (16B)reported on the results of a collaborative study on an HPLC method for the determination of a-zearalenol and zearalenone in corn. The method has been adopted official first action by AOAC. Czerwiecki (54B)determined zearalenone in wheat and rye samples by cleaning up grain chloroform extracts on silica gel column and separation of column eluate by TLC. The mycotoxin was detected by spraying the plate with alcoholic aluminum chloride, heating at 130' for 5 min, and visualization under UV. Limit of detection was 300 ppb. Liu et al. (150B) developed a competitive indirect enzyme-linked immunosorbent assay (ELISA) for the detection of zearalenone in methanol-water extracts of corn, wheat, and pig feed samples. Warner et al. (288B) reported a screening method for zearalenone in corn by competitive direct enzyme-linked immunosorbent assay. Average zearalenone recoveries from corn spiked at levels of 57, 151, and 307 ppb were 50, 119, and 123%, respectively. Levels of zearalenone detected in naturally contaminated samples were comparable to those determined by liquid chromatography. Tanaka et al. (254B) reported a rapid and sensitive method for the determination of zearalenone in cereals by HPLC with fluorescence detection. Zearalenone was extracted with acetonitrile-water (3:1), purified on a Florisil column, resolved by using 90% water saturated chloroform-cyclohexane-acetonitrile-ethanol (5015:2:1), and quantitated by fluorescence measurement detecting zearalenone in wheat, barley, corn, and cereals with picogram sensitivity. A combination of this HPLC method with GC method for trichothecenes may be applied to the simultaneous detection of zearalenone, nivalenol, and deoxynivalenol In cereals. Golinski et al. (94B) described chemical confirmatory tests for ochnatoxin A, Citrinin, penicillic acid, sterigmetocystin, and zearalenone performed directly on TLC plates. After 218R
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extraction and preliminary cleanup, the mycotoxins were easily separated by TLC using toluene-ethyl acetate-90% formic acid (6:3:1)developing solvent. The developed chromatogram was exposed to vapors of pyridine or acetic anhydride or a mixture was overspotted on the mycotoxins. With this treatment ochratoxin A, citrinin, penicillic acid, and zearalenone were converted to new fluorescent compounds, which were rechromatographed with the same developing solvent and examined under UV at 365 nm. Sterigmatocystin was confirmed chemically using TLC plates impregnated with 0.6 N sulfuric acid or 10% oxalic acid in methanol. Lepom (148B) simultaneously determined citrinin and ochratoxin A in wheat and barley using RP-HPLC-fluorescence detection. Valente et al. (276B)developed a minicolumn screening and a TLC quantitation methods for determining ochratoxin A in corn, peanuts, beans, rice, and cassava. A method for the determination of ochratoxin A in pork kidneys was developed by Wilken et al. (294B). Homogenized sample was extracted with ethyl acetate, acidified, and chromatographed on a silica gel column eluting ochratoxin A with ddute formic acid in chloroform. The evaporated eluate was redissolved in methanol and analyzed by two-dimensionalTLC with fluorescence detection or by RP-HPLC with fluorescence detection. Several reviews were published related to pharmaceutical residues in food. Bishop et al. (18B)wrote a review with 59 references on classical and recent methods for antibiotic determination in milk. A review by Bories (25B) discussed the control of pharmaceutical residues in foods of animal origin and methods of determining residues with the example of anabolic hormones. Clark et al. (43B) discussed screening methods and instrumental techniques for determining drug residues in foods of animal origin and the potential use of enzyme immunoassay, and of two mass spectrometers in tandem in screening for veterinary residues. Petz (200B) reviewed chemical residue analysis of veterinary drugs in food, general methodology, and GC procedures. Shaikh et al. (226B) published an overview of physical-chemical methods for determining aminoglycosideantibiotics in tissues and fluids of food-producing animals. Archimbault et al. (6B)determined chloramphenicol in poultry by reversed-phase HPLC and absorbance detection. Radioimmunological determination was used by Arnold et al. (7B)for chloramphenicolresidues in swine muscle, milk, and eggs. Bergner-Lang et al. (17B) determined chloramphenicol in milk by reversed-phase HPLC-EC. Haagsma et al. (105B) described a rapid sample preparation method for the determination of chloramphenicol in swine muscle by HPLC. Keukens et al. (139B) reported two HPLC methods for analysis and confirmation of chloramphenicol residues in meat with off-line cartridge sample cleanup and on-line diode array UV-Vis detection. Schmidt et al. (217B)used electrochemical detection to determine chloramphenicol residues in fish. Determinationof diethylstilbesterol in canned steamed pork by gas chromatographywas reported by Lin et al. (149B). Van Peteghem et al. (277B) reported a method for diethylstilbesterol residue determination in meat samples that involved chromatographic purification and radioimmunoassay. Ashworth (8B)reviewed the liquid chromatographic assay of tetracyclines in meat. Botsoglou et al. (26B)determined tetracycline, oxytetracycline, and chlorotetracycline by reversed-phase HPLC with monitoring at 361,357, and 377 nm, respectively. Hoshino et al. (12IB)analyzed purified antibiotic extracts from beef, pork, and chicken using reversed-phase HPLC and UV detection at 268 nm. Moats (167B)determined tetracycline antibiotics in blood serum, muscles, liver, and kidney of cattle by HPLC employing polymeric and reversed-phase column. Oka et al. (186B) semiquantitatively detected and determined tetracycline and related compounds in foods by chromatography on highperformance or reversed-phase silica gel TLC plates. Prepacked CI8 cartridges were used by Oka et al. (187B) for tetracycline residue analysis in animal liver. Meat and fish were analyzed by Onji et al. (19OB)for its tetracycline content using HPLC-UV after sample cleanup on an Amberlite XAD-2 column. Honey oxytetracycline residues were analyzed by using reversed-phase HPLC-UV at 355 nm, by Sporns et al. (241B) and by Takeba et al. (253B). Terada et al. (258B) determined tetracycline residues in foods using RP-HPLC-UV at 340 nm. Traldi et al. (270B) described a
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rapid and sensitive method for the selective detection and quantitation of oxytetracycline residues at the ppb levels in crude extracts of bovine meat and milk. The technique employed was a tandem mass spectrometric method: CAD MIKE spectrometry. Quantitation was performed by single ion monitoring of CAD species of oxytetracycline and of ita internal standard. Shaikh et al. (225B)described a method for the determination of neomycin in animal tissue. Heat deproteinized extracts of animal tissues were acidified to pH 3.5-4 and directly analyzed by.RP-ion paired HPLC with o-phthaldehyde postcolumn derivatization and fluorometric detection. Lactam ring antibiotics in milk were detected by Brown et al. (31B)using a simple fast and inexpensive enzyme immunoassay. Moats (168B)determined penicillin G and cloxacillin residues in pork and beef tissues by RP-HPLC-W at 220 nm. The method was suitable for other monobasic penicillins but not for dibasic or amphoteric penicillins. Chromatographic methods were reported by Moats (169B)for the determination of macrolide antibiotic residues in tissues and milk of food producing animals. Two-dimensionalTLC has been used for the detection of tylosin in poultry, meat, eggs, and milk and for erythromycin in poultry meat, and HPLC using reversed-phase end-capped C18 columns which has also been used for determination of tylosin in milk, blood, and tissue of animals. The LC method was more sensitive than microbiological assays for detection of tylosin in tissues of treated swine, and recoveries of tylosin by LC method were frequently several-fold higher. Munns et al. (173B)reported a multiresidue method for the determination of eight neutral p-lactam penicillins in milk by RP-HPLC-fluorescence detection. Nagata et al. (176B)used RP-HPLC-UV at 222 nm to determine ampicillin residues in fish tissues. Horie et al. (119B) determined spiramycin in swine, cattle, and chicken muscles using RP-HPLC-UV at 232 nm and identification by MS. Nagata et al. (177B)determined spiramycin in chicken tissue by using Zorbax C8 column-UV at 231 nm. Kanamycin was determined by Nakaya (178B)in muscle and kidney of cattle using RP-HPLC-fluorometry. Terada et al. (259B)simultaneously determined penicillin G, penicillin V, and ampicillin in milk using RP-HPLC with a mobile phase containing sodium alkylsulfonate. Prior to HPLC, samples were pretreated with a SepPAK CIScartrid e. The peaks corresponding to each 0-lactam antibiotic can \e confirmed with the treatment using penicillinase. Terada et al. (260B)also determined penicillin G in edible animal tissues. The method consists of an off-line cleanup step using a basic aluminum oxide column and a Sep-PAK CI8.cartridge and an on-line precolumn concentration and purification system. Thorogood et al. (264B)reported on their evaluation of the Penzim method (a rapid enzymic assay) for the detection of P-lactam antibiotics within 20 min. Raw whole milk was used to establish its repeatability and reproducibility for the determination of penicillin G. Electrophoric methods for the detection of residual antibiotics in meat and eggs were reported by Ionova et al. (127B)and in meats by Tao et al.
(256B). Haagsma et al. (103B)described a rapid procedure for the determination of sulfamethazine in swine tissues which comprises sonication and extraction with methylene chloride, cleanup of the extract on a combination of silica and reversed-phase C18 Sep-PAK cartridges, and RP-HPLC analysis on a Hypersil ODS column with acetonitrile-10 mM ammonium nitrate (3:l) at pH 6.8 with UV detection at 254 nm. Haagsma et al. (104B)reported a rapid method for determining five sulfonamides in ground pork using a cation-exchange resin column for cleanup followed by analysis of purified extracts on a Chrompack column and UV detection at 254 nm. The results of a collaborative study on a TLC screening method for the detection of five sulfonamides in swine tissue were re orted by Haagsma (106B).HobsonFrohock (117B)used 8 C and HPLC for determining medicinal additives in poultry tissue. The use of droplet countercurrent chromatography and size exclusion chromatography was suggested to improve sample cleanup. Application of the photodiode array detector in the field of residue analysis was discussed and an example given of its use in methodology development. Malisch (155B)described a procedure f9r the extraction, cleanup, derivatization, and quantitative determination (by GC and HPLC) of >60 antimicrobials, anti-
parasitics, and growth promoters in meat, milk, and eggs with emphasis on sulfonamide determination. Nagata et al. (I 7 4 4 175B) described HPLC methods for the determination of residual thiamphenicol and ethopabate in chicken. Neidert et al. (181B)mehured sulfathiazole residues in honey using a rapid quantitative TLC and fluorescent scanning densitometry. Residual thiamphenicol in yellow tail muscle was determined by Otsuka et al. (192B)by RP-HPLC. Parks (196B)developed two procedures for the simultaneous determination of sulfa drugs and/or dinitrobenzamide coccidiostats, and their monoamine metabolites in chicken liver. Parks et al. (197B)quantitated zoalene and its two major monoamino metabolites using RP-HPLC with an electrochemical detector in the reductive mode. Paulson et al. (198B) described HPLC and GC-MS methods for identification and quantitation of sulfamethazine metabolites in swine tissues. Schwartz et id.(218B)described a simple method for rapidly screening sulfathiazole in honey. A GC-MS procedure using isotopically labeled internal standards and selective ion monitoring was used by Simpson et al. (237B)to assay five sulfonamide residues in liver and muscle tissue of swine, poultry, and cattle. Tranquilizer residues, namely, xylazine, azaperone, acepromazine, propylporomazine, and chloropromazine, were determined in alkaline homogenates of beef, pork meat, and kidney by extraction into an organic solvent and then into an acid followed by RP-HPLC with UV and amperometric detection as reported by Etter et al. (75B).Blomkvist et al. (22B)reported on the qualitative and quantitative analysis of monensin A sodium salt in the low nanogram range in samples of chicken fat by TLC and fast atom bombardment MS. Blum et al. (23B)determined the thyrostatic drug methylthiouracil (MTV) by HPLC and HPTLC in tissues of frozen-thawed samples of fattening cattles. Hoshino et al. (30B)determined monensin in chicken meat by HPLC with fluorescence detection. Monensin was also determined in milk by Karkocha (135B)by two-dimensional TLC. TLC plates sprayed with a 3% vanillin solution in methanol was used for visualization. Martinez et al. (1598)developed a method in which monensin residues were extracted from beef liver tissue, acetylated, partitioned, and reacted with B-anthryldiazomethane (ADAM) to form a fluorescent derivative for quantitation by LC. A multiresidue method was developed by Martinez et al. (160B)whereby residues of monensin, salinomycin, narasin, and lasalocid were determined in beef liver. The ionophores were extracted with aqueous methanol, purified by both alumina and Sephadex LH-20 column chromatography, and then derivatized with ADAM (directly with lasalocid) and via acetylation for the other three. The ADAM derivatives were then purified on a silica gel column and determined by RP-8 HPLC column using fluorescence detection. Takatsuki et al. (2518)analyzed monensin residues in chicken tissues by normal-phase HPLC of its ADAM fluorescent derivative. Dimenna et al. developed a TLC bioautographic assay for satinomycin in chicken liver (62B)and in chicken fat and skin (63B).Awasthi (9B)described an extraction cleanup method for GC determination of synthetic pyrethroid residues in fruits and vegetables. Ito et al. (128B)determined natamvcin. an antifur& residue, in natura cheese by UV spectrophkometry and RP-HPLC. Aitzetmueller et al. (2B)developed a normal-phase HPLC method for determining metaldehyde residues in vegetables. Metaldehvde was extracted with toluene and then deDolvmerized b i acid and derivatized to acetaldehyde dinkrophenylhydrazone which was chromatographed and detected by W. Bloeck et al. (21B)determined aldehydes and ketones in bottled and canned apple juice by converting them into corresponding 2,4-dinitrophenylhydrazoneswhich were analyzed by reversed-phaseHPLC on a Zorbax ODS column with 42% aqueous acetonitrile and absorbance monitoring at 365 nm. Buckley et al. (33B) used electron capture gas chromatography to determine traces of formaldehyde in milk as its 2,4dinitrophenylhydrmne. DeFreitas et al. (568)determined formaldehyde in meat by photometry with acetylacetone. Hayashi et al. (11OB)determined trace amounts of the mutagen methylglyoxal in foods and beverages by a newly developed method that involves reacting Me glyoxal with cysteamine at pH 6 to give 2-acetylthiazolidine which was analyzed by GC on a fused silica capillary column and monitored ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
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by thermionic N / P specific detector; formaldehyde was determined in coffee as its thiazolidine derivative, by Hayashi et al. (111B)as well as sweetened commercial food items (112B). Trace amounts of formaldehyde in aqueous extracts and model mixtures simulating foods were determined by Pertsovkii et al. (199B) by GC of its 2,4-dinitrophenylhydrazone derivative. The method was suitable for monitoring the migration of formaldehyde from polymeric materials into food products. Shin et al. (233B)analyzed n-hexanal in heads ace vapor over cooked brown rice by direct vapor injection 8C-FID on a column of 18% Carbowax 20M on Chromosorb H P and correlated between oxidative deterioration of unsaturated lipids and n-hexanal during the storage of brown rice (224B). Black et al. (20B)detected hydrogen peroxide in pasteurized cream by mixing the cream with tungstic acid, filtering, and forming a stable yellow complex in the filtrate with titanium tetrachloride the absorbance of which was measured at 415 nm. Srinivas et al. (242B)described a method for determining hydrogen peroxide in milk which is based on the catalytic decomposition of HzOz by a y irradiating catalyst and measuring the liberated oxygen with a gas measuring buret. A review on the contamination of foods by polycyclic aromatic hydrocarbons (PAH),polychlorinated biphenyls (PCBs), and heavy metals was published by Gonzalez (96B)discussing levels, toxic effects, and determination of these contaminants. Coates et al. (45B) analyzed PAH in plant materials using a method that involved extraction with acetonitrile (sonication), partition into pentane, and fractionation on a microsilicic acid column followed by GC-FID. Joe et al. (131B) determined trace levels of carcinogenic and noncarcinogenic PAHs in smoked foods, by reversed-phase HPLC on a Zorbax ODS column with both fluorescence and UV detection, PAHs were determined by Lawrence et al. (147B) a t nanogram/kilogram levels in meat, fish, dried dairy products, cereals, leafy vegetables, and vegetable/marine oils by reversed-phasegradient elution HPLC and fluorescence detection. Takatsuki et al. (252B) presented a method for PAHs in fish and shellfish using HPLC and fluorescence detection. Welling et al. (29OB) compared two cleanup procedures €or analysis of PAHs in edible oils, one method comprised a liquid-liquid extraction followed by XAD-2 chromatography and the other involved a complexation with caffeine-formic acid followed by HPLC in combination with wavelength programmed fluorescence detection. Morozzi et al. (171B)described an analytical method for determining a-benzopyrene and other PAHs in smoked or cooked foods using TLC on cellulose acetate plates and detection by UV fluorescence. Xia et al. (296B) used paper chromatography followed by fluorometric measurements of a-benzopyreneof benzene eluates from paper chromatograms. 3,4-Benzopyrene was determined by Song et al. (239B) in edible oils by caffeine complexation, followed by silica gel column chromatography and TLC on acetyl cellulose plates with densitometric detection. Dennis et al. (61B)described a method for the analysis of nitro-PAH in foods using a coupled capillary GC thermal energy analyzer. Joe et al. (130B)analyzed sever smoked foods for basic N-containing polynuclear aromatic hydrocarbons (NPAH) using a Vydac CI8 column with acetonitrile-water (9:l) with UV and fluorescence detectors connected in series. The migration of substances from ackaging materials into foods and food models and mekhog for determining such migrants in foods was reviewed by Giacin (89B). Chernitsyna et al. (40B) described a headspace GC-FID method for determining the migration of organic substances from polyethylene and polypropylene used as food contacting materials. BHT migration from polystyrene and polypropylene packaging materials into a fatty food model was determined by Cweik et al. (53B) using GC-FID on a 10% OV-101 on GasChrom Q column with argon as carrier gas. Acetaldehyde migration from polyethylene terephthalate containers was determined by Lorusso et al. (151B)using headspace GC-MS. Snyder et al. (238B)evaluated a new FDA migration cell used to study migration of styrene from polystyrene into various solvents. Headspace capillary GC analysis of residual solvents in food packages was applied by Rochelli et al. (212B). Two vaporphase injection systems on packed and capillary columns were
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compared. Solvents released from printing inks and adhesives can be distinguished from thermal decomposition products. Zenner et al. (305B) determined the volatile solvents given off by pack material coatings for food by headspace GC on a column of 20% polyethylene glycol adipate on porolith. Xylene, ethylene glycol, ethylene glycol acetate, acetone, ethyl acetate, ethanol, butyl acetate, and toluene were found. Results were discussed with respect to food contamination by these compounds. Tencheva et al. (257B)determined the concentrationof free radicals in irradiated prunes, nuts, and corn using EPR spectroscopy. Ward et al. (286B)applied liquid chromatography-electrochemical detection for the determination of toxic byproducts of boilable polyurethane cooking pouches. Ethylene dibromide (EDB) residue confirmation in grain and food products was reported by Barry et al. (1OB)using GC/MS with electron impact or negative ion chemical ionization selected-ion monitoring. The three commonly used methods for the determination of ethylene dibromide (EDB) fumigant residue in grains and grain-based products, namely, soaking in hexane, triple codistillation with hexane from an aqueous sample solution, and soaking in acetonewater (51), have been compared by Clower et al. (44B), and EDB recovery efficiency of each was reported. Gilbert et al. (93B) developed an automated headspace capillary GC-MS method using selected-ion monitoring for determination of EDB residues in fresh fruits. Heikes (113B) developed a purge and trap method for determination of EDB in whole grains, milled grain products, intermediate grainbased foods, and animal feeds and in table-ready foods (114B). EDB collected on adsorbent Tenax TA is eluted with hexane, determined by GC-EC, and confirmed with Hall electrolytic conductivity detection using a second GC column. The highest levels of EDB were also confirmed by full scan GC/MS. Konishi et al. (142B) determined EDB in foods and grains by GC-EC using a high-resolution capillary column. Flour products were GC analyzed for EDB by McKay (165B)using a 10% SP1200 + 1% phosphoric acid on Chromosorb W column. Automated purge and trap GC-EC methods were used by Moon e t al. (170B) and by Pranoto-Soetardhi et al. (204B) for EDB residue analysis in rice and wheat flours and cereals. Van Rillaer (278B)determined residual EDB in wheat cereals, and dried fruits by GC-EC. DeVries et al. (58B) determined carbon tetrachloride, ethylene dichloride, and ethylene dibromide in grain and grain-based products by capillary GC-EC after hexane codistillation using an internal standard (1,2-dichloropropane and 1,2-dibromopropane). A headspace GC method for determining methyl bromide in food ingredients was developed by DeVries et al. (59B),and Delton et al. (60B)determined carbon tetrachloride and ethylene dichloride in grain by volatilization in a hermatically sealed glass container followed by headspace GC-FID. Stijve et al. (246B) reported on the results of an interlaboratory study for determination by GC-MS of 2-chloroethanol (a residue arising from ethylene oxide fumigation) in spices. Toyoda et al. (269B) determined minute quantities of chloroform in foods by GC-MS analysis of pentane extracts of the steam distillates of fats, oils, Tofu, noodles, and beverages. Phosphine residues in rice were determined spectrophotometrically by Rangaswamy et al. (209B) and by Scudamore et al. (220B)who determined it in cereal grains and nuts using GC on a Poropak Q column with P-specific thermionic detection. N-Nitroso compounds in foods was the subject of a review by Eisenbrand (70B) who covered the detection and determination of nitrosamines in foods as well as the problems of sample contamination and artifact formation. Scanlan et al. (216B) gave an update of new analytical techniques for determining volatile and nonvolatile nitrosamines in foods and beverages and Sen (223B)wrote an extensive review on recent trends in nitrosamine analysis in foods. Sen et al. (222B) developed a simple direct extraction method for the determination of volatile N-nitrosamines in rubber nipples and pacifiers. It consists of overnight extraction of the sample with dichloromethane in the presence of ascorbyl palmitate for N-nitrosation inhibition, filtration, concentration using a Kuderna-Danish concentrator, and final analysis by GC-thermal energy analyzer (TEA). Thompson et al. (263B) determined N-nitrosamines and N-nitrosamine precursors in
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rubber nipples from baby pacifiers by GC-TEA. Beattie et al. (13B) determined nonvolatile nitrosamines by moving belt liquid chromato raphy/mass spectrometry (LC/MS) and spectra achieved y ammonia chemical ionization. Dunn et al. (67B) analyzed cured meat samples for N-nitrosoproline (NPRO) using methanolic extraction, followed by GC-TEA. Gavinelli et al. (88B) analyzed volatile nitrosamines in foods by a new method involving simultaneous distillation-extraction. Hu et al. (123B) determined volatile nitrosamines in foods by GC-TEA. The sample is distilled at 110-120°, the distillate was extracted with dichloromethane, extract concentrated, and subsequently GC analyzed on a 10% poly(ethy1ene glycol) column. Gracheva et al. (98E)determined N-nitrosamines by isolation from food samples, denitrosation, refluxing the secondary amine obtained with an 8-10-fold excess of 8-methoxy-6-q~olinesulfonylaziridine in aqueous alcohol at pH 7-9, and measuring the fluorescent derivatives formed. HPLC was applied by Kim et al. (140B) for the determination of N-nitrosodialkylamines in fermented and salted foods. Massey et al. (161B)determined N-nitrosoamino acids by denitrosation/TEA. Sen et al. (221B) developed a simple HPLC/chemiluminescence detection method for the analysis of N-nitrosamides in foods and beverages based on postcolumn denitrosation of the compounds with HBr-HOAC or HIHOAC, followed by the detection of liberated NO by a chemiluminescence detector. N-Nitrosothiazolidine and nonvolatile (N-nitrosourea) in foods were determined also by Sen et al. (224B) using the chemical denitrosation/TEA method; in addition, two GC/ TEA for determining nitrosothiazolidine and N-nitrosothiazolidine-4-carboxylicacid in cereal, meats, and fish were mentioned. Piasecka et al. (201B) reported an improved method for determining N-nitrosamines in beef meat by isolation by distillation under reduced pressure followed by GC on a column of 10% PEP 20M on Chromosorb AWDMCS. Tricker et al. (272B) developed a method for the analysis of three N-nitrosodipeptide derivatives in cured meat by HPLC on a Zorbax CN column, with acetone-acetic acid-hexane (181:81) as mobile phase and chemiluminescence detection. Ergot alkaloids in wheat and rye flours and breads and other cereal products were determined by Baumann et al. (12B) using reversed-phase HPLC-fluorometry after initial extraction and cleanup of samples by an extralut column. Klug et al. (141B)described a method for determining ergometrine, ergometrinine, ergosine, and ergotamine on a Hypersil ODS column (3 rm) with acetonitrilewater (47:53) as mobile phase. Ware et al. (287B) determined ergot alkaloids in wheat by HPLC using a porous cross-linked poly(styrene-divinylbenzene) column with a mobile phase of acetonitrile-O.05 M dibasic ammonium phosphate (55:45) at pH 10 and fluorescence detection. Potato glycoalkaloids were determined by Hellenaes (I 16B) who used Sep-PAK cartridges replacing commonly used alkaline precipitation for cleanup of tuber extracts, followed by reversed-phase HPLC and W detection. Resulb showed good agreement between this method and an ELISA and colorimetric methods. Colchicine alkaloids in tissues and biological fluids of cows were determined by Yoneda et al. (302%). Samples were extracted with acetone, acetone solutions defatted with petroleum ether, zinc sulfate, and barium hydroxide solutions added to the acetone extract for protein removal followed by chloroform extraction of alkaloids and subsequent HPLC-UV at 350 nm using a column of Lichrosorb RP-18 with acetonitrile-methanol phosphate buffer as mobile phase. Cyanogenic glycosides and cyanohydrins were determined by Brimer et al. (30B) in plant tissues by enzymic postcolumn cleavage and electrochemical detection after reversed-phase HPLC. Chikamota et al. (41B)indirectly determined cyanide concentrations in beans by measurement of acetone and 2butanone formed from the hydrolysis of bean cyanogenic glycosides using GC-MS. Dalgaard et al. (55B)analyzed crude and partially purified extracts from cassava for cyanogenic glycosides by electrochemical detection of cyanide ion liberated by enzymic postcolumn cleavage. Detection limit was in the low picomole range. Maitani et al. (154B) determined cyanogenic compounds in health foods made of Japanese apricot by treatment with P-glucosidase followed by steam distillation and colorimetry of liberated cyanide ion. Free cyanide content
%
was determined colorimetrically with enzymic treatment. Histamine and agmatine were analyzed by Matsunaga et al. (162B)by GC-MS. Matsunaga et al. (163B)simultaneously determined tyranine, histamine, putrescine, 0-phenylamine, cadaverine, agmatine, and tryptamine in soy sauce, miso, and cheese by reversed-phase HPLC. Offizorz et al. (183B) determined histamine in fish and canned fish by capillary isotachophoresis. Ramantanis et al. (207B) fluorometrically determined histamine and other biogenic amines in dry sausage after extraction with TCA, followed by purifying the extract on a weak acid cation-exchanger, derivatization with o-phthaldialdehyde, and measurement of reaction products at 445 nm after excitation at 360 nm. This method was more precise than the TLC method by same authors (208B). Tiecco et al. (266B) used high-resolution liquid chromatography to determine histamine and 10 other biogenic amines in sausages. Walters (285B) determined histamine and other related compounds in fish by HPLC with postcolumn reaction and fluorometric detection. Hashiba et al. (108B)determined 0-phenylethylamine and putrescine in soy sauce by ion exchange chromatography. Ingles et al. (126B)analyzed foods for their content of biogenic amines by ion exchange and HPLC methods. In the latter the amines were chromatographed as their fluorescamine derivatives followed by identity confirmation using field-desorption MS. Tonogai et al. (268B) developed a headspace GC method for the determination of volatile amines and ammonia in raw fish and fish products. Wakabayashi e t al. (282B) quantified mutagenic and carcinogenic heterocyclic amines in cooked foods by HPLC with a combination of reversed-phase and cation-exchange columns with electrochemical detection. Yamaizumi et al. (297B) employed stable isotope dilution for determining mutagens in cooked food by combined LCthermospray MS. Yen (300B) determined biogenic amines in fermented soybean by reversed-phase HPLC of their dansyl derivatives on a Lichrosorb RP-18 column with acetonitrilemethanol-H20 (1:2:1) mobile phase. An automated ion-exchange chromatographic method for the composite analysis of biogenic amines in cheese was used by Zee et al. (304B). Cuq et al. (52%) published a review on the formation of lysinoalanine in thermal processing of food proteins, especially at alkaline pH, and its determination in food, and Edmonds et al. (68B)used directly combined HPLC/MS for the analysis of heterocyclic aromatic mutagens in cooked foods.
CARBOHYDRATES Several books have been published during this review period including: T h e Analysis of Food Carbohydrates, edited by Birch (17C);Carbohydrates, edited by Collins (21C);The proceedings of the conference held in Copenhagen, Denmark, on "New Approaches to Research on Cereal Carbohydrates, edited by Hill et al. (37C);and the 42nd volume in Advances in Carbohydrate Chemistry and Biochemistry, edited by Pigman et al. (64C). Several review articles have been published on carbohydrate analysis. Clode (20C) discussed general methods of carbohydrate isolation and X-ray crystallography,TLC, GC, HPLC, IR, and NMR spectrometric, and polarimetric analysis of carbohydrates. The analysis of food glycosides was reviewed by Dziedzic et al. (24C). Folkes et al. (28C) wrote a review on analytical methods for the characterization of glucose syrups. Folkes (29C) reviewed GC methods for carbohydrate analysis in foods. Physical, chemical, and biochemical methods of analysis of food carbohydrates were reviewed by Kearsley (41C). HPLC methods for determining sugars and polysaccharides in food including information on extraction, cleanup, separation, and detection systems, as well as applications were covered in a review by Macrae ( 5 0 0 Pirisino (65C) reviewed fixed-ion resin and amino-bonded silica columns used in HPLC of carbohydrates in foods. Methods of determining the degree of starch damage in cereals including microscopic, enzymic, and instrumental procedures were published by Podgorska (66C). A review on the application of gel permeation chromatography in the separation of starch components and derivatives from food was published by Pranzik (67C). Rathbone (68C) discussed the use of NMR in the structural analysis of food-related carbohydrates. Reimerdes et al. (70C)reviewed qualitative and quantitative chromatographic, spectrometric, and other ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
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methods of carbohydrate analysis in food. Shallenberger (79C) reviewed the principles of optical polarimetry, the optical rotatory characteristics of sugars, and applications of polarimetry to sugar structure studies and quantitative analysis in foods. Sumida et al. (83C) wrote a review on chromatographic analysis of sugars (mono-, di-, oligo-, and polysaccharides) of soybean milk by HPLC. Athnasios (4C)developed a method for the analysis of trace levels of D-glucosone in complex food matrices by isolating D-glucosone using reversed-phase microcolumn chromatography, followed by reacting it with 2,4-dinitrophenylhydrazine (2,4-DNPH) to yield the corresponding osazone which was subsequently determined by normal-phase TLC and normal-phase HPLC, with absorbance detection at 436 nm. Den Drijver et al. (23C) used a strongly basic anion-exchange HPLC column coupled with an amperometric detector to detect u-glucosone in 7-irradiated sugar solutions, irradiated model fruit systems, as well as in irradiated whole fruit. Enzymic-spectrophotometric methods for the analysis of mono, di-, tri-, and polysaccharides as well as sugar alcohols in food products were reported by Beutler who determined xylitol ( I I C ) ,D-sorbitol (12c),maltose ( 1 3 3 , raffinose (14c), lactose and D-galactose (15C),and starch (16C). Fozy et al. (30C) determined glucose, lactose, and sucrose by an enzymic method in natural and milk chocolates. Frank et al. (31C) developed a method for determining the lactose and sucrose contents of ice cream mix. The method is based on measuring the freezing point depression resulting from incubating samples with invertase and @-galactosidase.Kleyn (42C)reported the results of a collaborative study of a method for enzymic determination of lactose in milk. The method was adopted official first action by AOAC. Matsumoto et al. (52C) developed an amperometric flow injection method for the determination of fructose in fruits using an immobilized fructose-5-dehydrogenase reactor. The same authors (53C) determined lactose in milk by flow injection analysis using a chemically modified lactose electrode. Lactose was determined in whey by hydrolysis with fl-galactosidase followed by oxidation of the galactose with galactose dehydrogenase, and subsequent spectrophotometric measurement of the NADH formed, as reported by Reimerders et al. (69C). Tsujisawa et al. (87C) determined lactose in milk, margarine, butter, cheese, ice milk, and milk powder by an improved enzyme assay with a reagent containing fl-galactosidase, hexokinase, glucose-6-phosphate dehydrogenase, and NADP in pH 7.5 phosphate buffer, followed by spectrophotometric measurement of NADH formed a t 340 nm. Miwa et al. (5612)reported an enzymic method for the simultaneous determination of glucose, fructose, and sucrose in foods. After glucose was measured by hexokinase and glucose-6-phosphate dehydrogenase, fructose was measured by the addition of glucose phosphate isomerase, and sucrose was successively measured by the aid of invertase. Walter et al. (93C) reported on the results of a collaborative study for the enzymic determination of glycerol in grape juice, wine, and gum drops. The method involved the use of glycerokinase, pyruvate kinase, and lactate dehydrogenase with appropriate substrates and the formed NAD was measured spectrophotometrically. A glucose sensor was developed and applied by Watanabe et al. (95C) for the determination of glucose in fish muscle and blood serum. Starch was determined in cereal grains by Aaman et al. ( I C ) using an enzymic method which includes gelatinization of starch and simultaneous partial hydrolysis using a thermostable a-amylase, complete hydrolysis using amyloglucosidase, and determination of released glucose by the glucose oxidase method. Garcia et al. (32C) compared the Fehling method and an enzymic method (using aminoglucosidase and glucose oxidase/peroxidase) for starch analysis in meat products (sausage). Both methods were equally accurate but the specific enzyme method gave greater precision. The Fehling method, as adopted in official regulation, was not useful for analysis of samples with less than 2% starch. Holm et al. (38C) enzymically determined starch in raw wheat and cereals. A method was described by Karkalas (40C) for the determination of native and modified starch in a variety of foods, and Yasui (1OOC) determined maize starch in glutinous rice cake by MS 13C/'*C isotope ratio. Walter (92C) reported the results of collaborative study for the enzymic determination of starch in foods; the method has been adopted 222R
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by the Swiss Official Methods Committee. Beach et al. (8C) used a paper chromatographic method for the separation and quantitation of minor nonabsorbed sugar (lactulose) and nonabsorbable oligosaccharides. Betschart et al. (9C) analyzed lactose hydrolysis products by HPLC on a sugar PAK-1 column with water as mobile phase. Cai et al. (18C) determined mono-, di-, tri- and polysaccharidesin honey, beets, grapes, sweet wine, and wort by HPLC on a WBondapak carbohydrate column with aqueous acetonitrile as mobile p aye. A Hypersil5 amino column with aqueous acetonitrile, and infrared (IR) detector were used by Cirilli et al. (19C) for sugar determination in molasses, honey, fruit juices, and other food substances. Deifel (22C) reported a TMS-GGFID method for the determination of sugars in honey. Goetz (34C) determined carbohydrates in dietetic nonalcoholic beverages by HPLC on an HPX-87A cation-exchange column with 0.01 N sulfuric acid as mobile phase; glucose at low concentrations could be analyzed in the presence of 250-fold fructose concentrations. Grossi et al. (35C) reported on results of comparative determinations of sugar in wheat flour by GLC and HPLC and indicated close correspondence between results of methods. Hughes et al. (39C)used HPLC to determine fructose, glucose, and sucrose in cabbage as well as residual sugars and mannitol in sauerkraut. Senkalszky et al. (78C) described a TLC method for the determination of sucrose, raffinose, and stachyose in leguminous plants. The sugars were extracted by refluxing with ethanol and were separated on Polygram cel300 layers using propanol-ethyl acetate-water (6:1:3) as mobile phase. Quantitation was by densitometry, following spot visualization with cy-naphtholin phosphoric acid. Knudsen (43C)developed an HPLC method for the determination of sucrose, raffinose, and stachyose in leguminous seeds as soybeans, chick peas, garden peas, and red kidney peas using a LiChrosorb NH, column, a 35% water in acetonitrile as mobile phase, and as interference type refractive index (RI) detector capable of detecting as low as 10 ng of oligosaccharides. Kobayashi et al. (442)separated amylose and amylopectin components of starch by size-exclusion HPLC on a two-column system with dimethyl sulfoxide as mobile phase. The method proved useful to monitor the purity of amylose and amylopectin preparations and to rapidly estimate the amylose/amylopectin ratio of starch samples. He et al. (36C)determined amylose in defatted rice grains by amperometric titration. Glucose and sucrose in soft drinks, breakfast cereal, and cake mix were determined by Koerner et al. (45C) by chemiluminescenceflow injection analysis using enzymatic conversion and a microporous membrane flow cell. Kunerth et al. (46C)modified the anthorne, carbazole, and orcinol reactions used for the quantitation of hexoses, uronic acids, and pentoses, respectively, to improve sensitivity in the analysis of unavailable carbohydrate (fiber). Lercker et al. (49C) analyzed royal jelly for its content of glucose, fructose, and sucrose by high-resolution gas chromatography (HRGC) of the sugar-TMS derivatives on a short capillary column with SE-52 stationary phase fiim and helium as carrier gas. Mardal et al. (51C) developed a procedure for the determination of sugar content in beets using a nontoxic clarifying agent (calcium oxide and aluminum oxide) instead of lead acetate. The sugars and organic acids in the pulp of Keitt mangoes at various stages of ripeness were analyzed by HPLC as was reported by Medlicott et al. (54C). The major sugars were identified as glucose, fructose, and sucrose. Molnar-Per1 et al. (57C) analyzed soybean soluble saccharides up to pentasaccharides by TMS-GC. Nebytov et al. (58C) determined 14 sugars in sweet pepper, plum, tomato, and strawberry. Extraction of sugars with water was followed by HPLC analysis using a hydoxylated silica gel column with adsorption modified by piperazine, aqueous acetonitrile as mobile phase, and an interference refractive index detector. Ohtsuki et al. (59C)determined free sugars in the hydrolyzates of water-insoluble substances of orange juice, brown sugar, rice bran, jam, roasted soybean flour, adzuki paste, and corn meal and glucose, galactose, and fructose in kiwi fruit (60C) by HPLC using an anion-exchange column with 0.2 M borate buffer (pH 8.4) and 0.7 M borate buffer (pH 8.7) for stepwise elution of disaccharide and monosaccharides, respectively, and by postcolumn reaction with 2-cyanoacetamide at 280 nm.
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The determination of carbohydratesin food by ion exchange HPLC of their borate complexes and postcolumn reaction was also discussed by Reimerders et al. (71C). The same authors (72C) described an HPLC method for the analysis of lactulose and epilactose in milk and milk products after heat treatment in the presence of high levels of lactose arid other sugars. The method is based on the separation of the sugar borate complexes by anion-exchange chromatography using two optimized buffer systems. Ion exchange HPLC on sugar-PAK1 column and distilled-deionized water containing 0.1 % calcium acetate as mobile phase was employed by Melton et al. ( 5 5 0 for the analysis of sugars in apple juice. Ruggeri et al. (73C) determined sugars, particularly lactose in human milk substitutes, by defatting with hexane, centrifuging, filtering, and chromatographing an aliquot of the aqueous phase on a Micropak NH2-10 column with acetonitrile-water (8020). Valdehita et al. (89C)separated sugars from milk preparations by TLC and determined them by in situ densitometry. The results of a collaborative study on an HPLC method for the determination of lactose purity using fructose as an internal standard were reported by Saucerman et al. (74C). The method has been adopted official first action by AOAC. Shidlovskii et al. ( 8 0 0 colorimetrically determined lactose content in sodium caseinate by precipitating casein with acetic acid in the presence of sodium acetate, reacting casein-free filtrate with phenol, and measuring the phenollactose complex at 490 nm. Simon et al. (81C) evaluated 18 methods to quantitate reducing sugars in carrots by paper chromatography;reducing sugar determination with dinitrosalicylic acid was rapid and correlated very well with values obtained by HPLC. An automated colorimetric method for the determination of glucose, fructose, and sucrose in fruits, vegetables, and fermentation liquors was described by Tawfik et al. (850.The method uses p-hydroxybenzoic acid hydrazide and 2-thiobarbituric acid as color reagents for the determination of total reducing sugars and fructose, respectively. Zheng et al. (101C) partially purified reducing sugars of soy sauce by using acidic alumina column chromatography,diluting with water, and determining them by measuring color produced by reaction with 3,5-dinitrosalicylic acid at 475 nm. Xie et al. (99C)used 3-hydroxy-2-naphthoic hydrazide as a precolumn UV derivatizing reagent for the determination of sugars in honey by HPLC on an amino-bonded column using aqueous methanol as mobile phase. The carbohydrate composition of tea plant honey samples was determined by Zhu et al. (102C) using HPLC, GC, activated charcoal column chromatography, paper chromatography, and mass spectrometry. Paynter et al. (61C) evaluated an ion exchange HPLC system for measuring glucose content in foods, beverages, bakery waste, and waste syrup by comparing the data with results form the glucose oxidase assay system. Sugars in raw and baked potato were determined by Picha (63C) employing an ion exchange HPLC method with RI detector. U et al. (88C) determined sugars in mandarin juice by fractionating sample extracts using C18 Sep-PAK cartridges followed by chromatography on a pBondapak amine column using aqueous acetonitrile as mobile phase and detection by RI. HPLC on mixed cation-exchange resins was employed by Van Riel et al. (9OC) for the separation of mono-, di-, and trisaccharides mixtures. Watanabe ( 9 5 0 described an HPLC method for determining reducing carbohydrates in fruit juices by an amino-bonded column with aqueous acetonitrile as mobile phase and amperometric detection using copper bis(phenanthroline) as postcolumn reagent. Tamate et al. (84C) determined glucose, fructose, sucrose, maltose, and raffinose in sweet potato and taro by 13C NMR and HPLC. Sugars in hydrolyzed commercial food gums were determined by TMS-GC using @-D-glucopyranosideas an internal standard as reported by AL-Hamzi et al. (2C). Angelini et al. (3C) detected, identified, and determined some vegetable gums, by hydrolyzing with 2 N trifluoroacetic acid in 80% ethanol and reducing the liberated monosaccharides with sodium borohydride to the corresponding sugar alcohols which were determined by GC of their acetate derivatives on a column of 3% SP 2330 on Supelcoport. A method for the rapid determination of galactose containing thickeners in meat products was reported by Bauer et al. (7C)which is based on acid hydrolysis of samples under increased pressure and
subsequent enzymic determination of liberated galactose. Bettler et al. (1OC) determined mixtures of gellin and thickening agents in foods by electrophoresis on s i l y l a d glass fiber paper. A gas chromatographicmethod was evaluated by Lawrence for the determination of food grade gums in dairy et al. (480 products, salad dressings, and meat sauces. Scherz (75C) described a qualitative and semiquantitative method for determining alginates in foods whereby the polysaccharide is hydrolyzed by methanolic HC1 and hydrolysis products were separated by TLC and visualized by the uronic acid specific naphthoresorcinol-HC1 reagent. The same author (76C, 77C) separated polysaccharide thickening agents by thin-layer electrophoresis on plates coated with octanol and borate buffer. Sjoberg et al. ( 8 2 0 reported a method for the identification of food thickeners by pyrolysis GC and capillary GC/MS. Thier (86C)identified and quantitated natural polysaccharides in foodstuffs by capillary gas chromatography of methylglycoside silyl derivatives. Englyst et al. (WC)determined non-starch polysaccharides in cereal produts by GLC of constituent sugars. Faulks et al. (26C) described a procedure for the determination of nonstarch polysaccharidesin foods whereby starch is removed by treatment with heat-stable a-amylase and resistant starch by treating with dimethyl sulfoxide and amyloglucosidase followed by colorimetric measurement of total neutral sugars and uronic acids in the acid hydrolyzates of the starch-free material. Forni et al. (29C)reported a method for determining the methoxy number of pectins. Pectin was treated with NaOH and the liberated methanol is GC-FID using a Porapak Q column packing and N as carrier gas. Petrzika et al. (62C) reported a method for quantitative determination of the monomers of pectins. Various pectin preparation were hydrolyzed and trimethylsilyated and monomer derivatives analyzed by GC-FID on a column of 3% OV-17 on Chromosorb WHP using phenyl-/3-D-glucopyranoside as internal standard. Voragen et al. (91C) investigated the analysis of pectins as the anhydrogalacturonic acid (AGA) content by ion-pair HPLC of the degradation products resulting from enzymic hydrolysis. Wedlock et al. (97C) reported a new colorimetric assay for pectins using 2-thiobarbituric acid as color reagent. Wang et al. (94C) examined the chemical method for the estimation of available carbohydrates in foods from plants. The results were comparable with the bioassay method. Wenlock et al. (98C) reported an improved fractionation method for determining dietary fiber values using a mixture of amyloglucosidase and a-amylase to digest starch; the fiber components found in 138 cereal and cereal-containing meat products were given. Baker (5C) used near-IR reflectance spectroscopy to determine fiber, starch, and total carbohydrates in potato chips, corn chips, extruded snacks, popcorn, cracker, and pretzels, while Baker et al. (SC)used two computerized scanning near-IR reflectance instruments to determine total sugar content in ready-to-eat breakfast cereals. Near-IR spectrometry was used by Giangiacomo et al. (33C) to determine glucose, fructose, and sucrose in aqueous mixtures at 10, 25, and 40% total sugars. Lanza et al. (47C) applied near-IR spectroscopy in the transmission mode to predict the total sugar content of a variety of juices.
COLOR Amakawa et al. (ID) partitioned oil-soluble natural dye extracts between hexane and ammonium hydroxide. The hexane fraction was analyzed for @-carotenecontent using normal-phase HPLC, and the aqueous fraction components, curcumin, norbixin, and bixin,were resolved on a Zorbax ODS column. Ushiyama et al. (11D) fractionated natural oil-soluble dye extracts from prepared foods using silica gel chromatography and further resolved the three fractions by TLC. @-Carotene, capsaicin, bixin, curcumin, chlorophyll, Cu chlorophyll, norbixin, Na Cu-chlorophyllin, and Na Fechlorophyllin were detected with TLC. Synthetic dyes were extracted from soft drinks and lemonade syrups using the ion-pairing agent trioctylamine by Puttemans et al. (9D). After back extration into aqueous sodium chlorate, the samples were analyzed by reverse-phase "PLC. The artificial dyes ANALYTICAL CHEMISTRY, VOL. 59, NO. 12. JUNE 15, 1987
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Amaranth, carmine, Lemon yellow, Sunset yellow, indigo, and Brilliant Blue were similarly analyzed using reverse-phase HPLC by Ye et al. (130). Nanogram detection was achieved by using 190 nm. Kamikura et al. ( 4 0 )analyzed the natural colors crocin and crocetin in gardenia fruit by reverse-phase HPLC. A variety of natural pigments and synthetic dyes including carmine, amaranth, Sunset yellow, Brilliant Blde, indigo monascus color, safflower yellow, betainin, and laccaic acid were resolved and quantitated by TLC on polyamide and polyamide-silica gel G mixtures by Yang et al. (120). Kanda ( 5 0 )adsorbed water-soluble natural pigments on polyamide, then further resolved the compounds by TLC on polyamide plates. The pigments analyzed included enocyanin, safflower yellow, lac dye, cochineal, betarin, gamboge, Cu Na chlorophyllinate, and Monascus dye. A method for quantitative extraction of synthetic water soluble dyes from aqueous sources with 0.1 M quinine in chloroform in the presence of 0.5 M boric acid was developed by Kobayashi et al. (70). Twenty-one dyes, including 11 azo, 5 triphenylmethane, 4 xanthene, and 1 naphthol derivative, were tested. Yin et al. (140) resolved water-soluble food dyes by ion-pair reversephase TLC using silica gel G plates treated with phenyltrichlorosilane and several ion pair reagents: Me4NBr, EMNBr, Bu4NC1, or hexadecylbromopyridine. Khachik et al. ( 6 0 )separated three classes of natural pigments, xanthophylls, chlorophylls, and carotenoids, from vegetables by using reverse-phase HPLC. Cis-trans isomers and other within-class components were resolved. @-Carotene, xanthophylls, and pheophytins were detected by spectrometry at 451,447, and 667 nm, respectively, after fractional isolation on a polyamide column by Mader and Chladova ( 8 0 ) . Chlorophyll a and b, and their degradation products pheophytin a and b, were determined in vegetable oil using a pPorasil column by Rahmani et al. (100). Anthocyanins in colored beverages were determined by sorbent extraction, separation on cellulose TLC plates, and color reaction visualization by Zloch (150). Aromatic amines, including benzidine, aniline, 4-aminobiphenyl, and 4-aminoazobenzene, were detected and quantitated in FD&C Yellow No. 5 (tartrazine) by Bailey and Bailey (20). The determination was achieved by diazotization (Rand coupling with 3-hydroxy-2,7-naphthalenedisulfonate salt) followed by reverse-phase HPLC. Scattering problems encountered in surface reflectance measurements of meat color were resolved by Iversen and Palm (30)by using an integrating sphere and converting reflectance spectra to the C.I.E. 1976 L*a*b* coordinate color system.
ENZYMES General books on enzymes include Plant Proteolytic Enzymes, edited by Dalling (7E),and Methods of Enzymatic Analysis, edited by Bergmeyer et al. ( I E ) , which cover methods for peptidases, proteinases, and their inhibitors. a-Amylase and P-amylase of Tritical flour were separated by affinity and hydrophobic chromatography and assayed spectromphotometrically with p-nitrophenylmaltoheptoside substrate by Carlsson et al. (4E). Finney (1OE)modified the falling number test to quantitate a-amylase in wheat flour. A procedure was developed for the determination of fungal a-amylase additives in wheat flour by Van den Noortgaete (28E)using the viscosity attained in a Brabender amylograph as a measure of amylase activity. Taeufel et al. (27E) found the S-tablet test (Sofa test) to be simple, rapid, and accurate for determining a-amylase in ceral products. Cinco et al. (6E) described a procedure for the isolation and determination of a-amylase inhibitors in white and red kidney beans and determined their heat stability. A rapid procedure and the equipment required for the assessment of preharvest sprout damage of cereal grains was described by Jensen et al. (16E) who proposed the method as a basis of a grading system that reflects the distribution of enzyme activity among individual grains. Demmer and Werkmeister (9E)differentiated fresh and thawed pork by determining the presence of the enzyme (3hydroxyacyl CoA dehydrogenase (NADH). Two methods for distinguishing between fresh and frozen thawed liver were described by Gottesmann and Hamm (13E);in one method the released HADH activity is measured photometrically by means of an enzyme test and in the other by means of a simple color reaction. A spectrofluorometric procedure using 4224R
ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
methylumbelliferyl esters as substrates was developed for the determination of low lipase activities in foods by Haslbeck et al. (14E). Linfield et al. (18E)developed a new method for lipase activity using olive oil as the substrate with periodic sonication. The determination of lipase activity and free fatty acids of milk using colorimetric automatic titration was proposed by Cartier et al. (5E). McKellar and Cholette (20E) modified the method for determining the extracellular lipases of Pseudomonas fluorescens based on hydrolysis of 6-naphthyl caprylate and photometry and applied it to skim milk. A method for lipase activity from P. fluorescens was optimized by Paquette and McKellar (24E)using a super/simplex optimization computer program. Stead (26E) developed a fluorometric method for the determination of P. fluorescens lipase using the fluogenic substrate 4-methylumbelliferyloleate and adapted it for skim milk powder, whey powder, and whey protein concentrate. A fluorometric assay of lipase in rice bran was developed by Saunders and Heltved (25E) using 4methylumbelliferyl heptanoate as substrate and applied to determination of conditions for rice bran stabilization. Fretzdorff (11E) developed a method to determine lipoxygenase activity in corn, wheat, barley, and oats using an 0-selective electrode to measure the 0 uptake during the reaction. Kwee (17E) described an improved method to determine alkaline phosphatase based on a photometric method which is applicable to colored products and a wider variety of milk products. Methods of sample preparation for detecting alkaline phosphatase in casein were studied collaboratively by Murthy and Peeler (21E); the alternative rapid sample preparation method was adopted official first action by the AOAC. Paggi et al. (22E) developed a colorimetric method for the determination of peroxidase in milk using H,Oz and the Rothenfusser reagent. Wasserman and Wagner (29E) described a rapid colorimetric peroxidase assay to determine blanch efficacy in green beans. A method to determine proteinase from P. fluorescens P1 by an enzyme-linked immunoassay technique was described by Birkeland et al. (2E)and it was found to offer the combination of sensitivity and specificity for the detection of these enzymes in milk and dairy products. Paggi et. al. (23E) determined protease activity in milk samples by incubation with NaN3 followed by the addition of TCA, filtration, and treatment with fluorescamine for fluorometric detection. Fukal et al. (12E)reported the residual activity of partially inactivated papain is markedly dependent on the substrate and increased as the relative molecular weight of four tested substrates decreased. The residual pepsin and chymosin activity in cereal was investigated by Majeed and Ernstrom (19E)using different extraction procedures and assay by a linear agar diffusion method. Herrmann and Krause (15E) described the apparatus and method to determine the activity of rennet preparations by measuring change in viscosity of a solution containing casein. An assay technique for quantifying milk-clotting enzymes in milk and whey solutions without prior removal of casein was described by Carlson et al. (3E). Yada and Nakai (30E) investigated the relation between physiochemical properties and enzymic activity (milk-clotting to proteolysis activity ratio) of aspartic proteinases by using the mltivariate statistical technique known as principal component analysis. A method for the quantitative determination of trypsin inhibitor in vegetables and meat products was described by DePalozzo and Callejas @E), who suggested the possibility of applying it for the determination of soybean added to food.
FATS, OILS, AND FATTY ACIDS Analysis of Fats and Oils, a book edited by Hamilton et al. (GF), is recommended to the fats and oils analyst for review and reference. Several review articles have been also published. Arens et al. (7F) published a survey where methods are described in detail for determining soap and phosphatide residues in refined oils. Christie et al. (24F) published a review on recent developments in lipid analysis, and a review on rapid methods for the quality control of edible oils was published by Frega et al. (47F). Goh et al. (56F)reviewed the minor constituents of palm oil, and a review and discussion on simple chemical and physical methods for measuring flavor quality of fats and oils was published by Gray (60F).Guan et al. (62F) presented
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a review on effects and anal sis of secondary lipid oxidation products, and Homberg (72h authored an article on studies of sterols in foods, discussing the isolation of lipids and sterols from foods, the use of sterol determination in food research, and the sterol content of some plant and animal fat. A review on nondestructive monitoring, application of techniques as IR and NMR spectroscopy in monitoring meat and meat products, discussing lipid and protein determination in meat by NMR, and lipid, protein, and moisture determination by IR spectroscopy, was published by Kopp et al. (94F). TLC and GC procedures for separation and characterization of unsaponifiable matter in vegetable oils were published by Lercker et al. (103F). Luf (108F)published a review on analysis of fatty acids. Monacelli et al. (126F)reviewed the advances in fat analysis with emphasis on GC, NMR, and HPLC. Organoleptic analysis of flavors by physicochemical methods was the subject of a review by Mordret et al. (129F). Reineccius (149F)published on isolation, separation, and characterization of flavor compounds in lipids. Schiefer et al. (15IF)reviewed the enzymic-spectrophotometric methods of determination of phosphatidylcholines in biological materials, e.g., amnistic fluids and blood, and of lecithins in foodstuffs. Sehwarz (158F)published a review on methods for determining fatty acids and glycerides in foods, the physical properties of fats and their sterol content, and the determination of the degree of fat oxidation. The methodologies used to determine geometric (cis-trans) and positional isomers of unsaturated fatty acids in fats and oils were reviewed by Strocchi (117F). Totani (1830reviewed the microquantitation methods for determination of lipid peroxides in foods, especially vegetable oils. Methods including TBA test, cyclooxygenase procedure, glutathione peroxidase method, chemiluminescence, GC, HPLC, and TLC-FID methods for determining lipid peroxides were discussed. Usuki (186F)published a review on relations between chemiluminescence and peroxide, acid, carbonyl, and iodine numbers in thermally oxidized and autooxidized edible oils. Ward (1938')presented a review on the use and limitation of TBA assay in estimating lipid oxidation in food. Yunusova et al. (204F.lpublished a review on methods of stereospecific analysis of foods for determining the molecular structure of glycerides and phospholipids. Spectrophotometric methods for analysis for glycerides, fatty acids, and their derivatives by use of carbon-13NMR were reviewed by Zimniak (206F). Athnasios et al. (9F)published a method on the determination of cis,&-methylene interrupted polyunsaturated fatty acids in fats and oils by capillary GC on a 60M SP 2340 capillary column. Gas chromatographic results agreed well with those obtained by an enzymic lipoxygenase method. Bannon et al. ( I O F ) determined the composition of fats with fatty acids containing four or more carbon atoms by gas chromatography of fatty acid methyl esters (FAME); the optimum method of methylation was discussed. Aldolf et al. (2F)authored a paper on the isolation of w3-polyunsaturated fatty acids and methyl ester fish oils by silver resin chromatography. Boniforti et al. (17F)determined positional and geometric isomers of unsaturated fatty acids commonly found in vegetable oils by converting the methyl esters of fatty acids to epoxides with rn-chlorobenzoic acid, followed by capillary GC-MS. Cao et al. (20F)determined palmitic, oleic, linoleic, linolenic, arachidonic, and erucic acids in rapeseed by GC-FID of their methyl esters. Conway et al. (27F)used hydrazine to hydrogenate the double bond of cyclopropenoic fatty acids of seed oils without cleaving the cyclic system and with minimum effect on the degree of unsaturation of the remaining double bonds prior to GC analysis of methyl esters. Gas chromatographywas used to analyze the fatty acids of hazelnut oil as reported by Demirbas (36F).Dupuy et al. (37F)used direct sampling capillary gas chromatography for determining volatiles and flavors of vegetable oils. Gere et al. (54F)determined cyclic fatty acids formed during heating of sunflower and rape oils by GC-FID of their methyl esters on Carbowax 20M with hydrogen as carrier gas. Gildenberg et al. (55F) reported the results of an international collaborative study of a gas chromatographic method for determination of trans unsaturation in margarine. Coefficients of variation were consistently better for the determination of total trans acids by GC vs. IR analysis.
The method has been adopted offical first action by AOAC. Hibino et al. (68F)reported on the analysis of fatty acids in concentrated polyunsaturated fatty acid fish oil by using diethylene glycol succinate (DEGS) packed column. Overlaps of Me ester polyunsaturated fatty acid peaks when using DEGS column were resolved by GC-MS and by GC on a Carbowax 20M capillary column. Hibino et al. (69F)reported the results of a collaborative study for the determination of eicosapentaenoic (IPA) and docosahexaenoic (DHA) in polyunsaturated fractionated fish oil. Homer (73F)described methodologies for the capillary gas chromatography of milk fat and fatty acids and compared (740 GC methods for the determination of fatty acid methyl esters and sterols in milk fat and modified milk fat with other methodologies. Gas chromatographic methods yielded valid estimates of total polyunsaturated fatty acids in milk fat compared with lipoxidase methods and trans fatty acid value in milk and butter compared well with data obtained by IR spectrometry. Kawai et al. (89F)determined the fatty acid composition of butterfat, margarine (containingmilk fat), and coconut oil by GC of their methyl esters; short-chain (c&3 and C16J fatty acid methyl esters were measured by temperature-programmed GLC on a 15% OV-275 column and long chain (c&24) by isothermal GLC on a column of diethylene glycol succinate. A comparison of two standard titrimetric procedures for determination of free fatty acids content in oils extracted from oilseeds and vegetable oils was Kroll et al. (98F)reported on the done by Kershaw (WF). results of a collaborative study on a FAME-GC method for determining combined and free monomeric fatty acids in refined soybean oil, used frying fats, and two oil mixtures. trans-Octadecenoate and trans-9-trans-12-octadecadienoate were analyzed by Lin et al. (105F) in fresh lean and fatty tissues of pork and beef by argentation TLC and capillary GC. Magak'yan et al. (11OF)determined chanakh cheese fatty acids by GC. Plamitic, myristic, stearic, and lauric acids were the predominant saturated fatt acids and oleic, linoleic, linolenic, and dodecadienoic aci s were the predominant unsaturated acids. Mallet et al. (111F) studied derivatization techniques for improving the separation of fatty acid esters by capillary GC, by modifying the carbon chain properties by addition reactions on the double bonds. Matsui et al. (120F)identified fatty acids in human blood serum and in soybean and colza oils by determining the equivalent chain length (ECL) values of C14-22 fatty acid esters using various glass capillary columns. Misir et al. (124F) proposed and evaluated a rapid transesterification method for the preparation of fatty acid methyl esters (FAME) for gas chromatographic analysis using tetramethylammonium hydroxide in methanol and compared it with conventional estrification methods for a variety of vegetable and animal oils and fats. Better recoveries of low chain fatty acids (e.g., C4) and also for unsaturated C1 fatty acid isomers where achieved when the rapid methoi was employed. Moneam et al. (127F)analyzed total fatty acids extracted from S. terebenthifolius berries with light petroleum, diethyl ether, or CHC1,:MeOH (2:l) by FAME-GC-FID. Pyrolysis-GC analysis was used by Nazer et al. (136F)as an identification method of fats and oils. Pyysalo et al. (146F)reported capillary GC methods coupled with detection by mass fragmentation and retention index monitoring (RIM) for fat analysis. A rapid method for the determination of double bond positions in monounsaturated fatty acids by GC-MS was reported by Shibahara et al. (162F).Strocchi et al. (176F) determined unsaturation in hydrogenated soybean and palm oils and in margarine oil by GC on a 15% OV-275 on 100-120 mesh Chromosorb P AW/DMCS at 220° and nitrogen as carrier gas. Stack et al. (174F)developed a capillary GC-FID method for the simultaneous quantification of fatty acids (as methyl esters) and sterols (silyl esters) in orange juice. Spangelo et al. (173F)determined individual free fatty acids in milk by GC-FID using a column of 10% SP-2330 on Chromosorb W. Sumimoto et al. (179F)described a capillary GC-FID method for determination of fatty acids in food preparations including fish, meat, and eggs, oils and fats, and beans, milks, grains, and confectionary products. With the exception of beans, C14*, CIS,., C~?:O, C18:1, C y , . and were detected in all food preparations. In ad ition C2a4, C2a5,and C22:6were detected
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in fish but were absent or present only in trace levels in other food preparations. Takagi et al. (181F)analyzed soft margarines for their fatty acid content using capillary GC of fatty acid methyl esters. The content of the geometricaland positional isomers of oleic acid was determined by GC of the ozonolysis products of the cis and trans monoenoate fractions, separated by argentation silicic acid TLC. Tsuda et al. (185F)described a method for GC determination of sorbitan fatty acid esters in confectionmy products as sorbitan monostearate. Erucic acid content in rape oil was determined by Wang et al. (19lF)by FAMEGC-FID on columns of QF-l,OV-17, or SE-30. Yamazaki et al. (2OIF) determined erucic acid in rapeseed by near-IR reflectance spectroscopy. Woo et al. (196F)described modified techniques for improved GC quantification of free fatty acids in dairy products. Zhou et al. (205F)analyzed free fatty acids of several vegetable oils by capillary GC of fatty acid methyl esters on a column coated with cross-linked methyl silicone. IUPAC commission on oils, fats, and derivatives (83F)published the results of two collaborative studies for the determination of butyric acid in butter fat alone or blended with other fats. Recseg et al. (1480 determined fatty acid trans isomers in margarine and hydrogenated rape oil by GC on packed columns of OV-275 or Silar 1OC. The results agreed well with those by a standard IR spectrometric method. HPLC preparative separation of milk fatty acids as their methyl derivatives was reported by Christie et al. (25F) with satisfactory resolution of C4-Cl8 fatty acids esters using LiChrasorb 10 RP column with isocratic elution with MeCNH20 (955) as mobile phase. Hirata et al. (70F) reported on the analysis of free saturated, unsaturated, and branched fatty acids by reversed-phase HPLC with MeOH containing 1% phosphoric acid as mobile phase and low UV detection. Hwang et al. (78F) used HPLC for quality evaluation of sesame oil. Kihara et al. (91F)described a simple precolumn saponification and esterification reactor for preparation of phenacyl, p-bromophenacyl, or 2-naphthyl esters of fat and oil fatty acids prior to HPLC analysis. Lu et al. (107F)determined fatty acid composition in rapeseed oil during hydrogenation by HPLC on Nucleosil C18,5pm, and MeCN as mobile phase. Matsumoto et al. (121F)reported a micro liquid chromatographic system directly coupled to a quadrupole mass spectrometer through a vacuum nebulizing interface that was applied to the analysis of free fatty acids of bean oil, rape oil, palm oil, and milk fat. Netting (137F)presented a one-pot procedure for the saponification of fats and oils, and the subsequent estrification of the resulting fatty acid salts with pentafluorobenzyl bromide followed by the separation of the pentafluorobenzyl esters primarily on the degree of unsaturation by normal-phase HPLC. Ritchie et al. (151F) used normal-phase HPLC to separate lipid classes as was exemplified by separation of methyl ricinoleate, ricenoleic acid, and ricinoleyl alcohol and fractionation of cocoa butter and superglycerinated partially hardened rape seed oil. Robinson et al. (152F) compared RI, UV, and mass detectors for HPLC analysis of glyceride mixtures. A new double column HPLC method for rapid separation of fatty acids (C12-C22) was published by Sat0 (156F).Vioque et al. (189F) separated free fatty acids by RP-HPLC after conversion to p-phenylazophenacyl esters. An HPLC method was developed by Wood (197F)for the analysis of seed oils containing cyclopropene fatty acids after hydrolysis and conversion of the acids to phenacyl derivatives using a two-column system that allowed the resolution and quantitation of malvalic, sterculic, and dihydrosterculic acids as well as other fatty acids in cottonseed and sterculia foetiola oils. Yabe et al. (198F) determined gossypol in edible cottonseed oil by HPLC on a Hypersil M 0 5 column with MeCN-N20-THF (8018:2), pH 2.5, as mobile phase and UV detection in 235 nm. Lipid fractions (phospholipids, sterols, glycerides, and free fatty acids) were determined in lipids from grill and frozen fish by a method combining separation with a hexane-chloroform-ether-potassium acetate (85:15:17:1) as a mobile phase and flame ionization detection (FID). Analyses were performed on an Iatroscan analyzer using silica gel coated chromatorods. For separation of saturated and unsaturated triglycerides, chromatorods impregnated with silver nitrate and mobile phase of CHC1,-benzene-acetic acid (10:90:1) 226R
ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
system were used. Samples were applied to chromatorodsand organic components were pyrolyzed in hydrogen flame, recorded, and calculated automatically, as reported by Pisareva et al. (142F).Ratnayake et al. (147F) also used Iatroscanthin-layer chromatography-flame ionization detection for the rapid analysis of canola gum lipid composition. Sebedio et al. (159F)quantitatively analyzed the methyl esters of fatty acids geometrical isomers and of trilgycerides differing in degree of unsaturation by Iatrascan TLC/FID using silver nitrate impregnated rods. Fraser et al. (44F)detected chlorophyll derivatives in soybean oil using reversed-phase HPLC. Antioxidants in tallow and vegetable oils were determined by Indyk et al. (79F) by normal-phase HPLC with UV detection at 280 nm. Wei et al. (194F)determined BHA, BHT, and PG in oil fat and food by TLC and GC. Maruyama et al. (117F)separated and quantitated underivatized saturated and unsaturated monoacylglycerols by reversed-phase HPLC and UV detection at 210-215 nm. Ascorbyl palmitate was determined in vegetable oil and lard by reversed-phase HPLC and UV detection by Vicente e t al. (188F). Cholesterol was determined by Arai et al. (5F) using an integral multilayered analysis element. Hurst et al. (77F) presented an HPLC method for the determination of cholesterol content as an indicator of egg solids. Kou et al. (96F) described a method for the determination of 25-hydroxycholesterol in a wide range of materials including foods. Lipid extracts were initially purified on octadecyl silicic acid cartridges and by reversed-phase HPLC before quantitation by normal-phase HPLC on a silicic acid column and a variable wavelength detector. 25-Hydroxycholestero1was not detected in lard, cream, fresh egg yolk, or spray-dried egg yolk powder but was detected and its identity confirmed by mass spectrometry in egg yolk powder after heating at l l O o for 4 days. Maerker et al. (109F)determined a number of standard cholesterol oxides by direct on-column GC (5% phenylsilicone-coatedcapillary column with temperature programming) with good resolution, recommending its use to measure these oxides in foods. Fischer et al. (40F)determined oxycholesterols in various foods by GC and in foods of animal origin by GC-MS (410. Masoom et al. (118F)described a method for determination of cholesterol by flow injection analysis with immobilized cholesterol oxidase and hydrogen peroxide produced was detected amperometrically. Masson et al. (119F)determined cholesterol in butter by rapid saponification with KOH and elution of the unsaponifiable fraction from a Celite 545 column with chloroform followed by silylation and GC on a column of 3% SP-2250 on Supelcoport (100-120 mesh) at 245O with FID. Mordret et al. (128F)developed a GC method for the determination of cholesterol in fats and oils and in margarine using cholesterol as internal standard. C-7 oxidized cholesterol derivatives (C-7 OCDs) in muscle and other foods were determined by Park et al. (138F)without saponification by chromatographing the total lipid extracts on silica gel to concentrate trace sterol oxides from triglycerides, cholesterol, and phospholipids. Sterol oxides in eluates were determined by normal-phase HPLC on a pPorasil column with 7% 2propanol in hexane, detecting 7-ketosterols at 233 nm and 7-a-hydroxycholesterol at 208 nm. Recoveries of C-7 OCDs added to beef approached 100%. Pancake mix, french fries, raw beef, fried chicken, cooked hamburger, beef jerky, and liver sausage were analyzed. Sugino et al. ( I 78F) developed a method for the determination of cholesterol epoxides as the p-nitrobenzoate derivatives in spray-dried egg products using reversed-phase HPLC. Bianchini et al. (13F)reported on the determination of sterol and triterpene alcohol acetates in natural products by reversed-phase HPLC and GC-MS. Brumley et al. (19F) identified sterols in vegetable oils by capillary GC-MS-E1 of sterol butyrate esters and determined them by packed column GC-FID. Chaouch et al. (21F)determined tocopherols in peanut, corn, olive, soybean, and sunflower oils by HPLC and by differential pulsed voltammetry. Fujimoto et al. (48F)determined sterols in edible oils by reversed-phase HPLC and UV detection at 205 nm. IUPAC commission on oils, fats, and derivatives (81F,82F)published two papers on the determination of total sterol in fats and
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oils. Gracian Tous et al. (59F)described a method developed by collaborative study for the determination of erythrodiol in vegetable oils and the separation of eight structurally closely related sterols on C8 and C18reversed-phase columns with UV detection at 206 nm was reported by Holen (71F). Hortsmann et al. (75F) described a rapid method for isolation of sterols from plant and animal fat and oils and for determining the content of these fats and oils in foods. Jonker et al. (85F)reported an improved method for determination of free, esterified, and glycosilated plant sterols in foods. A method for the detection of sterol epoxides in foods by colorimetric reaction with picric acid was reported by Lee et al. (IOIF). Mrugasiewicz et al. (131F)analyzed sterols in corn by extraction with chloroform and determination at 615 nm after reacting with the Liebermann-Burchard reagent. Nasirullah et al. (134F)reported a TLC method for the analysis of unsaponifiable matter of edible and nonedible seed oils. Naudet et al. (135F)reported on a new official procedure (IUPAC 2.404) for sterol determination in plant or animal lipids. Separation of triglycerides and hydrocarbons from seed oils by HPLC with IR detection was reported by Bhati et al. (12F). Triglycerides of C,-C, of cocoa butters from different parts of the world were separated by GC by Chaveron et al. (23F). Christopoulou et al. (26F)used a high-performance size exclusion chromatographic method for the separation and quantitation of fatty acids and mono-, di-, and triglyceride mixtures. Separation was achieved on two columns packed with 5-pm styrene/divinylbenzene copolymer and connected in series, using toluene as eluent, and components were monitored by refractometry. Fiebig (38F) reported reversed-phase HPLC method for triglyceride separation on LiChrosorb RP18 with propionitrile as mobile phase. Frede (46F)described factors for improving triglyceride separation by reversed-phase HPLC using propionitrile as mobile phase and RI detector. Geerarert et al. (50F)discussed several ca illary GC and HPLC methods fro triglyceride analysis inclu8ng separations by carbon number, by number of unsaturated fatty acids (within each carbon no.), and by double bond locations (ozonolysis), using reversed-phase HPLC, and presented a scheme for the analysis of chocolate fats (including cocoa butter, butter oil, cocoa butter equivalents, and vegetable oils) and for the analysis of compound chocolate. Geerarert et al. (51F,52F) reported on the capillary GC-FID analysis of triglycerides of palm, grape seed, cottonseed, soybean, olive, corn, peanut, rape, coffee, and coconut oils and of butterfat, egg yok, and chicken fat. The triglycerides were separated according to chain length, and the retention was highest with triglycerides containing the most unsaturated acids. A paper on HPLC of triglyceride determination with gradient elution and mass detection was published by Herslof et al. (67F). Kamat (86F)reported a method for the determination of mono-, di-, and triunsaturated triglyceride content of corn, soybean, and rape oils by TLC-FID. In another paper, Kamat (87F)used a TLC-FID method to quantitate dipalmitoolein, palmitodiolein, and triolein by quantitatively oxidizing them with KMn04to the corresponding azelagolycerides which were separated and determined by TLC-FID using squalene as an internal standard. Lee (102F)developed two methods for the separation of medium chain triglycerides using reversed-phase HPLC. Both methods employed C18HPLC column and isocratic elution, with a differential refractometer detector, and a UV detector a t 210 nm using Trimonanoin as the internal standard for quantitation. The method is suitable for milk, whey, and sobyean based matrices, and with minor modification, medium chain triglyceride levels ranging from 10 to 50% of total fat could be determined. The determination of the structure of glycerides in olive oil was the subject of a publication by Mariani et al. (112F). Marjanovic et al. (113F)determined triglycerides (C2-C52) in fats (cocoa butter and its substitutes and lard) by &C on short capillary SCOT (support-coated open tubular) columns and in milk fat by high-temperature GC on a 1% Dexsil3-SS column (114F). Martinez-Castro et al. (115F)used tetramethylammonium hydroxide as catalyst in the methylation of both free fatty acids and glycerides of fat prior to analysis of milk fat by capillary GC. Morisaki et al. (130F)determined
tributyltin in marine food products. Fish or shellfish was homogenized with HCl-MeOH to convert tributyltin oxide to tribyltin chloride which after fractionation using a silica gel column was derivatized to its trimethylsilyl derivative and analyzed by GC. Direct inlet system ammonia chemical ionization mass spectrometry was use by Murata et al. (132F)for analysis for triglycerides of linseed, safflower, and lettuce seed oils. A method for the quantitative determination of the triglyceride species composition of vegetable oils by reversedphase (RP) HPLC via flame ionization detection was described by Phillips et al. (141F),separations were achieved by using Zorbax ODS columns with gradient elution with methylene chloride in acetonitrile. The method was applied to butter before and after randomization, soy oil, and pure olive oil. Pocklington et al. (143F)reported on the development, by collaborative study, of a standardized method for determination of the component triglycerides of animal and vegetable oils. The procedure involves the separation of triglyceride groups containing the same number of C atoms, by direct GC of the lipid solutions on packed columns under temperature-programmed conditions. Podlaha et al. (144F)studied the triglyceride (TG) composition of 28 cocoa butter samples by HPLC. Shukla et al. (163F)separated triglycerides from cocoa butter by HPLC on two Spherosorb reversed-phase columns with MeCN-THF (7327) as mobile phase and W monitoring at 220 nm. The analysis of triglycerides in oils and fats by liquid chromatographywith laser-light scattering detector was reported by Stolyhwo et al. (175F).Toeregaard et al. (182F) separated palm oil, milk fat, and model mixtures of intact glycerides by capillary GC with OV-101 as stationary phase on the basis of their number of C atoms and on the number of unsaturated fatty acid in the triglyceride molecule. Wada et al. (19OF)reported on triglyceride analyses of vegetable oils and animal fat by GLC, field-desorption mass spectrometry (FD-MS),and HPLC. The combination of these techniques provided significant information by which the major molecular species of triglycerides in naturally occurring fats and oils could be estimated. Yoshida et al. (203F)reported a simple and rapid method for the enzymic hydrolysis of triacylglycerols based on the enzyme deacylation of triacylglycerols on a single TLC plate followed by analysis of the hydrolytic products separated from the reaction zone by multiple development of the plate. The method is applicable to the analysis of most natural fats and oils. A semimicro method for the determination of iodine values of lipids by bromide ion selective electrode was developed by Abdel-Moety et al. (IF). Kolarovic et al. (93F)reported an on-line gas chromatographic method which allows direct calculation of iodine values of edible fats and oils. Sheeley et al. (161F)compared the determination of iodine values in commercial soy lecithin samples and lecithin standards by the AOCS official method (Wijs) and by measurement of proton NMR signals for vinylic protons and found good agreement between the two methods. Agienko et al. (3F)reported a highly sensitive thiobarbituric acid (TBA) test for predicting the resistance of fats in milk substitutes to oxidation during storage. Pokorny et al. (145F) described a modified method for determination of 2-thiobarbituric acid value in fats and oils, which utilizes 1-butanol as the sole solvent. The method was satisfactory for evaluating lard, cooking fat, soybean, sunflower, and rapeseed oils in stage of beginning rancidity. A simplified plate diffusion technique for the determination of lipid antioxidant activity was described by Araujo et al. (SF). Asano et al. (8F)described a method for the detection of lipid peroxides in foods. Inverse gas chromatography was found by Bird et al. (14F)to be suitable for study of the oxidation of vegetable oils. Blumenthal et al. (15Fj developed a method for determination of oxidized (polar) substances in fat and a new quick test for the detection and semiquantitation of alkaline contaminant material such as soap in fresh and used vegetable frying oils and animal/vegetable oil blends (16F). Bradley (18F)reported the results of a collaborative study on methods of determining milk fat. Chaveron et al. (22F) reported the results of a collaborative study on a GC method for determining vegetable fats in chocolates on the basis of variations in the triglyceride composition. Low concentrations
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of milk fat were determined by Cotton (28F) in skim milk and cream plant wastewaters using a modified procedure of Roese-Gottlieb with preconcentration of the sample. A comparative study of six analytical methods for quality evaluation of frying fats was published by Croon et al. (29F, 30F). Cruddgington (31F) reported the results of a study of the determination of fat in dried milk. Bengtsson (11F) reported that the near-iR reflectance method for determining oil content in rapeseeds was superior to the gravimetric analytical methods. Davies et al. (32F) derived equations for estimatingoil concentration in mayonnaise containing 11-75% oil in mayonnaise-based salads using near-IR. Fat content in meats (ground pork, beef, and chicken) was determined by near-IR reflectance as reported by Nagao et al. (133F). De Konin et al. (33F) reported the results of a critical study on a num%er of lipid extraction methods from fish meal. The application of proton NMR in food analysis was discussed by Defour ( 3 4 0 . Specific examples considered were the determination of the solid/liquid phase ratio in refined and hydrogenated coconut oil and the determination of total fat in chocolate. Gambhir et al. (49F) simultaneously determined the moisture and oil content in rapeseed-mustard by pulsed NMR. Guan et al. (62F) determined fatty acids in vegetable oil by carbon-13 NMR. Lambelet et al. (99F)used low-resolution pulsed NMR to determine solid content in cocoa butter and edible oils. A rapid NMR method for fat analysis (total and solid fat content) was developed by Leung et al. (104F). Patersson et al. (140F, 139F) reported a general pretreatment and measuring procedure for solid fat content (SFC) determination usin pulsed NMR on tempering fats and tempering fats in blen!s with milk fat. Low-resolution NMR w a used ~ by Renou et al. (150F)for determining fat content in meat products. Ryseva et al. (155F)determined the level of solid triglycerides in cocoa butter and in some of its commercial substitutes. Wang et al. ( 1 9 2 0 presented a new double-tube addition method for measuring the oil content of seeds and other food samples by pulsed NMR with diode detection. Phospholipid separations from vegetable oils were studied by Ajana et al. ( 4 0 by dialysis of crude oils against petroleum ether which allowed the recovery of almost all phospholipids (98%), fractionation by HPLC, and TLC. Fozy et al. (42F) described a rapid enzymic spectrophotometric method for determining lecithin in cocoa, chocolate masses, and soybean phosphatides. Goh et al. (57F)determined total phospholipids in crude palm oil using colorimetry. Analysis of phospholipids in soy lecithin by HPLC was reported by Hurst et al. (76F) who analyzed chloroform solutions of soy lecithin by HPLC usin a normal phase (pPorasi1) column and a mobile phase MeC?N-MeOH-85% H3P04(78010:9) with UV detection a t 205 nm. Ishiguro et al. @OF) used different methods to determine lecithin in food preparations including precipitation with acetone, colorimetric measurement of phosphorus, TLC, and GC. Acetone precipitation gave high results because of the presence of coprecipitated sterols and other substances while the colorimetric method gave variable resulb. TLC allowed the determination of total lecithin as well as the individual phosphatides and GC was satisfactory for soybean lecithin. Martovshchuk et al. (116F) described an apparatus for measuring the interphase tension between a vegetable oil and water. The value obtained is a measure of the hydrophilic phospholipid content of the oil and thus of its degree of refining. A method for determination of lecithin in foods by TLC separation followed by spectrophotometricmeasurement of phosphorus was developed by Senelt et al. (160F).Sotirhos et al. (170F)reported an HPLC method for soybean phospholipid analysis using a silica column, a mobile phase of hexane-2-propanol-water,and UV detection at 210 nm. The same authors (172F) used both normal-phase and reversedphase HPLC for further analytical studies of soybean phospholipids. Traitler et al. (1840 described the comparative determination of phosphatidylcholine(lecithin) species in food products by fast atom bombardment computer averaging integration spectrometry (FAB-CAI). Autoxidized fats were studied by Frankel et al. (43F) to elucidate the genesis of volatile lipid oxidation products. Thermal homolytic and acid heterolytic decomposition processes were compared using GC/MS. Gomes et al. (58F) evaluated thermal oxidation in vegetable oils following tech228R * ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
nological treatments or frying by FAME-GC. The sensory properties of volatile lipid oxidation product and methods for the determination of lipid oxidation in food were reviewed by Hall (63F). Hall et al. ( 6 4 0 studied the formation of secondary lipid oxidation products in spray-dried cream and whole milk powders by static and dynamic headspace sampling and gas chromatography. Hara et al. (6639 used reversed-phase HPLC with RI detector for the separation and determination of autoxidized ethyl oleate, linoleate, and linolenate. The hydroperoxideswere separated according to the number of double bonds and hydroperoxy groups and geometrical (cis-trans and trans-trans) configuration of double bonds, but not on the basis of position of hydroperoxy groups. Kikugawa et al. (92F) reported on the chromogenic determination of lipid hydroperoxides by reacting with sesamol dimer, in the presence of Hb. The violet-colored reaction product had an absorption maximum at 550 nm. By this method 0.1 pmol of methyl hydroperoxide could be detected with higher sensitivity than by the conventional peroxide value (POV) method. Lang et al. ( I O O F ) described a sensitive method for the determinationof the lipid peroxidation product 4-hydroxynonenal in biological samples as well as lipid-containing foodstuffs. Mikula et al. (123F) reported on reaction conditions for measuring oxidative stability of oils by thermogravimetric analysis. Headspace chromatographicanalysis of heated soybean oil was applied by Snyder et al. (168F) to determine the effect of hydrogenation and additives on the formation of total and individual volatile components. Sotirhos et al. ( 171F) used HPLC for the analysis of oxidative and polymerized decomposition products in commercial vegetable oils and heated fats. Szumilak et al. (180F)reported that precision of the iodometric method for determining peroxides in soybean was markedly improved by using potentiometric measurements. Valentova et al. (187F)determined total polar oxidized fatty acids of the fat fraction isolated from dehydrated meat and dehydrated chicken soup and of fat from frying doughnuts and from roasted peanuts by reversed-phase HPLC with RI detector. Woestenburg et al. (195F) reported the results of an interlaboratory test for examining the performance of the automated Rancimat method for determining the oxidative stability of edible oils. Yagi et al. (199F) used a methylene blue derivative for the determination of lipid peroxides in foods. Results obtained by this method coincided well with those by the iodometric method and paralleled those obtained by the thiobarbituric acid method. Yamamoto et al. (200F) detected low level lipid hydroperoxides by chemiluminescence. Deman et al. (35F) developed a new instrument for thermopenetrometry of fats, the use of which was demonstrated with butter and margarine. Fletcher et al. (41F)published a report comparing the various procedures for determining total yolk lipid content. Frede et al. (45F) studied the variation in melting and crystallization temperatures of milk fat by differential scanning calorimetry (DSC) and discussed the use of DSC for detecting foreign fats in milk fat. Gegiou et al. ( 5 3 0 reported on methodology for determining cocoa butter equivalents (CBE) in plain and milk chocolate. Grover et al. (61F) detected palas oil in ground nut and vegetable oils by analyzing the unsaponifiable fraction of fat by TLC with fluorescence detection under UV irradiation. Methods for determining glycerides and free fatty acids in butter flavoring materials were examined by Kat0 et al. (88F). GC was most suitable for free fatty acids and gel chromatography was most suitable for glycerides. Korynova et al. ( 9 % ' determined ) the butterfat content in chocolate products by determining the level of butyric acid titrimetrically. Krishnamurthy et al. ( 9 7 0 detected tricresyl phosphate (TCP) and tri-a-crysyl phosphate (TOCP) in contaminated edible oils by TLC. TOCP was analyzed by GC-FID for confirmation and quantitation of its level in oils. Linfield et al. (106F) reported a new method for the assay of lipase activity. Maxwell et al. (122F)described a method for the quantitative extraction and simultaneous class separation of milk lipids. Lipid classes were separated into neutral and polar fractions by column chromatography on a Celite column with sequential elution using solvents of increasing polarities. The extraction of lipids and their quantitative classification in meat products were carried out through the combined use of TLC and GC as described in a publication by Miteva
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Discriminant and cluster analyses of GC profiles of Worcestershire sauce volatiles were utilized by Aishima (3G)to differentiate sauces. The discriminant functions consisted of 12/85 peaks which were identified as terpenoids, phenols, and heterocyclic compounds. Carpenter et al. ( I I G ) related GC profiles of orange juice to processing conditions by application of multivariate methods. Izquierdo et al. (32G) applied principle component analysis to orange juice processing; the first principle component related to time and temperature of storage, and the second principle component related to cold-filled juices. Four GC peaks of orange juice essence, terpinen-4-01, trans-2-hexena1, an unidentified sesquiterpene, and an unknown compound, were used by Mayfield et al. (47G)to identify orange varieties. Chang and Reineccius (13G)developed a 40-m continuous dialyzing device to isolate flavors from mixtures as a function of sample and solvent flow rates. Tenax GC was used to trap intact fruit and vegetable aroma volatiles for subsequent GC analysis by DePooter et al. (I7G).The artifact backgrounds for Tenax GC and Tenax TA were compared by MacLeod and Tenax TA was found to be cleaner, and a more Ames (46G); efficient preconditioning regimen was proposed. Methods for the analysis of encapsulated (emulsified) flavors were screened FLAVOR acetone precipitation, simultaneous by Kernik et al. (37G); steam distillation/solvent extraction, and Fosslet methods Several reviews relevant to flavor analysis were published yielded uniform recoveries for both low and high boiling in 1984, 1985, and 1986. Busch (10G) reviewed applications compounds. Microwave desorption of thiamine decomposition of tandem mass spectrometry to fruit and spice flavor analysis. products from graphite was described by Reineccius and Chromatographic methods for the determination of phenols Toulemonde and Beauverd (67G)described Liardom (5.6G). and flavonoids in foods and beverages were covered by Hardin a device for injection, trapping, and near instantaneous miand Stutte (27G).The limits and perspectives of GC-FTIR crowave desorption for application to fruit volatiles. in flavor analysis were reviewed by Idstein and Schreirer (31G). Liddle and Bossard (43G)developed methods for the detection Adam (2G)described a method for volatile analytes whereby of /3-asarone, coumarin, hydrocyanic acid, pulegone, safrole, purged and trapped components are desorbed onto an inand a- and /3-thujones in foods and beverages. Reineccius and column cold trap (-100 "C) for concentration prior to GC Anandaraman (57G)contributed a general review of volatile separation. Cryofocusing of headspace volatiles at the head flavor analysis. Meat flavor volatile composition, analysis, and of a capillary column by Wylie (7%')afforded enhanced sensory testing were evaluated by Shahidi et al. (60G).Shaw sensitivity and permitted multiple headspace overlays and and Moshonas (61G)reviewed the use of mass spectrometry splitless injection. Badings et al. (4G,6G)developed an auin the identification of citrus flavor compounds. Food offtomatic purge and trap system in which efficiencies were flavor analyses were discussed by Whitfield and Shaw (74G). dependent upon trap composition, purge flow rate, trap temCapillary GLC of vegetable oil quality was achieved by perature, and total purge gas volume. Dirinck et al. (18G) direct sampling onto a cross-linked 5 % phenylmethyl silicone developed a dynamic headspace sampling apparatus applicable to GC-MS analysis of strawberry and apple volatiles. Goncolumn by Dupuy et al. (21G).Artifacts were encountered by Liddle and Bossard (44G)when using hydrogen as carrier zalez and Gra (25G)compared headspace concentration by gas for the analysis of anethole; dihydroanethole was produced closed circuit circulation through Porapak Q, with simultaupon sample injection. Nitz (53G)achieved greater componeous distillation/ether extraction, and found the headspace nent resolution using multidimensional GLC in which fractions technique to be faster and equally as reliable as distillafrom a packed column are further separated by capillary GLC tion/extraction. Kolb (38G)compared equilibrium and dynamic headspace procedures; in general equilibrium techconnected either to MS or a sniffing port. Schreier et al. (59G) compared capillary GC-MS and capillary GC-FTIR for niques were preferred for splittless injection, cold trapping, cherimoya fruit volatile analysis; GC-MS showed greater multiple headspace extraction, and calibration by standard sensitivity. Greater stationary phase thickness (0.45 pm) and addition. Borek et al. (9G)modified a laboratory vacuum rotary evaporator condensation coil to achieve nitrogen-driven higher temperatures (120 "C) were found by Shibamoto (62G) to yield better GLC Kovats indicies for alcohols and aldehydes. headspace preconcentration of volatiles from fruits and vegNormal-phase HPLC of cold pressed lime oil by Chamblee etables. Food volatile concentration methods, including direct headspace, headspace concentration, Nickerson-Likens, and et al. (12G)provided fractions for GC-MS that yielded 23 new solvent extraction, were compared by Leahy and Reineccius components. Rouseff (58G)isolated the bitter limonoids from (42G); simultaneous distillation/solvent extraction was found grapefruit, obacunone, nomilin, and limonin, by preparative to be most efficient at the 50 ppb level. Using a static HPLC. Ginger flavor compounds, 6-shogaol, 6-gingerol, 8headspace technique, Voilley and Bosset (71G) determined gingerol, and 10-gingerol, were isolated by Smith (63G)using the partition and activity coefficients for model flavor comreverse-phase HPLC with electrochemical detection. Van der pounds in high viscosity media. Greef et al. (69G)applied LC-MS, field desorption MS, and high resolution mass electron impact MS to identify the major Strecker-type compounds in cheddar cheese were isolated oleoresins of black epper. and analyzed by Dunn and Lindsay (20G)using Tenax-GC High-resolution ?C NMR has been applied to both qualheadspace trapping and acetonitrile extraction; Tenax-GC itative and quantitative analysis of essential oils and natural trapping was found most suitable for routine testing. Cheese flavors by Kubeczka and Formacek (40G).Ravid et al. (55G) headspace volatile GC profiles generated by steam distillation were able to quantitatively resolve (+) and (-) enantiomers were found by Lin and Jeon (45G)to be dependent upon of natural and synthetic linalool by 'H NMR using a chiral cheese age and solids concentration in the cheese slurry. A lanthanide shift reagent. The enantiomers of y-lactones were headspace volatile trapping technique for powdered milk and evaluated using 'H NMR by Weinstein et al. (73G)using the dairy products was developed by Badings and DeJong ( 5 G ) . chiral solvation reagent, (R)-(-)-2,2,2-trifluoro-l-(9-anthryl)- Horita and Hara (29G)found that more low boiling compounds are recovered from tea by using simultaneous steam ethanol. distillation/ether extraction than by using vacuum stripping; George (24G)characterized passion fruit flavors by Cardistillation time was deemed critical. Hutt and Herrington bowax 20M capillary GC-MS using chemical ionization with (30G) identified and quantitated the bitter principle in zucOH-. Volatile sulfur compounds from garlic oil were identified by Vernin et al. (70G) using a variety of GC-MS techniques chini, curcurbitacin E, using both reverse-phase TLC and reverse-phase HPLC. 4-Hydroxynoneal, a lipid peroxidation including electron impact and positive and negative chemical product, was extracted into methylene chloride, cleaned up ionization and single ion monitoring enhanced component on an ODS extraction column, and determined using reresolution.
(125F). Rosenthal et al. (153F)proposed an acid digestion method for fat determination in vegetable foods. Rossell et al. (154F)analyzed palm and coconut oil samples for fatty acid, triglyceride, sterol, and tocopherol composition as well as their melting properties. Slover et al. (164F)reported on the development and use of quality control samples in food lipid analysis. Smidovnik et al. (16%') developed a method for extraction and determination of lipids from corn starch, and analyses of honey lipids were reported by Smiljanic (166F).Smurygina et al. (1670reported on the results of fat determination in rennett and process cheeses by the Gerber and Van Gulik methods as compared with results of solvent extraction/gravimetric method and concluded that the Van Gulik method was superior to the Gerber method with respect to accuracy and reproducibility. Soliman et al. (169F)reported on the fatty acid composition of triglycerides and 2-monoglycerides of butterfat, beef tallow, cottonseed oil, admixtures of beef tallow with butterfat, and admixtures of cottonseed oil with butterfat. The determination of emulsifiers in various foods was reported by Yomota et al. (202F).
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verse-phase HPLC b Lang et al. (41G). A procedure suitable for dairy product Qzwas developed by Mills (48G)whereby protein volatiles are trapped on a porous polymer, desorbed, and resolved by capillary GC. Mori and Kiuchi (51G)preferred direct solvent extraction over simultaneous distillation/solvent extraction for quantitative detection of pyrrolidones, pyrroles, pyrazzines, and thiazoles in miso. Allyl isothiocyanate, 3-butenenitrile, and acetic acid were identified in mustard paste by Mounie et al. (52G) using solvent extraction and GC analysis. Nunez and Maarse (54G)preferred simultaneous steam distillation/ether extraction over static and dynamic headspace methods and strip/trap methods for the analysis of grapefruit volatiles. Ovine fat volatiles were profiled by Smuki and Bailey (65G) by heating the oil, purging volatiles onto a trap, and eluting trapped volatiles directly onto capillary GC-MS. Luminometry was applied by Tateo et al. (66G)to evaluate the storage stability and condition of citrus oils. Evidence for protein-phenolic binding during coffee roasting was obtained by Trugo and Macrae (68G) by spectroscopic analysis and size distribution changes in extractables as measured by SEC-HPLC. Chiang (15G)developed a sensitive HPLC procedure utilizing electrochemical detection to separate and quantitate capsaicins. Capsaicins can be detected in the presence of piperine by changing the detector potential or by measuring piperine at 340 nm UV. Piperine was measured by silica TLC with UV densitometry by Jansz et al. (34G). Kawada et al. (36G) separated capsaicin from dihydrocapsaicin using reverse-phase HPLC with electrochemical detection; the detection limit was 1 2 pg. Krajewska and Powers (39G) brominated capsaicins with pyridinium bromide perbromide to achieve reversed-phase HPLC separation of nordihydrocapsaicin from capsaicin. Kat0 and Sekikawa (35G)found direct injection of unstable lactones derived from butter flavor onto GC-MS system yielded best results. Moellering and Bergmeyer (49G) developed a specific enzymic method for detection of L-glucono-6 lactone in tissue and foods. The lactone is converted to gluconate-6-phosphate followed by oxidation with NADP' and spectrophotometric measurement of the resulting NADPH. Lactones from ghee were isolated with 80-9270 recovery by Wadhwa and Jain (72G) using a celite-digitonin-alumina chromatography column and acetonitrile elution. Collinge et al. (16G) developed a reverse-phase HPLC method for the analysis of glycyrrihizin and @-glycyrrheticacid in foods and beverages. Abraham and Deman ( I C ) developed a rapid infrared method for the determination of four isothiocyanates in canola oil; results were confirmed by GC and GC-MS. An enzymic method for the determination of acetaldehyde using aldehyde dehydrogenase and spectrophotometric measurement of NADH was conceived by Beutler (7G). Buetler (8G) worked out an enzymic method for ethanol determination by converting ethanol t o acetaldehyde using alcohol dehydrogenase and NAD+ and then measuring acetaldehyde as described above. Cyclic sulfur compounds in shiitake mushrooms, lenthionine, 1,2,4-trithiolane7 and 1,2,4,5-tetrathiane were determined using reverse-phase HPLC by Chen and Ho (14G). Dirks and Herrmann (19G)developed a reverse-phase HPLC method for the analysis of phenolics, hydroxycinnamoylquinic acids, and 4-(@-D-glUCOpyranOSy1oxy)benzoic acid in spices. Chlorogenic acid was the most abundant and frequently encountered compound. Liquid carbon dioxide extraction was utilized by Eberhardt and Pfannhauser (22G) to isolate an elderberry monoterpene precursor, 3,7-diethyl-octa-l,5-dien-3,7-diol. Cinnamaldehyde in cinnamon or cassia oil was determined by reaction with p-hydroxybenzoic acid hydrazide and 5 YO sodium hydroxide followed by spectrophotometric measurement a t 352 nm by El-Obeid et al. (23G);benzaldehyde did not interfere. Volatile aldehydes were converted to either thiazolidine or 2-acetylthiazolidine via reaction with cysteamine at pH 6 or 8, respectively, by Hayashi et al. (28G) and then determined by GC equipped with a thermionic N-P detector. Curcumin in spice mixtures was determined by Janssen and Gole (33G) by TLC resolution and conversion to rubrocurcumin with a mixture of boric acid and oxalic acid followed by fluorometric scanning. Molnar-Per1 et al. (50G)described an ion exchange method for the rapid separation of Maillard reaction products, deoxy fructosyllysines, and their pyridosine and furosine hydrolysis products. Spiro and Price (64G) developed a 230R
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method for the analysis of theaflavin and its mono- and digallate derivatives in tea solution by complexation with 2aminoethyl diphenyl borate (flavognost) and spectrophotometric measurement of the complex at 625 nm. An improved reverse-phase HPLC method for vanillin and related flavor compounds in vanilla extract was developed by Guarino and Brown (26G). This method is superior to the AOAC method because ethyl vanillin and p-hydroxybenzaldehyde can be resolved.
IDENTITY Chaveron et al. (12H)determined the presence of foreign plant fats in chocolate by GLC analysis of the Cm-C56 triglycerides and found the monooleic disaturated symetrical triglycerides most sensitive to the presence of nonchocolate fats. The presence of sesame oil was determined by Coors and Montag (14H)by HPLC analysis of sesamol, sesamolin, sesamin, and tocopherol with fluorometric detection. Farag et al. (20H) distinguished as low as 5% cow's milk in buffalo milk by regression analysis of GC fatty acid profiles of crystallized fats and mother liquor; myristic, palmitic, stearic, and oleic acid levels contributed to the equation. Gegiou and Staphylakis (24H) determined the presence or absence of cocoa butter equivalents in chocolate from GC or GC/MS analysis of triterpene alcohols. Gomez (26H) estimated mineral oil in vegetable oil at levels 10.1 YO using TLC. Mineral oil in vegetable oil has also been detected by Graciani et al. (28H) using HPLC separation of hydrocarbons isolated using silica gel chromatography. Gubman et al. (31H) assayed oil for the presence of phosphorus-containing compounds using a rapid and simultaneous reaction with molybdate and extraction into chloroform followed by spectrophotometric measurement. Theobromine in cocoa beans was quantitated by Hamann et al. (32H) using reverse-phase HPLC and phenacetin as internal standard. Hurst et al. (38H)measured caffeine, theobromine, and theophylline in cocoa using microbore reverse-phase HPLC and reported detection limits ranging from 100 to 150 pg. Harland and Oberleas (33H) developed an analytical method to measure phytate in vegetables and grains which employs anion exchange chromatography; the method was adopted as an official first action. Lemieux et al. (54H) compared three methods for phytate measurement: ferric chloride precipitation, ion exchange retention, and enzymatic hydrolysis. The ion exchange method was preferred for rapidity and low cost. Mazzola et al. (61H) applied 31PFT NMR to the analysis of phytate in foods and found excellent agreement with published ion chromatographic methods. Il'ina et al. (40H)developed a technique to measure carbon dioxide in noncarbonated beverages which utilizes both a gas electrode and a pH meter in tandem. Mustard seed coat presence was detected by Jamais et al. (41H) by colorimetric analysis of 4-hydroxyproline, after oxidation to pyrrole by Chloramine T and reaction with Ehrlich's reagent. Kikugawa et al. (48H) developed a chromogenicassay for lipid hydroperoxides whereby reation of hydroperoxides with sesamol dimer in the presence of hemoglobin (metHb, oxyHb, or carbonmonoxyHb) results in highly colored quinones or semiquinones; this technique was found to be more sensitive than the peroxide value method. Krueger and Krueger (51H)assessed the purity of natural vanillin by oxidation with sodium chlorite to vanillic acid, decarboxylation by treatment with bromine, and analysis of released carbon dioxide 13C/12Cisotope ratio using MS. Lee et al. (53H) measured furfural and 5-hydroxyfurfural in citrus juice using reverse-phase HPLC and reported a 50 ppb lower detection limit. Lever et al. (55H) realized 60 sample per hour turnover for furfural analysis using a continuous flow system incorporating furfural conversion to hydrazone, dialysis, into methanol, and fluorescence measurement of the zinc chealate. A reverse-phase HPLC method for furfurals in orange juice was reported by Marcy et al. (60H)in which distillation of the juice was employed as a cleanup step. Loeliger and Saucy (58H)applied chemilimunescence emmission to the determination of food autooxidation. By comparison with traditional peroxide value methods, the results from this technique were critically dependent upon the type of food being analyzed and the presence of food additives (antioxidants). Muuse and Van der Kamp (65H) determined the presence of fractionated butterfat in natural butterfat by gravimetric analysis of saturated triglycerides crystallized from hexane at 12.5 "C; this
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technique was found superior to fatty acid analysis, analysis of sn-%fatty acids, and cholesterol analysis. Lipid identification was achieved by Nazer et al. (67H) by applying multivariate statistical analysis to prolysis GC profiles. The presence of spore-forming bacteria in canned, low-acid foods (cream style corn and beef noodle soup) was confirmed by Schafer et al. (77H) using GC analysis of butyric acid and ~-(-)-2,3-butanediol;this technique was adopted as official first action. As low as 4% palm stearin in palm oil was detectec by Tan et al. (79H) by anal sis of slip melting point, iodine value, and GC fatty acid ancrtriglyceride composition. Results were highly dependent upon the type of palm stearin fraction that was added. Tanner and Limacher @OH) measured methanol, ethanol, and acetaldehyde in fruit juice by addition of citric acid and direct injection into a GC containing a Carbopack B/6.6 CW column and FID detection. Wrigley et al. (84H) reviewed the utilization of electrophoretic patterns of grains and other foods to determine and characterize their genetic complement or similarity. A histochemical determination of glucosinolates in rapeseed oil or sectioned rapeseeds was developed by Yiu et al. (86H) where glucosinolates are detected by reaction with N-2,6-trichloro-p-benzoquinoneimine which produces a yellow color. Quality of fruits and vegetables was determined by Akimoto (2H)using simultaneous quantitation of sugar and acid by 13CNMR. Barroga et al. (4H) measured polyphenols in mung beans using three methods (modified vanillin, Prussian blue, and protein precipitation) and found that results varied widely according to mung bean treatment, rather than the method used. Of the six rapid tests for frying oil quality, Croon et al. (15H)found the Foodoil Sensor and the Fritest tests most rapid and accurate. The country or origin of green coffee was determined by Dyszel(19H)using pyrolysis MS. Corn protein quality was related to the amide I1 to amide I infrared band intensity ratios by Fedenko (21H). G e i i e r et al. (25") found that changes in chocolate because of processing variations could be attributed to changes in the integrity of cocoa starch. Hill and Gasson (35H) developed a SDS-polyacrylamine gel profiling technique to determine the occurrence of casein hydrolysis by S. lactis proteases in milk. A headspace GC method for determination of ethanol in the aqueous phase of canned salmon was deeloped by Hollingworth et al. (36H) and adopted as official first action. Ohhashi (70H) published a freshness index equation for fish based on levels of ATP, ADP, AMP, IMP, inosine, and hypoxanthine. By profiling various protein extracts from different species of wheats, Huebner and Bietz (37H) were able to demonstrate relationships between species and profiles that are useful for quality control and breeding selection. Kamarei and Karel(44H) measured the extent of autooxidation in freeze-dried meats by fluorescence;excitation and emission wavelength maxima were different in extracts containing oxidized components. Nakhost and Karel (66H) developed a myoglobin-based indicator system for freeze-dried meat autooxidationin which myoglobin insolubility, metmyoglobin concentration, and dimer to monomer ratio are assessed. Grain spoilage by microorganisms was assessed by Kaminski et al. (45H) by colorimetric measurement of the volatile carbonyl acetone equivalents as oximes. The thiobarbituric acid method for rancidity in fish was improved by Ke et al. (46H) by incorporating acid hydrolysis and distillation steps prior to reaction with 2-TBA and spectrophotometryat 538 nm. Kneifel and Ulberth (49H) evaluated the extent of milk heat treatment by various casein precipitation procedures and SEC-HPLC profiling of milk proteins. Ammonia, a quality indicator substance for squid, was measured by LeBlanc and Gill (52H) by amination of a-ketoglutaric acid in the presence of glutamate dehydrogenase and NADH, and concurrent oxidation of tetrazole to colored formazan. Lin and Cousin (56H) measured the OPAglucosamine derivative by reverse-phase HPLC with fluorescence detection to estimate the extent of mold contamination of processed foods. Manz (5923 determined the presence of heat-denatured bovine and porcine proteins using an ELISA test developed for the a-2-globulin fraction. Rapeseed maturity (quality) was assessed by Minkowski and Schubert (62H) from the optical density of chlorophyll at 669 nm in a petroleum ether-ethyl ether extract. Using a-solanine as an antigenic hapten, Morgan et al. (63H) developed an ELISA test for potato glycoalkaloids which gave good cross reactivity with a-solanine, a-chaconine, and demissine.
Morishita et al. (64H) isolated vegetable phenolics by preparative reverse-phase HPLC and identified the components using 'H NMR and MS. Cheese quality has been assessed from ultrasonic transmission and reflection measurements by Northeved (68H). The extent of milk heat treatment was measured by Patel et al. (73H) using the methylene blue reduction test for residual xanthine oxidase enzyme. Used frying oil was detected from changes in the GC triglyceride dimer peak shapes by Rogstad (75H). Takahashi et al. (78H) described an extraction, cleanup, and HPLC electrochemical detection system for the carcinogenic compounds, aminoimidazoquinoline and aminoimidazoquinoxal,in heated beef extract. Oyster freshness was determined by Tsunoda et al. (82H)from residual succinate dehydrogenase activity as measured by concurrent reduction of tetrazolium chloride to red formazan. Patel (72H) reviewed competitive and noncompetitive immunologic methods for determination of staphylococcal enterotoxins. Biru et al. (6H) found ELISA simple and satisfactory for detection of staphylococcal enterotoxins in contaminated foods. Notermans (69H) and Wieneke (83H) likewise described ELISA tests for staphylococcal enterotoxins to be accurate for assessment of foods associated with poisioning outbreaks. Hyde and Stahr (39H) correlated volatile trapping thermal desorption GC/MS results from moldspoiled grains to the presence of mycotoxins. Carman et al. (9H) developed a rapid GC-FID method to detect and quantitate the plant toxin, myristicin, in fresh and frozen carrots. Casa et al. (10") developed an immunoelectrophoresis method to detect soluble horse muscle proteins in the presence of soluble bovine and procine muscle proteins. A test for soluble pig muscle protein was also developed by Casa et al. (11"). Garrone et al. (23H) detected hazelnut presence in chocolate by thin-layer electrophoresis of ammonium sulfate protein extracts on cellulose acetate. From proline, aspartic acid, and alanine levels, Greenberg and Dower (29H) were able to detect added whey protein in nonfat dry milk powder, regardless of heating. An ELISA test to detect soya protein in meat was developed by Griffiths et al. (30H). Janssen et al. (42H) detected soya proteins in heated meat by applying a selective immunoperoxidase system to blots derived from SDS polyacrylamide gels; antigenicity was decreased in the presence of liver at 25 OC. Jones and Patterson (43H) developed an indirect ELISA test for unheated meat species identification that uses crude antisera rather than highly differentiated purified antibodies. Krause and Belitz (50H) milk from different species by isoelectric focusing of their y-2-caseins. Muscle protein presence in mixtures with soya protein and rind was achieved by Lindberg et al. (57H) by reverse-phase HPLC profiling of dansylated amino acids and application of multivariate statistical analysis. As low as 0.5% soya protein was detected in meat, cooked or uncooked, by Ravestein (74H) using an ELISA test; lower detection limits could be achieved by using immunoblotting techniques. Yehchen and Hsu (85H)detected protein hydrolysate in soy sauce by measuring the levulinic acid content by HPLC with bromocreosol purple postcolumn detection. Demmer and Werkmeister (17H) found that extracts from frozen pork and not fresh pork contained the mitochondrial enzyme, 0-hydroxyacyl-CoenzymeA dehydrogenase. Fresh liver was discriminated from frozen liver by Gottesmann and Hamm (27H) using the marker enzyme, P-hydroxyacyl-Coenzyme A dehydrogenase; results were not definitive for chilled liver samples. Salfi et al. (76H) differentiated between fresh and frozen fish by separating aspartate aminotransferase isozymes and staining for enzyme activity. Chen and Lin (13H) measured the 14Ccontent of plants by using Aquasol-2 as liquid scintillant and a low background scintillation counter. Derbesy (18H)reviewed the practical uses of stable isotope analysis for quality assessment of flavoring materials; 14C,13C/12C, 2H/1H,and l8O l60ratios were taken on vanillin and anethole. Palagyi (71 measured 1311 in drinking water by entrapment on a polyurethane column impregnated with a tert-alkylamine-I complex and taking counts on the affinity column directly. To and Rack (81H) measured 1311in formaldehyde-preserved milk by first separating protein and liquid phases and then oxidizing I- to iodine, extracting with carbon tetrachloride, reducing iodine to I- with HS03-, and precipitating PdI for both phases.
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Boegl and Heide (7H, 8H) determined foods that had been treated with y irradiation or ultraviolet irradiation using chemiluminescence. y irradiation of spices was measured by Heide and Boegl (34H) by measuring the chemiluminescence of a mixture of the spice with luminol solution. Light yield and the time-course of emission were different for each spice, and oxygen concentration, pH, and luminol freshness affected the results. Kiel(47H) developed a microchemiluminescent probe material to assess peroxidative, heat, and ionizing radiation damage to cells by making a glutaraldehyde crosslinked complex from serum albumin, a heme protein, and a luminescer. Acton et al. (IH) determined the structure of protein gels using ultrasound imaging. A screening technique for lectins in vegetables and spices was developed by Andersen and Ebbesen (3H)which utilizes line-drive immunoelectrophoresis and hemadsorption. Bianchini et al. (5H) determined the sterol and triterpene composition of sunflower oil by HPLC analysis of their acetates. Free formaldehyde was determined in meat by DeFreitas et al. (16H) by extraction, distillation in the presence of sodium sulfate and phosphoric acid, and photometry. Lysinoalanine was detected and quantitated in milk proteins by Fritsch (22H) by ion exchange chromatography and postcolumn reaction with OPA and fluorescence detection.
MINERALS Trends in methodology continue to favor multielement techniques. The application of inductively coupled plasma atomic emission spectrometry (ICP-AES) techniques also continue to increase. Review articles pertaining to multielement analysis consist of the following: Mannino (584 who reviewed electrochemical techniques for the determination Pb, Cu, Zn, Cd, As, and Hg in foods; Herrador et al. ( 3 6 4 who compiled spectrophotometric methods for Pb, Hg, Cd, Se, and As in milk; and Boyer et al. (154 who examined the interlaboratory variability in trace element analysis of collaborative studies conducted by the AOAC. A method for the determination of Mn, Fe, Cu, and Zn in tropical foods was reported by Benzo et al. (134 who digested the samples with H N 0 3 H2SO4/H2Ozfollowed by AAS. Puchyr and Shapiro (784 escribed a procedure for extraction and determination of Al, Fe, Sn, Zn, Ca, Mg, Ni, Cu, Cr, Ca, and K in foods by AAS. Trace elements were determined in milk by AAS, neutron activation analysis, and photon-induced X-ray emission by Gharib et al. (284. Kluessendorf et al. ( 4 7 4 described a procedure for Pb, Cd, and Zn in livers by Zeeman AAS of solid samples. Knezevic and Kurfuerst (484 compared solid sampling and digestion techniques by graphite-tube AAS for the determination of Cd, Pb, Hg, Cu, and Cr in food packaging materials and found the values obtained comparable. Yan et al. (1084 found comparable results by ion chromatography (IC) and AAS for the determination of Cu, Zn, Fe, Mn, Ca, and Mo in beverages; the IC method shows no matrix effect and unlike AAS is suitable for simultaneous elemental analysis. A method for the determination of Fe, Cu, Mn, Co, Cr, Mo, and Ni in milk by electrothermal AAS was described by Mingorance and Lachica (634. Simultaneous determinations of nine elements in a reference standard and fruit juice were reported by Harnly (354 who used a commercially available aerosol depositioncarbon furnace atomizer with a multielement atomic absorption continuum source spectrophotometer. Evans and Read ( 2 2 4 determined Li and Rb in foodstuffs using flame atomic emission and absorption spectrometry. ICP methods are being used more commonly and the following have been reported for food analysis: Lyons et al. (564 described a procedure for the determination of Ca, Zn, Mn, Fe, Mg, and P in feed and plant material; Shiraishi et al. (864 applied the technique to the direct multielement analysis of total diet samples for major, minor, and trace elements; and Takeo (954 described instrumentation and methodology to determine minerals and trace elements in tea. A collaborative study for the determination of Ca, Cu, Fe, Mg, Mn, P, K, Na, and Zn in infant formulas was reported by Suddendorf and Cook (94J) and the ICP method was adopted official first action by the AOAC. Nickdel and Barros (714 described a procedure for major and trace elements in citrus juices using an automated fast sequential multielement spectrometer combined with ICAP-AES.
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Sample preparation and mineralization techniques for elemental analysis have been emphasized in some publications. Microwave oven digestion techniques were reported by Ishii (434 and by White and Douthit (1054 who tested the technique with NBS reference materials and found good agreement for the elements Ba, Ca, Mg, Mn, P, K, Na, S, and Zn using ICP. DeMura et al. ( 2 0 4 report a microwave oven digestion method for the determination of Zn, Cu, Mn, Pb, and Cd in food and reported recoveries of 84-113%. Gillain and Rutagengwa (294 compared two ashing methods for the determination of Zn, Cd, Pb, Cu, Sb, and Bi in milk by differential pulsed anodic stripping polarography and found the Teflon bomb ashing method gave satisfactory results for the more volatile trace elements. A preparative digestion procedure for biological and diet samples prior to the analysis of essential minerals by AAS was described by Hill et al. (384. Murphy et al. (664 compared wet ashing and flame/furnace aerosol sampling techniques for the determination of Cd, Cu, Mn, Ni, and Cr in food by AAS. An automated wet digestion procedure for the determination of As, Cd, Cu, Hg, Pb, Se, and Zn in animal tissue was described by Salisbury and Chan (814. A procedure including sampling, transport, drying, homogenization, digestion, and voltimetric measurement for the determination of Zn, Cd, P, Cu, Ni, and Co in meat of slaughtered cattle was described by Narres et al. (704. A review of the certification of reference materials by the National Bureau of Standards was published by Alvarez (34 and Miller-Ihli and Wolf (624 described the characterization of NBS SRM 8431 for 17 elements. Aluminum and iron in food samples and water were determined by Yan and Schwedt (1094 using ion chromatography and postcolumn derivatization. McCabe and Ottaway (604 described a novel method for the determination of As, Sb, and Se in animal food protein as their hydrides using AAS. Oxygen bomb combustion and automated AAS with hydride generation was used by Narasaki (684 for the determination of As and Se in butter and polythenes. Muenz and Lorenzen ( 6 5 4 described a procedure for the selective determination of inorganic and organic arsenic in foods by AAS using the hydride generation technique. Methods for the determination of As in sugar, beet pulp, and molasses by AAS after hydride formation were studied collaboratively by Huijbregts et al. ( 4 0 4 and compared to neutron activation and absorptiometric methods. Arsenic in food samples by AAS with graphite furnace was reported by Dabeka and Lacroix ( 1 9 4 who described a routine method involving dry ashing, by Okubo et al. ( 7 3 4 who used nickel ion with wet digestion, and by Tsukada et al. ( 9 6 4 who reported a rapid microwave oven digestion method. A spectrophotometric method for the determination of boron in natural waters and vegetable matter was described by Aznarez and Mir ( 7 4 . Ochiai et al. (724 determined boron in foods by dry ashing, dissolving the ash in dilute HCl, and chromatography on a cation-exchange resin column and fluorescence detection. Analytical methods for the determination of Ca and Mg in wine were reviewed by Baluja-Santos et al. ( 9 4 . Kindstedt et al. ( 4 6 4 described an improved complexometric method for the determination of calcium in cheese using hydroxynaphthol blue as the indicator with EDTA titration. Calcium and potassium were determined in skim milk powder by A1 Hitti et al. ( 1 4 who used a dry ashing procedure with ionselective electrodes. Alvarez de Eulate, et al. ( 2 4 determined Cd, Cu, and P b in food grade salt by extraction of the ammonium pyrrolidinedithiocarbamate complex with 4methyl-2-pentanone followed by AAS. Direct solid sampling analysis of Cd, Pb, and Hg in fresh seafood by Zeeman AAS with graphite furnace was described by Grobecker et al. (314. Narres et al. (694 determined Cd and Pb in milk directly with platform furnace Zeeman AAS. Olayinka et al. ( 7 4 4 developed a slurry technique for the determination of Cd in dried foods by electrochemical atomization AAS. Cobalt was determined in foods by Barbera et al. ( 1 1 4 after wet digestion, liquid extraction, and AAS. Copper was determined in milk powder by Khammas et al. ( 4 5 4 by electrothermal atomic absorption and atomic emission spectrometry. Chromium was determined in meat samples by Schindler (834who digested the sample with HNOBfollowed by graphite tube AAS with Mg(NO,), added as a modifier. Farre et al. ( 2 3 4 reported an AAS method for the determination of Cr in foodstuffs in which the organic matter is digested with HNOJ, followed by
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oxidation to Cr(V1) and extraction with methyl isobutyl ketone. Iron in wines, foods, and minerals was determined by salinas et al. (804 using a new reagent-5,5-dimethyl-l,2,3-~yclohexanetrione 1,Zdioxime3-thiosemicarbazone and absorbance measured a t 550 nm. Singh et al. ( 8 9 4 proposed 1-(2quinolylazo)-2,4,5-trihydroxybenzeneas a sensitive chromogenic reagent for the simultaneous determination of Fe and Cu in foodstuffs, body tissue, and milk samples. Viladrich Gonzalbez et al. (1024 compared AAS and ICP for the determination of Fe and Cu in fats. A method employing isotope dilution fast atom bombardment mass spectrometry was developed by Gharaibeh et al. ( 2 7 4 for the quantitative determination of Fe in foods. A rapid method for the determination of P b in milk has been proposed by Mannino and Bianco ( 5 7 4 who used potentiometric stripping analyses without sample pretreatment. A method for the determination of P b in spinach involving minimum sample preparation was described by Stephen et al. ( 9 2 4 , who used electrothermal AAS. Andersen ( 4 4 described a screening method for the determination of Pb in infant formulas and powdered milk using Zeeman corrected graphite furnace AAS. A graphite furnace AAS method for the determination of Pb and Cd in foods after nitric-perchloric acid digestion and coprecipitation with APDC was reported by Dabeka and McKenzie (184. Cold-vapor AAS was used by Koops et al. (504 for ultratrace amounts of Hg in milk products and by Coles et al. (16J) who described a reference method in detail for the determination of Hg in foods. A method of digestion by using a mixture of HCl, HN03, and H2S04was developed by Louie et al. ( 5 5 4 for the determination of Hg in a wide range of food products with a detection limit of 0.01 mg/kg using cold-vapor AAS. Mercury loss during pretreatment and digestion of plant materials was investigated by Semu et al. ( 8 5 4 who found that digestion with HN03/KBr03resulted in a recovery of 90-100% of the added Hg. Grobenski et al. ( 3 2 4 developed a method for the determination of Hg by Zeeman graphite furnace AAS and successfully applied it to several environmental samples. Kruse (524 reviewed mineralization methods for the determination of Hg, Cd, and As in fish products by AAS. Methods for the determination of total Mo and V in foods were described by Evans and Caughlin ( 2 1 4 who measured Mo at 680 nm as the toluene-3,4-dithiolate complex and V at 415 nm by its catalytic effect on the oxidation of gallic acid with peroxymonosulfuric acid. Kohiyama et al. ( 4 9 4 found that extraction with HC1 is suitable for the routine analysis of nickel in hydrogenated oils using AAS. Vaeth and Hob (995) determined trace amounts of Ni and Fe in fats and oils by AAS with a reduced sample treatment procedure. A validation study was reported for a fluorometric method for the determination of Se in food by Vaessen et al. ( 9 8 4 who decomposed the samples in a closed system and complexed the Se(1V) with 2,3-diaminonaphthalenea A wet decomposition procedure with a mixture of "OB, HC103, and HC104 was described by Irsch et al. ( 4 2 4 for the determination of Se in samples of plant and animal origin using the hydrideAAS method. A sodium ion selective electrode method has been reported by Fulton et al. ( 2 6 4 for the determination of sodium directly in processed meat products. A slurry method for direct flame emission determination of Na and K in processed meat and pizza products was reported by Wichman et al. (1064 who used a sonic cavitational homogenizer for sample preparation. Tin was etermined in canned foods by Aznarez et al. (BJ)using AAS and hydride generation in a nonaqueous medium. Hocquellet ( 3 9 4 described the direct determination of tin at ultratrace levels in fats and oils by AAS with electrothermal atomization. Total tin determinations were reported by Krull and Panaro ( 5 1 4 using continuous on-line hydride generation followed by dc plasma emission spectroscopy (HY-DCP); organotin analysis and speciation can be accomplished by interfacing this HY-DCP setup with HPLC. Gutierrez et al. ( 3 4 4 described a rapid extractive spectrophotometric method for the determination of Sn in canned foods with 5,7-dichloro-8-quinolinol. A fluorometric method for the determination of Sn at the nanograms per milliliter level in canned beverages was reported by Rubio et al. ( 7 9 4 who reacted Sn with diacetylmonoxine nicotinylhydrazone to form a fluorescent complex. The determinations of Sn and Pb in canned fruit juice by differential pulsed polaragraphy were reported by Guinon et al. (334who
d
used Hyamine-2389 and appropriate electrolytes to separate Sn and P b peak potentials to allow the simultaneous determination of these elements. Titanium in milk powders was determined by ICP-AES by Van Betteray-Kortekaas et al. (1004 after heating at 450°, fusing with Kfi207,and dissolving in a hot H2S04solution. Zinc was determined in milk by Singh et al. (885) using l-(2-quinolylazo)-2,4,5-trihydroxybenzene as a spectrophotometric reagent. A selective spettrofluorometric determination of zinc with 5,7-dibromo-8-quinolinol and its application to food samples was described by Fernandez et al. (244. An AAS method for the determination of trace amounts of zinc in canned juices after ion exchange separation was reported by Aziz-Alrahman (64. Multiple simultaneous anion analysis was reported by Schmuckler et al. (84.4who separated H2P0,, Cl-, Br-, NO,, I-, and S042-in fruit juices on a reversed-phase C18chromatographic column. Total bromine in food was determined by Oyamada et al. ( 7 5 4 who ashed the sample, reacted the liberated bromine with styrene monomer, and determined the resulting bromostyrene by as chromato aphy with electron capture detector (GC-ECDY. Stijve (93fdso used GC-ECD to determine inorganic bromide in foods by reaction with propylene oxide and found the results to be comparable to the ethylene oxide method. Nangniot et al. (675) compared bromide residues in vegetables by gas chromatography and by ion selective electrode after separation of other halides by ion-exchange chromatographyand preferred the latter method because of accuracy, rapidity, and simplicity. Mori et al. (64.4 used a postcolumn derivatization procedure to determine potassium bromate in food by HPLC. Residual chlorine in foods due to NaOCl or bleaching owder was determined by Hidaka et al. ( 3 7 4 who used heagpace gas chromatography after conversion of the chlorine to cyanogen chloride. The Volhard and potentiometric methods for the determination of chloride in meat products were compared in a collaborative study reported by Beljaars and Horwitz (124. Balulescu (104 determined salt in foods using an automated ion-selective electrode method at a rate of 40 samples hour and measuring C1, Na, and K. Johnson and Olson (4 made a comparison of available methods for the determination of salt in cheese including the Mohr, Volhard, ion selective electrode, and chloride analyzer procedures. Matsumoto et al. ( 5 9 4 described a conductometric flow injection analysis method for the determination of salt in food products at a rate of 70 samples/hour. Singer and Ophaug ( 8 7 4 described methods for acid diffusable and total F1 content in food. Total iodine in foods was determined by an automated colorimetric method based on iodide-catalyzed reduction of cerium by Fischer et al. ( 2 5 4 . Wiechen and Kock (1075) developed a routine method for the determination of low iodine concentration in milk based on the Sandell-Kolthoff reaction. A new method for the determination of I in food samples by isotope dilution mass spectrometry was described by Schindlmeier and Heumann ( 8 2 4 who decomposed the organic matrix with a mixture of acids and isolated the I by extraction with CCIQ Lawrence et al. (535) determined iodide in table salt by X-ray fluorescence after absorbing the HI generated from the sample onto an ion-exchange resin loaded paper disk. The determination of I radioisotopes in milk has been improved to increase accuracy and sensitivity and to shorten analysis time by Bettoli et al. (144 who concentrated the I isotopes by anion-exchange chromatography on AgC1Si02and then determined them by iodide-specific membrane electrode and y and ,8 counting. Iodine radionuclides in milk, vegetables, and fish were also determined by Meloni et al. (614 who used y-ray spectrometry for lEI and 1311and liquid scintillation counting for '9. The well-known Kroller method for the determination of cyanide was modified by Van Eeden et al. (1014 who replaced the harmful chemicals benzidine and Br with barbituric acid and N-chlorosuccinimide and applied the method to human foods and animal feeds. Nitrate-N in vegetables was determined by Hunt and Seymour ( 4 1 4 using an automated anion-exchange HPLC technique. Vlacil and Vins (1034 determined NO3- in milk products and milk-based infant formula using liquid chromatography on Spheron and direct photometric detection at 205 nm. Nitrate and nitrite in food products were determined by Unger and Heumann (975) using isotope dilution mass spectrometry; 15 NO, and 15 NO2- spikes were used for the dilution technique and negative thermal ions measured in the
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mass spectrometer. Nitrate and chloride ions in food were determined by Penchuck et al. ( 7 7 4 using a single-column ion chromatography technique. A procedure to measure P content of soybean and corn oil has been developed by Sinram (905)using the relationship between P level due to phosphatides in vegetable oil and turbidity formed in phosphatide mixtures; P vs. turbidity data formed nearly linear relations for crude, degummed, once-refined, bleached, and deordorized soybean and corn oil process samples. List et al. (545) determined phosphate and SOz in fruit juices and wine by flow injection analysis and photometry; a gas diffusion cell was used to eliminate interference for the determination of SOz. Warner et al. (1045) reevaluated the Monier-Williams method for determining sulfite in food and reported recovery values for a variety of commercial food products. Results of a 10-min flash distillation and 10-min ion chromatography determination compared favorably with the results from the conventional Monier-Williams method for total sulfite in foods according to Anderson et al. (54. Sulfur on grapes and wheat was determined by Goewie et al. ( 3 0 4 using a liquid chromatograph with UV and electrochemical detection. A fluorometric reaction rate method for determining hydrogen peroxide a t the nanomolar level was proposed by Peinado et al. (765) and applied to the analysis of coffee, tea, and milk samples; the method is based on the Mn(I1)-catalyzed oxidation of 2-hydroxynaphthadehyde thiosemicarbazone. Srinivas et al. ( 9 1 4 described a method for the continuous determination of HzOzin food based on the catalytic decomposition of HzOzby LaCoO,; the 0 liberated is measured by a gas measuring buret. A method has been developed to determine headspace Oz, NP, and COz in beverages and packages by Cook et al. (I75) using headspace gas chromatography.
MOISTURE Book that are of interest to analysts involved with moisture measurements are Aquametry. Part 2, Electrical and Electronic Methods: A Treatise on Methods for the Determination of Water" (12K) and Moisture Sorption: Practical Aspects of Isotherm Measurements and Use (8K). Bussiere et al. ( I K ) determined the water activity (aw) of confectionery products using various calculation methods. Unsaturated solutions of sodium chloride were proposed by Chirife et al. ( 3 K )for calibrating hygrometers for the determination of aw. Gerschenson et al. (5K) discussed the influence of organic volatiles such as 1,2-propyleneglycol on aw measurements with fiber-dimensional hygrometers. Theoretical prediction of aw of several standard saturated salt solutions agreed well with experimental measurements for most salts studied at 15' and 35' degree according to Kitic et al. (6K). Measurements of aw of salt solutions and foods by several electronic methods were compared by Stamp et al. (13K) to direct vapor pressure measurements; measurement of aw of foods gave values differing by an average of 0.051 aw units compared with VPM readings. A simple dew-point hygrometer which injects water into a sample gas and its application for determining moisture in foods by measuring the relative humidity differences were reported by Ueda et al. ( I 4 K ) . Sanna (11K) reported the results of a collaborative study to revalidate the reliability of AOAC method 30.005 for the determination of moisture in spices by distillation; for most spices, the method presented in this study was acceptable, whereas red pepper produced less satisfactory results. Rueegg et al. (IOK,9K) made a comparison of four commercially available Karl Fischer (KF) reagents and compared the water content in milk and milk products as determined by KF titration and reference oven drying method. A Karl Fischer method using a high potency KF reagent was applied by Koizumi et al. (7K) to the determination of moisture in high-moisture foods. Pulsed NMR was used by Gambhir et al. (4K) for the simultaneous determination of moisture and oil in oilseeds. Chin et al. (2K) reported the results of a collaborative study using microwave oven drying for the determination of total solids in processed tomato products and the results agreed well with the vacuum oven drying method.
ORGANIC ACIDS A reversed-phase HPLC method for simultaneous determination of benzoic acid, sorbic acid, and four parabens in 234R
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meat and nonmeat products was developed by Ali (115). Ashoor et al. determined acetic acid in vinegar and other foods by HPLC on an Aminex HPX-87H ion exchange column (2L) and citric acid in a variety of foods using the same column with a micro-guard ion-exclusion cartridge and UV detection at 210 nm (3L). Badoud et al. (4L)reported an HPLC method for the analysis of the main carboxylic acids in coffee, wine, and fruit juices using conventional and small-bore columns. Boehme et al. (8L)analyzed bread organic acids by HPLC. Chikamoto et al. (10L)simultaneously determined ethanol and propionic acid in bread and cake mixes by GC analysis of the steam distillates of samples. Rabe (49L) determined sorbic acid in bread and bakery products by colorimetric,TLC, GC-FID, and HPLC on RP-8 or RP-18 columns. The merits of the different methods were discussed. Chonan ( I l L )determined steam distillable propionic, butyric, caproic, and caprylic acids in milk by reversed-phase HPLC of their p-bromophenacyl esters with UV monitoring at 254 nm. Coppola et al. (IZL)reported the results of a collaborative study of a reversed-phase HPLC method for the determination of quinic, malic, and citric acids in apple juice and cranberry juice cocktail. Analyses were performed using two reversedphase columns, phosphate buffer (pH 2.4) mobile phase, and UV detection at 214 nm. The method has been adopted official first action by AOAC. Gancedo et al. (15L)analyzed oxalic, citric, galacturonic, malic, and pyrroleindone carboxylic acids in tomato juice by HPLC. Sorbic acid in jam and marmalade was determined by reversed-phaseHPLC and UV detection as reported by Goto et al. (17L). Hayakawa et al. (18L)determined the oxalic acid content of spinach by the HPLC of defatted aqueous extracts using a strong anion-exchange column with phosphate buffer (pH 4.1) as mobile phase and UV detection at 202 nm. Oxalic acid was also determined in spinach by Kok et al. (26L) using ion-interaction reversed-phase HPLC and amperometric detection and by Ohkawa et al. (4%) in spinach and beverages by GC analysis of the dimethyloxalate ester. Lin et al. (30L)analyzed wine and juice carboxylic acid by HPTLC on cellulose; developed chromatogramswere stained with xylose-aniline reagent and densitometrically scanned at 546 nm. Mattiuz et al. (35L)determined short chain (C,-C,) organic acids in nutritive sweeteners as table sugar and high-fructose corn syrup using ion-exclusion HPLC coupled with suppressed conductivity detection. Mazzola et al. (36L)analyzed phytate in foods using an ion chromatographic method and a ,*P Fourier transform NMR spectrometric method. Mentasti et al. (37L)reported a method on derivatization, identification, and separation of carboxylic acids in wines and beverages by HPLC. Matsuo et al. (34L)analyzed soy sauce for benzoic acid and levulic acid by TLC on kiesel gel 60 F-254 plates and by gas chromatography on a 10% DEGS + 1%H3P04on Chromosorb W (AW DMCS) 60-80 column. Benzoic acid and p hydroxybenzoate esters were simultaneously determined in soy sauce using reversed-phase HPLC and UV detection at 256 nm, as reported by Otsuka et al. (43L). Panari (44L) simultaneously determined pyruvic, succinic, lactic, formic, acetic, propionic, and pyroglutamic acids in cheese by HPLC on an Aminex-HPX 87H column at 42' with 0.013 N sulfuric acid as mobile phase and UV detection at 220 nm. Picha (45L) developed an HPLC technique for the analysis of malic, citric, succinic, and trace amounts of oxalic and oxalacetic acids in raw and baked sweet potato. Chromatography was carried out using an Aminex HPX-87H cation-exchange column at 75' with 0.0008 N HzS04as mobile phase and detection at 214 nm. Malmberg et al. (32L) determined chlorogenic acid in potato tubers by reversed-phase HPLC with UV detection at 313 nm and by GLC of silyl derivatives of chlorogenic acid or of quinic acid. Results of chromatographic methods (HPLC + GLC) were compared with the results of a spectrophotometric method and an enzymic hydrolysis method. Puttemans et al. extracted organic acids from food matrices by ion-pair formation with tri-n-octylamine and after back extraction to an aqueous phase, simultaneously determined synthetic dyes, benzoic acid, sorbic acid, and saccharin in soft drinks and lemonade syrups (47L) and sorbic acid, benzoic acid, and saccharin in yogurt (48L). Rocklin et al. (50L) separated and detected organic acids in wine and milk by ion
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chromatography with chemical suppression and conductivity detection. Tsuji et al. (54L) separated quinic, malic, and shikimic acids in plum fruit using cation-exchange HPLC and UV detection at 210 nm. An empiric formula for determination of lactic acid in starter cultures in reconstituted skimmed milk on the basis of its pH was reported by Joex et al. (2IL). Kogure et al. (255) determined the acid content of fruit juices by treating the juice with NaHC03 or its analogues and measuring the C 0 2 produced by the reaction. Cereda et al. (9L)determined formic, acetic, propionic, butyric, lactic, and succinic acids in fermented cassava starch by silicic acid chromatography. Fujita et al. (14L)used DEAE-cellulose column chromatographyand UV absorbance at 325 nm for the estimation of chlorogenic acid in pear and apple fruits. Matsumoto et al. (33L) investigated conductometric flow injection analysis for measuring the organic acid content of fruits and Murakami et al. (40L) colorimetrically determined sorbic acid in a wide variety of foods in the presence of ethanol. Coffee nonvolatile acids were determined by Engelhardt et al. (13L) using capillary isotachophoresis and capillary gas chromatography. The GC method was the most sensitive and is the method of choice for exact work. Capillary isotachophoresis was more rapid and reproducible and may be used in screening studies. Kikunaga et al. (24L) determined free and total oxalic acid, oxalacetic acid, a-ketoglutaric acid, citric acid, and succinic acid in spinach using capillary isotachophoresis. Prochazka et al. (46L) determined formic, acetic, propionic, butyric, valeric, and caproic acids in molasses using an automatic isotachophoresis analyzer. Several enzymic-spectrophotametric methods for determining food organic acids were published. Bergmeyer et al. (5L) discussed a method for determination of acetate in foods like wine and fruit juices by using acetate kinase, transacetylase, citrate synthase, and malate dehycrhosphorogenase following sample pretreatment for removal of 2-oxoglutarate, pyruvate, and lactate. Beutler (7L) determined acetate in beverages using acetyl-coA synthase, citrate synthetase, and malate dehydrogenase and sorbic acid (6L)in foods and fruit preserves. A procedure for determining L-(+)-tartrate was described by Giffhorn et al. (16L). Oxalate was determined in beer and fruit juices by oxalate oxidase, catalase, and aldehyde dehydrogenase as reported by Heinz et al. (20L). Kayahara et al. (23L) determined acetic, succinic, and citric acids in soybean pastes. Lagemann et al. (27L)analyzed cocoa and cocoa products for oxalic acid. Moellering (38L)discussed citrate analysis in liquid and solid foods. Schaller et al. (51L) oxidized formic acid to COzby NAD in the presence of formate dehydrogenase and measured the formad NADH spectrophotometrically. Healey et al. (19L) determined formic, acetic, propionic, and butyric acids in cane molasses by GC analysis of their benzyl esters on a column of 20% DEGS on Chromosorb W. Katagiri et al. (22L)GC determined lactic, citric, succinic, and pyroglutamic acids in miso. Lamkin et al. determined propionic acid in corn (2%) and in grain sorghum (29L)by GC. Littmann (31L) determined nonvolatile acids in shell eggs and sugar-treated liquid eggs by GC of methyl esters on packed and capillary columns and found that microbial spoilage of eggs was accompanied by a rise in lactic and succinic acids. Mollica et al. (39L)determined the nonvolatile organic acids in sugar maple sap by TMS-GC on a mixed liquid phase column of 4% SE-52/2% SE-30 on Chromsorb W-HP with N as carrier gas and FID detection. Oen et al. (41L) analyzed sweet cherry cultivars for L-malic, quinic, citric, chlorogenic,phosphoric,galacturonic, glucuronic, glucaric monolactone, gluconic, and oxalic acids by precipitation of the acids as lead salts, liberating the free acids, drying, and analyzing with TMS-GC and GC/MS. Butyric and caproic acids were determined in milk fat by reaction with methanolic barium hydroxide, fitering, releasing the two acids, and GC analysis on Chromosorb W AW 100/120 with 15% SP-1220 1% phosphoric acid as reported by Spahis et al. (52L). suda et al. (53L) analyzed soft drinks and jams for their content of sorbic, dehydroacetic, benzoic, malic, and tartaric acids by ion exchange of extracts and liquid-liquid partition of acids. Sorbic, dehydroacetic, and benzoic acids were gas chromatographed on a 5 % DEGS + 1% phosphoric acid column whereas succinic, fumaric, malic, and tartaric acids were TMS-GC determined on a 3% SE-30 column.
4
NITROGEN Osborne (78M) wrote a comprehensive review comparing and contrasting all chemical and physical methods for measuring the protein content of cereals. Aiyar et al. (2M) optimized the Kjeldahl procedure for commercial lactalbumin by. incorporating a 24-h preincubation with sulfuric acid and using mercuric oxide rather than copper sulfate catalyst. Use of the oxidant peroxymonosulfuricacid was claimed by Hach et al. (43M) to preclude the use of metal catalysts and salts in the Kjeldahl procedure; colorimetric detection was achieved by an improved Nesslerizationreaction. Horvath et al. (47M) compared Kjeldahl and near-IR techniques for protein measurement in the presence of nonprotein nitrogen (phenylalanine) and cellulose; near-IR yielded superior results for protein in the presence of phenylalanine. Kjeldahl analysis digestion step for animal feed was reduced by Kane (55M) using a catalyst composed of copper sulfate and titanium dioxide. Venter et al. (103M) optimized the semimicro Kjeldahl protein procedure for powdered dairy products by scrutinizing catalysts, sample size, digestion procedure, and distillation procedure. Bender (9M)reviewed 50 methods for protein quality determination. Abd El-Salam et al. (1M)demonstrated quantitative differences between species using .a single calibration on the Milkoscan 104 A/B infrared milk analyzer. Sjaunja and Andersson (93M) evaluated a new infrared milk analyzer, the Milko-Scan 605. Ameth (4M) described a continuous flow apparatus that determines protein by reaction of trinitrobenzenesulfonic acid with an acid hydrolyzate and measurement at 420 nm. Maximum protein solubilization from peas was found by Banu et al. (6M)to be dependent upon particle size, solvent/flour ratio, ionic strength, and pH. Findlay et al. (31M) characterized meat tenderness by analysis of differential scanning calorimetry (DSC) heating thermograms with respect to endothermic reaction order and number of cooperative units participating in the transition. Ihekoronye (49M) employed trinitrobenzenesulfonic acid to monitor the reaction rate of enzymatic hydrolysis of proteins using various protease mixtures and protein substrates. Keller and Neville (56M) compared four colorimetric procedures, biuret, Lowry-Peterson, Bio-Rad Coomassie Blue, and Pierce BCA, for determining the protein content of human milk correlations with micro-Kjeldahl were 0.96,0.97,0.89 and 0.99, respectively. Amide nitrogen in sodium carbonate extracts of food products was determined by Paredez-Lopez and Guevara (80M) using an ammonia-specific electrode. The presence of soy protein in meat was determined by Raghavan et al. (86M) by pyrolysis GC and quantitation of o-methyoxyphenol, dimethoxyp enol, and 2,3-dithiabutane. In a comparison of Kjeldahl, biuret, and near-IR methods for rapeseed protein content, Bengtsson (1OM) found that near-IR was more convenient to use routinely and yielded comparable data. Honigs et al. (46M) developed a mathematical algorithm for the discriminant selection of unique sample spectra which improved calibrations based on selected training sets. Near-IR wavelength calibrations were developed by Kaffka and Martin (54M) for protein determinations in “animal protein meal”. Valdez and Summers (102M) found protein determinations of poultry muscle tissue to be more precise with near-IR than with chemical methods. Chong et al. (20M) applied 14-MeV neutron activation analysis to measure organic nitrogen by utilizing carbon and oxygen interference. An automated proton activation analysis technique was described by Constantinescu (22M)to measure total nitrogen levels in cereals. Overley (79M) measured the nitrogen, hydrogen, carbon, and oxygen contents of cereals and other chemical compounds using neutron attenuation analysis. Protein in cereal meals was also measured with 14-MeV neutron activation analysis by Samei et al. (9OM). A monospecific antiserum was developed by Barnett and Howden (7M) using a heabresistant glycoprotein antigen from peanuts and was applied to the detection of heat treatment via rocket immunoelectrophoretictechniques. Two sandwich ELISA methods having little cross reactivity were developed by Fritschy et al. (34M) to detect both wheat a-gliadins and whole gliadins. McKillop et al. (70M) also developed an ELISA test for wheat gliadins. Enzyme-coupled monoclonal antibody tests for different wheat proteins, including gluten, gliadin, and cooked gluten, were developed by Skerritt et al. (94M),Skerrit (95M),and Skerritt and Smith (% Greiner &if).
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et al. (39M) developed an immunoturbidimetric assay for the detection of whey protein in nonfat dry milk using antibodies raised against whole bovine whey. An ELISA test for quantitative determination of denatured P-lactoglobulin in milk was described by Heppell(45M). Protein lactosylation was detected by Matsuda et al. (68M) using antibodies specific for e-deoxylactulosyllysine. Immunochemical methods for the measurement of a variety of food ingredient proteins were presented by Merger et al. (71M). An ELISA method for the detection of soy protein in soy lecithin, soy oil, and soy-based margarine was reported by Porras et al. (85M). Andrews et al. (3M) utilized fast protein ion exchange liquid chromatography with Mono Q and Mono S resins to resolve major milk protein classes; a 81, a s2, p-, K-, and y-caseins were resolved on Mono S, and whey proteins were resolved on Mono Q. Both casein and whey proteins were separated by Bican (14M) using a Protein Pak DEAE-BPW ion exchange HPLC column. Carpenter and Brown (18M)applied size exclusion HPLC to resolve and quantitate casein micelles after treatment with calcium. Gel filtration on Sephacryl s-1000 separated casein micelles by size and from whey according to Ekstrand and Larsson-Raznikiewicz (27M). Green (38M) resolved K-casein by polyacrylamide gel electrophoresis and characterized the fractions by chymosin sensitivity and by staining with Ethyl-Stains-d. Manji et al. (66M)fractionated whey proteins by anion exchange Chromatography eluting with a sodium acetate ionic strength gradient. Two-dimensional PAGE analysis of wheat proteins, incorporating isoelectric focusing and SDS-PAGE,resolved 480 discrete spots according to Lei and Reeck (60M). Lei and Reeck (61M) also compared two-dimensional gels of triticale proteins with those from their parental durum and rye species. A PAGE system for wheat gliadins was optimized by Lookhart et al. (63M) with respect to operating temperature and buffer composition. Wheat gliadins were fractionated by Popineau and Pineau (84M) using SP Trisacryl M, a mechanically and chemically stabilized cation exchange resin. Cuq and Cheftel(24M) reviewed detection methods, biological effects, and toxicity of lysinoalanine formed by thermal and alkaline processes. The detection of biologically available lysine via chemical, biological, microbiological, and enzymatic methods was reviewed by Zomborszky (IIOM). Beutler (12M) described an enzymatic method for glutamate determination where formazan, resulting from the combined actions of glutamate dehydrogenase and diaphorase with NAD/NADH and INT, is measured at 492 nm. Beveridge and Harrison (13M) modified the 2,4,6-trinitrobenzenesulfonatemethod for amino nitrogen in juice, juice concentrate, and liquid fruit products. Lysinoalanine was measured as its heptafluorobutyryl derivative by Bueser and Erbersdobler (15M)using GLC and a 3% SE-30 column. Precolumn derivitization of proline and hydroxyproline with 4-chloro-7-nitrobenzofurazan afforded Carisano (17M) a sensitive fluorometric HPLC assay. Chung et al. (21M) assessed amino acid racemization in alkalie-treated proteins via a dextrorotatory-specific enzyme reactor composed of D-amino acid oxidase and catalase immobilized on porous succinamidopropyl glass beads. Csiba (23M) developed a colorimetric method for hydroxyproline that is amenable to automation and depends on the reaction with p-(dimethylamino)benzaldehyde. In a study on sulfur-containing amino acid recovery from proteins, Dennison and Gons (25M) determined that recoveries vary with the food matrix regardless of oxidation and hydrolysis conditionsemployed. By oxidizing sor hum with performic acid prior to HCl hydrolysis, Elkin anfGriffith (28M) observed increases in cysteine, methionine, and histidine recoveries and destruction of tyrosine and phenylalanine; these authors suggested that one sample preparation method is not suitable. Gustine (42M) measured S-methylcysteine sulfoxide in Brassica extracts by reversedphase HPLC with fluorescence detection after precolumn derivitization with o-phthalaldehyde. Methionine, assmethionine sulfoxide, was determined by Hayashi and Suzuki (44M) in proteins by hydrolyzing with 3 N p-toluenesulfonic acid a t 110 OC for 22 h. MacDonald et al. (64M) reported on a collaborative study where sulfur-containing amino acids were measured in food and feed proteins by ion exchange chromatography following oxidation with performic acid prior to HC1 hydrolysis; the method was adopted as official first action. In a study on the inter- and intramolecular cystine contents of wheat gliadin proteins, Nadirov (74M) found interbiotype 236R
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differences using polarographic analysis. Recovery of methionine from feed concentrateswas improved by adding water to the formic acidlhydrogen peroxide oxidation mixture according to Slump & Bros (97M). Williams et al. (108M) measured the methionine content of peas. Eka and Oyeleke (26M) pTeferred pronase enzyme digestion of sorghum grain and maize over acid or base hydrolysis for tryptophan determinations. In a comparison of ion exchange HPLC with conventional ion exchange chromatographic amino acid determinations, Elkin and Griffith (26M) found that HPLC is more reproducible with respect to retention times but yields lower tyrosine and phenylalanine values and is less reproducible with respect to peak area. Elkin (30M) also compared reversed-phaseHPLC of OPA-amino acids with conventional ion exchange chromatogra hic techniques and found that both methods yield comparaE1e results; however, proline and cysteine were not detected by HPLC and glycine and threonine were not completely resolved. Friedman and Noma (33M) reported the analysis of (phenylethy1)aminoalanineand lysinoalanine in casein and soy protein using ion exchange chromatography. Gehrke et al. (36M) recommended higher acid hydrolysis temperatures (145 "C) for shorter durations (4 h) to achieve greater precision from subsequent chromatography of liberated amino acids. Huet and Pernollet (48M) determined tryptophan after barium hydroxide digestion by chromatography on Fractogel TSK HW 40 S and postcolumn derivitization with o-phthalaldehyde. A gas chromatography method for enzyme-released amino acids, as N-trifluoroacetyl butyl esters, was reported by Ihekorouye ( 5 0 . Ingles and Gallimore (52M) described a reversed-phase HPLC method for the separation of amino acids derivitized with fluoroescamine. Kuninori and Nishiyama (59M) separated and quantitated free and bound ferrulic acid as well as tyrosine in wheat seeds using reversed-phase HPLC and postcolumn fluorescence spectral analysis. Reaction of e-trinitrophenyllysine with carbohydrates during hydrolysis in the trinitrobenzenesulfonate method was reduced by James and Ryley (53M) by minimizing hydrolysis times. Molnar-Per1 et al. (73W applied several dye-binding techniques, including Orange G, acid orange 12, and amido black 10B, to the determination of reactive lysine. Per1 et al. (83M) determined reactive lysine by selective removal of reactive residues by acid modification with l-phenylazo-2-naphthol-6,8-disulfonic and acylation with propionic anhydride (histidine and arginine also react with this reagent). Ray (87M) measured available lysine by reacting the intact protein with 2,4-dinitrofluorobenzene followed by hydrolysis and thin-layer chromatographic resolution. Tomarelli et al. (%M) determined reactive lysine in infant formulas by reaction with trinitrobenzenesulfonate, hydrolysis, and reversed-phaseHPLC analysis with detection at 346 nm. A microbiological method for nutritionally available lysine was developed by Tuffnell and Payne (99M) using an auxotroph of E . coli which synthesizes P-palactosidase enzyme in proportional response to lysine; the galactosidase activity was measured by conventional procedures. A rapid procedure for determination of lysine was described by Viroben (104M) where total lysine is measured by reaction ith Acid Orange 12 before and after sample reaction with propionic anhydride. Picomole detection levels for OPA-derivitized amino acids resolved by HPLC were achieved by Lookhart and Jones (62M) by using ethanethiol rather than mercaptoethanol during derivitization. An enzymatic method to determine aspartic acid (and asparagine after deamination) was outlined by Moellering (72M) where aspartic acid is converted to oxaloacetic acid which is reduced by NADH in the presence of malate dehydrogenase; NADH consumption is followed at 339 nm. Ribarova and Shishkov (88M)reported an improved equation to calculate the amino acid contents of foodstuffs from hydrolysis-chromatography data. Nielsen and Hurrell(76M) determined tryptophan by vacuum hydrolysis with lithium or sodium hydroxide followed by reversed-phase HPLC with fluorescence detection. Saura-Calixto and Canellas Lourdes Soler (91M) determined tryptophan in nuts and seeds by ion exchange chromatography and postcolumn reaction with p-(diethy1amino)benzaldehyde and glyoxylic acid followed by spectrophotometric analysis. Tyrosine and histidine were determined as red azo dyes by Tummuru and Sastry (1OOM) following reaction with diazotized 4-chloro-2-nitroaniline. Ukeda et al. (101M)reported a rapid protein measurement for dairy products whereby the
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reaction of glutaraldehyde with protein is measured amperometrically using a Clark oxygen electrode. When measuring 3-methyl-~-histidinein muscle tissue, White and Lawrie (107M) found that recoveries from acetone powders were superior to those from fresh tissue. Arnstadt (5M) measured urea in urease-treated milk by reaction with p-(dimethy1amino)benzaldehydeand colorimetry a t 435 nm. Beattie et al. (8M) utilized HPLC-MS with a moving belt interface and ammonium chemical ionization to measure nonvolatile nitrosamines; silylation of the polyimide belt helped to reduce decarboxylations and denitrosations that occurred during transfer. Gavinelli et al. (35M) determined seven volatile nitrosamines by simultaneous distillation-extraction and GC analysis with thermal energy detection. Sen et al. (92M) minimized artifact nitrosamine formation from the analysis of rubber baby bottle nipples by pretesting methylene chloride for nitrosation potential and by incorporating propyl gallate (an inhibitor of nitrosation). An enzymatic method for ammonia was reported by Bergmeyer ( I I M ) whereby NH3 is consumed in the conversion of 2-oxoglutarate to glutamic acid with simultaneous loss of NADH. A continuous flow apparatus for ammonia and urea (as ammonia) measurement was described by Kirst et al. (57M) where upon reaction with perchlorate in the presence of nitroprussate, a blue colored reaction product is formed. A flow injection analysis for urea in cow's milk was reported by Oltner et al. (77M) where an enzyme reactor containing urease generates ammonia gas which is separated by a gas diffusion cell and measured by bubbling it into a color reaction solution. Hypoxanthine in fish was determined by Burns and Ke (16M) using reversed-phase HPLC with a mobile phase consisting of 0.01 M potassium phosphate, pH 4.5. Grass1 and Supp (37M) described an enzymatic determination for inosine monophosphate whereby IMP is converted to hypoxanthine and ribose-5-phosphate and the hypoxanthine is oxidized to uric acid which is measured a t 293 nm. The effects of pH, temperature, and ionic strength on ion-pair reversed-phase HPLC analysis of purine nucleotide monophosphates were studied by Mack et al. (65M). Nguyen et al. (75M) determined ribonucleoside 5'-monophosphates and their ieomers in potatoe tubers simultaneously by ion exchange HPLC. Ryder (89M) described ion exchange HPLC methods for the measurement of ATP and breakdown products in perchloric acid extracts of muscle tissue. Chang et al. (I9M) determined histamine, tyramine, tryptamine, histidine, tyrosine, and tryptophan in cheese using reversed-phase HPLC with a counterion-containing mobile phase. The agaritine content of commercial canned mushrooms was measured by Fischer et al. (32M)using cation exchange HPLC on Partisil SCX at pH 1.8. An IUPAC recommended method for determining azaarenes in meat using capillary GC profiling was reported by Grimmer and Naujack (40M). Grivas and Nyhammer ( 4 I M ) compared electrochemical methods with UV methods for quantitation of reversed-phase HPLC separated mutagenic imidazoquinolines and imidazoquinoxalines. Ingles et al. (5IM) detected biogenic amines in foods by ion exchange cleanup and HPLC analysis of fluorescent derivatives; positive identification was achieved by field desorption MS. a GC-FID method for the analysis of allylisothiocyanate and P-phenylethylisothiocyanatewas described by Kojima et al. (58M). Long chain aliphatic amines in fats were detected by Matschiner et al. (67M) upon reaction and separation with 4-methyoxy-7-nitrobenz-2,1,3-oxadiazole by TLC. Mayanna and Jayaram (69M) developed a method for dissolved caffeine by oxidimetric titration with aromatic sulfonyl N-haloamines. Patterson ( 8 I M ) described a new flame thermionic ionization detector for the Iatroscan rod chromatography system that is specific for nitrogen- and halogen-containing compounds. Peleran and Bories (82M) measured indole and %methylindole in pig fat back by combining selective solvent extraction with GC resolution and N/P-sensitive detection; identities were confirmed by MS. A multienzyme sequence to determine creatine and creatinine was reported by Wahlefeld and Siedel (105M) where creatine is phosphorylated yielding ADP, the liberated ADP and phosphoenolpyruvate are converted to ATP and pyruvate, and the pyruvate is converted to lactate with simultaneous loss of NADH. Wakabayashi (106M) developed a scheme to measure heterocyclic amines in cooked foods which incorporates treatment with blue cotton, partitioning against 0.1 N HC1, silica gel cleanup, and either reversed-phase or ion ex-
change HPLC with electrochemical detection. In a study on biogenic amines in cheese, Zee et al. (109M) found trichloroactic acid to be the best extraction solvent, but extraction efficiencies varied with cheese type, amine species, and relative concentration of the amine.
VITAMINS Books that are of use to the vitamin analyst for review and reference are Methods of Vitamin Assay-Fourth Edition ( 4 N ) ,Methods for the Determination of Vitamins i n Foods ( I O N ) , and Modern Chromatographic Analysis of Vitamins (15N). The separation of fat-soluble vitamins by HPLC from fish products was discussed by Lambertsen (36N). Methods and E in dietetic foods by HPLC were for vitamins A, C, D3, reported by Sell (49N). Gas chromatographic methods for fat-soluble vitamins in foods were reviewed by Davidek et al. (14N) and water-soluble vitamins were reviewed bv Velisek et ala'( 5 9 ~ ) . Bognar (8N) described an HPLC method for vitamin A in foods and reported the results of a collaborative study. The Carr-Price and an HPLC method for vitamin A in fortified milk were compared by Mills (42N) and found to be statistically equivalent. Coverly (13N) modified a continuous flow method for the determination of vitamin A in milk products and infant formula to increase the precision, recovery, and sampling rate. Speek et al. (53N) described a method for the determination of p-carotene by HPLC and the calculation of vitamin A activity in vegetables. Stancher et al. (54N) determined the isomer distribution of retinol and 3-dehydroretinol by HPLC and determined vitamin A active compounds in fiih oils. A TLC procedure for the determination of vitamin A in foods was suggested by Gerstenberg (22N) using fluorescence measurement after saponification and extraction. A reversed-phase HPLC method for the determination of vitamin A palmitate in nonfat milk and vitamin D in whole milk was described by Grace et al. (23N). HPLC methods for vitamin D in foods were reviewed by Kobayashi et al. (34") with emphasis on a method developed by the authors in 1981. Vitamin D3 in fat, oil, and margarine was determined by Rychener et al. (46N) by HPLC using vitamin Dzas an internal standard. Vitamins D2and D3 were determined by liquid chromatography in fortified milk and infant formulas by Landen (37N) after fractionating the vitamins from the lipid material by using gel permeation chromatography. Sertl et al. (50N) also determined vitamins D2 and D, in milk and infant formulas by normal-phase LC after using an aminocyano LC cleanup column to remove major interferences. HPLC procedures for tocopherols were described by Shen et al. (5IN) who separated a-,@-,y-, and 6-tocoherols on a short column to reduce analysis time, by Speek et al. (52N) who determined the four tocopherols, and a-tocotrienol in oil seeds using electron-impact mass spectroscopy for standardization, and by Rammell et al. (45N) who separated the four tocopherols and their corresponding tocomononals, and tocotrinols, and plastochromanol-8 in six seed oils using an amino-cyano HPLC column. A routine method for the determination of a-tocopherol acetate in fortified milk powder formulation using HPLC was described by Woollard et al. (63N). Vitamin K, in infant formulas was determined by Hwang (29N) using HPLC and UV detection. Zonta et al. (64") determined vitamin K, in soy bean oil after enzymic digestion, extraction, and alumina-column cleanup, followed by isocratic reversedphase chromatography with UV detection. Thiamin in foods was determined by Velisek et al. (58N) by gas chromatography with a flame photometric detector. Echols et al. (16N) evaluated solvents and recommended internal standards for the gas chromatographic determination of thiamin. Free and total thiamin in milk were determined by gas chromatography by Echols et al. ( I 7N) using a nitrogen-phosphorus detector. Thiamin in infant formula was determined by Ayi et al. f5N) by liquid chromatography using UV detection. Xneifel et al. ( 3 0 4 determined thiamin in milk products by HPLC after oxidation to thiochrome and subsequent fluorescence detection. Recent methods for the determination of thiamin and riboflavin are discussed and a new method for the simultaneous determination of these two vitamins is proposed by Augustin (3N). The use of HPLC for the simultaneous determination of thiamin and riboflavin was described by Finglas et al. (20N) in potatoes, by Mauro et al. (4IN) in enriched cereal products, and by Wimalasiri et al. ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
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(62N) in foods using both UV and fluorescence detection. Wills et al. (61N)determined thiamin and riboflavin in foods by HPLC and fluorometric methods and preferred the HPLC method for speed and accuracy. The use of HPLC for the determination of riboflavin was described by Ashoor et al. (2N) in milk and dairy products with UV detection, by Kneifel et al. (33N) in milk by fluorescence detection, and by Watado et al. (60N)in fresh fruits and vegetables with ion-pairing chromatography and fluorescence detection. On-line enrichment and isolation of vitamin B2 from large volumes of aqueous food samples followed by ion-pairing chromatography was described by Jaumann et al. ( 3 0 . Riboflavin was determined by Colugnati (12N) in fortified powdered milk and infant formula using cyclic pulsed voltammetry. An ion-pair liquid chromatographic method for the simultaneous determination of vitamins B2 and B6 in infant formula products was proposed by Ayi et al. (6N). A microbioassay procedure for the determination of free and bound niacin in cereals was described by Aki et al. ( I N ) . On-line generation of cyanogen chloride in the semiautomated determination of niacin and niacinamide in food products was proposed by Ge et al. (21N). An automated photometric method for the determination of niacin and niacinamide in grain and cereal products was proposed by Holz (28N)using 1,3-dimethylbarbituricacid and on-line generation of cyanogen chloride. A reversed-phase ion-pair HPLC method for the determination of nicotinic acid in instant coffee was described by Trugo et al. (55N). The use of HPLC for the determination of pyridoxin and the several forms of the vitamin in foods was described by Bognar et al. (8N),by Vanderslice et al. (56N),and by Gregory et al. (25N). A cation-exchange HPLC method for the seven major metabolic forms of vitamin B6 was described by Coburn et al. ( I I N ) . Ekanayake et al. (18N) described an in vitro, two-stage enzymic digestion system followed by HPLC to determine biologically available vitamin B6 in vitamin B6 fortified foods. Oesterdahl et al. (43N) compared a radioisotope dilution (RID) method for the determination of vitamin B12 in cereal with a standard microbiological assay with Lactobacillus leichmannii and found the RID method acceptable for routine determination of vitamin BIZ. Gregory (24N) reviewed liquid chromatographic methods for determining folacin in food and other biological materials. Folic acid in commercial diets was determined by Schieffer et al. (47N) using anion-exchange solid-phase extraction and subsequent reversed-phase HPLC. The determination of the biotin content in foods by means of a protein binding assay was reported by Bitsch et al. (7N). A radiometric microbiological assay using Kloeckera brevis was used by Guilarte (26N) for the analysis of biotin in a variety of food samples. Analytical methods for determining ascorbic acid in food products, biological samples, and pharmaceuticals were reviewed by Pachla et al. (44N) covering spectroscopic, electrochemical,enzymic, and chromatographictechniques. Both L-ascorbic and L-dehydroascorbic acid were determined by Kneifel et al. (32N) in milk and whey by paired-ion reversed-phase HPLC. An HPLC method was used by Kodaka et al. (35N) for the determination of total vitamin C after precolumn derivatization with 2,4-dinitrophenylhydrazine. Seki et al. (48N)separated ascorbic acid, dehydroascorbic acid, and diketoglulonicacid by HPLC with fluorometric detection and applied the method to the determination of ascorbic acid in fruit juice. A variety of foods were analyzed for vitamin C by Vanderslice et al. (57N) by HPLC and fluorometric detection. Photometric flow injection methods for the determination of ascorbic acid were described by HernandezMendez et al. (27N) and by Lazar0 et al. (40N). A UV method for the determination of ascorbic acid in soft drinks, fruit juices, and cordials was described by Lau et al. (38N). Differential pulsed polarography was used by Lau et al. (39N) for the determination of ascorbic acid in vegetables and fruits. Esaka et al. (19N) determined L-ascorbicacid in foods with immobilized ascorbate oxidase.
MISCELLANEOUS Books that are of use to the food analyst for review and reference are: Immunoassay in Food Analysis (13P),which covers principles of immunoassay and applications, Deuelopments in Food Analysis Techniques-3 ( l o p ) ,which is the 238R
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third in a series devoted to a discussion of recent developments in food analysis procedures, Analysis of Foods and Beverages, Modern Techniques (4P),and The Use of Statistics to Develop and Evaluate Analytical Methods (21P). A review discussion the application of near-infrared spectroscopy (near-IR) to the analysis of food and feed with emphasis on the measurement of moisture, protein, oil, starch, and fiber was published by Bernardini et al. (2P). Ronalds and Miskelly (17P) also reviewed near-IR applications in food analysis. Frankhuizen and Van der Veen (7P) reported on the calibration of near-IR reflectance apparatus for the rapid determination of major and minor constituents in milk powder and cheese. Near-IR was investigated by Sato et al. (18P)for measuring major constituents of raw milk and found the technique useful for measuring fat, protein, lactose, and total milk solids. Nadai and Mihalyi-Kengyel (14P) investigated equations for predictingmoisture, fat, and protein of raw meat by near-IR and Valdes and Summers (20P)investigated this technique for the determination of protein and fat in raw poultry. The rapid analysis of food packaging laminates by near-IR was reported by Davies et al. (623. A review article was published by Giacin and Brzozowska (8P) on the migration of substances from food-contacting materials into foods and methods for determining such substances. Hischenhuber (9P)reviewed the use of HPLC for determining food components, additives, and contaminants. A review of the application of HPLC in dairy science was reported by Miebs and Kirst (12P) including dairy product components, mycotoxins, contaminants, impurities, and preservatives. Woollard (22P) reviewed the expanding use of HPLC in the analysis of food for proteins, fats, carbohydrates, trace elements, amino acids, carboxylic acids, vitamins, additives, antioxidants, preservatives, coloring and flavoring materials, contaminants, aflatoxins, and other constituents. The application of ion chromatography in the food and beverage industry was reviewed by Cox et al. (5P); sample preparation and apparatus are covered in the article. Apparatus and methods for analysis of foods by differential thermal analyses and calorimetry were described by Raemy et al. (16P)who discussed thermal properties of carbohydrates, lipids, and proteins. Instruments and sensors for carrying out chemical, biochemical, and immunological methods of food analyses were reviewed by Kress-Rogers (1IP). A review on immunoassays in food analysis including principles of ELISA, development of kits, and applications was published by Allen ( I P ) . Test strips were compared by Schwedt and Altkofer (19P)with standard analytical procedures in the semiquantitative determination of pH, K, nitrate, sulfite, tartaric acid, and ascorbic acid in several foods and alcoholic beverages; results compared well although in some cases a simple cleanup procedure was necessary. Methods for the surveillance of radioactivity in food originating from natural and artificial sources were described by Boppel et al. (3P). A method to determine radionuclide levels in food by rapid pretreatment of samples with a modified microwave dehydration apparatus followed by radiation counting was developed by Nakaoka et al. (15P).
ACKNOWLEDGMENT The authors gratefully acknowledge the efforts of Carol Butler, Allen Oliver, and Nancy Ernst for computer assistance and Miriam Verner for typing the manuscript. LITERATURE CITED ADDITIVES (1A) Ali, M. Sher, J. Assoc. Off. Anal. Chem.. 1985,68, 488 CA1031115 , -1O -O -n (2A) Argoudelis, Chris J., J. Chromafogr., 1984, 303, 256. CA107(25):228621t. (3A) Ameth, Wolfgang; Wltzgall, Adelheid, fleischwirfschaff, 1985. 65, 637. CA 703(9):69832k. (4A) Barnett, Don, Food Technol. Aust., 1985. 37,503. CA704(1):4680k. (5A) Bauer, Frledrich; Stachelberger, Herbert, Chem ., Mikrobiol.. Technol. Lebensm.. 1984. 8. 129. CA701f151:128969u. (6A) Beutler; H. O:, Food Chem., i984, 75, 157. CA707(25):228591h. (7A) Blanchflower. W. John; Rice, D. A.; Hamilton, J., Analyst (London), 1985, 170, 1283. CA704(17):147252h. (8A) Brumley, W. C.; Warner, C. R.; Daniels, D. H.; Andrzejewski, D.; White, K.; Min. 2.;Cen, J.; Sphon, J., J. Agric. Food Chem.. 1985, 33, 368. CA 702(23):20267 le. (9A) Chester, T. L.; Innis, D. P.; Owens, G. D.,Anal. Chem., 1985, 57, 2243. CA 103(15):121827d. \
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--.
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(56A) Yanai. Kiyoshi, Japan, 1985, CA 704(3):18867p. ADULTERATION, CONTAMINATION, DECOMPOSITION (16) Acar, Jab; Klaushofer, Hans, Ernaehrung (Vienna), 1984, 8, 323. CA 702(21):183857b. (28) Aitzetmueiier, K.; Fox, J.; Arzberger, E.; Schoettier. H., Msch. Lebensm., 1984, 80. 201. CA707(15):128978~. (38) Alessandro, Rocco T.; Adams, James M.; Misklewicz, M., J. Assoc. Off. Anal. Chem., 1985, 68, 1154. CA 704(7):49924j. (48) Alleman, Thomas, 0.; Santlers, Robert A.; Madison, B., J. Assoc. Off. Anal. Chem., w1986, 69, 575. CA705(13):113741X. (58) Allen, Edward H., J. Assoc. Off. Anal. Chem., 1985, 68, 990. CA 703( 19): 159162w. (66) Archimbauit, P.; Ambroggi, Germaine, Reci. Med. Vet., 1986, 762, 495. CA 705(19):170737z. (78) Arnokl, D.; Vom Berg, D.; Boertz, A. K.; Maliick, U.; Somogyi, A,, Arch. Lebensmittlhyg., 1984, 35, 131. CA702(17):147628u. (88) Ashworth, Raymond B., J. Assoc. Off. Anal. Chem., 1985, 68, 1013. CA 703(19):159163~. (9B) Awasthi, M. D.: J. Food Sci. 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ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
(2858) Waiters, Mikla J., J. Assoc. Off. Anal. Chem., 1984, 67, 1040. CA 702(13):111574j. (2868) Ward, Colleen J. P.; Radzlk, D. M.; Kissinger, P., J. Liq. Chromatogr., 1985, 8, 677. CA 102(25):219698s. (2878) Ware, G. M.; Carman, A. S.;Francis, 0.; Kuan, S.,J . Assoc. Off. Anal. Chem., 1988. 69, 697. CA105(13):113753c. (2888) Warner, R.; Ram, 8. P.; Hart, L. P.; Pestka, J. L., J. Agric. Food Chem., 1988, 34, 714. CA 105(5):41333r. (2898) Wei, Ru Dong; Chang, Shenq Chyl; Wei, Ding Ling, K ' o Hsueh Fa Chan Yueh K'an. 1984, I f , 1559. CA102(9):77351x. (2908) Welling, Paul; Kaandorp, Ben, 2. Lebensm. Forsch ., 1986, 183, 111. CA705(15):132265m. (2918) Wetzel, D. L.; Wehling, R. L.; Lee, M. J.; Tweeten, T. N., Dev. Food Sci., 1988. 72, 667. CA 705(5):41342t. (2928) Whtaker. Thomas 8.;Dickens, James W.; Giesbrech, F., J. ASSOC. Off. Anal. Chem., 1986, 69, 508. CA105(3):23184p. (2938) White, J. W.; Meloy, R. W.; Probst, J.; Huser, W., J. Assoc. Off. Anal. Chem., 1986, 69, 652. CA105(13):113748e. Tiebach. R.; Weber, R.. 2. Le(2948) Wilken, C.; Bakes, W.; Mehlitz, I.; bensm. Forsch., 1985, 760, 496. CA 703(15):121816z. (2958) Wrolstad, Ronald E., Fluess. Obst, 1985, 52, 302, 306. CA103(13): 1036692. (2968) Xis, Xianming; Wu, Meiyun; Rao, Zeqing, Shipin Kexue (Beoing), 1985, 67, 1. CA703(3):21353c. (2978) Yamaizumi, 2.; Kasai, H.; Nlshimura, S.; Edmonds, C.; McCloskey, J., Mutat. Res., 1986, 173, 1. CA704(13):108002g. (2988) Yamazaki, T.; Inoue, T.; Yamada, T.; Tanimura, A.. Food Addit. Contam., 1986, 3. 146. CA705(2):12227d. (2998) Yamazaki. Takeshi; Ishiwata, Hajimu; Tanimura. A,, Eisei Shikensho Hdtoku, 1984, 102, 129. CAf03(11):86589d. (3008) Yen. Gow Chin, Chung Nung Yeh Hua Hsueh Hui Chih, 1986, 24, 211. CA103(11):86589d. (3018) Yip, George, J. Assoc. Off. Anal. Chem.. 1985, 68, 419. CA103(3):21310m. (3028) Yoneda. Y.; Hayashi, Y.; Shrokhi, M.; Hayashi, S., Shokuhin fisegakuZasshi, 1984, 25, 401. CA702(13):111654k. (3038) Yoshizawa, Takaml, Maikotokishin (Tokyo), 1984. 19, 8. CA 101( 19): 169120d. (3048) Zee, J. A.; Simard, R. E.; L'Heureux, L.,Lebensm. Technol., 1985, 78. 245. CA 703(17):140437t. (3058) Zenner, H. F.; Krzeminski, C., 2. Gesamte Hyg. Ihre Grenzgeb., 1984, 30, 622. CAf02(19):165315u. (3068) Zitko, V.. FoodScl. Technol, 1984, 1 1 , 533. CA101(17):149867z. (3078) Zyren, John; Elkins, Edgar R.. J. Assoc. Off. Anal. Chem.. 1985. 66,672. CA103(15):121824a. CARBOHYDRATES
(1C) Aaman, Per; Hesseiman, Klas Swed. J. Agric. Res., 1984, 14, 135. CA 702( 17): 147634t. (2C) ACHazmi, M. I.; Stauffer, K. R., J. Food Sci.. 1988, 51, 1091, 1097. CA 705(19): 1707023. (3C) Angelini, E.; Bonigli, C.; Mosca, M.; Bellomonte, G., Riv. Soc. Ital. Scl. Aliment., 1984, 13, 479. CA 102(23):202688r. (4C) Athnasios, Albert K., J. L i q . Chromatogr., 1984, 7, 1991. CAIOI1211: 187224~. ( 5 C j 'Baker, Doris, Cereal Foods World, 1985, 30, 389. CA103(13): 103522~. (6C) Baker, D.; Norris, K. H., Appl. Spectrosc.. 1985, 39, 618. CA103(11):86606g. (7c) BaUer, Friedrich; Stachelberger, Herbert, Chem ., Mikrobiol., Technol. Lebensm., 1984, 8, 129. CA701(15):128969u. (8C) Beach, Richard C.; Menzies, Ian, J. Dairy Res., 1986, 53, 293. CA 104 (19):167016n. (9C) Betschart, H. F.; Prenosii, J. E., J. Chromatogr., 1984, 299, 498. CA 101(19):169227u. (1OC) Settler, 8.; Amado, R.; Neukom, H., Mitt. Geb. Lebensmittelunfers. Hyg., 1985, 76, 69. CA 102(25):219699t. (11C) Beutler, Hans Otto, Methods Enzym. Anal., 1984, 6 , 484. CA102(9):75016t. (12C) Beutler, Hans Otto, Methods Enzym. Anal., 1984, 6, 356. CA102(9):75009t. (13'2) Beutler, Hans Otto, Methods Enzym. Anal., 1984, 6 , 119. CA702(9):74984v. (14C) Beutler, Hans Otto, Methods Enzym. Anal., 1984, 6 , 90. CA102(7):60876z. (1%) Beutier. Hans Otto. Methods Enzvm. Anal.. 1984. 6. 104. CA102(7):58809w. (16C) Beutler, Hans Otto, Methods Enzym. Anal., 1984, 6, 2. CA102f91:77340t. (17'6 Birch, G. G.. Analysis of Food Carbohydrate; Elsevier: England, 1985. CA 703(25):213729b. (18C) Cai, Xinyao; Zhu. Ye, Shipin Yu Fajko Gongye, 1985, 5. 9, 8. CA 104(7):49903b. (19C) Cirilli, G.; Clriiii, C. S. Aldana; Pulga, C.; Zaghini, L., Ind. Aliment. (Plnerolo, Italy). 1988, 25, 35. CA104(15):128358f. 120C) Clode. D. M.. Anal. Food Carbohvdr.. , . 1985. 125. CA103. (26):226704q. (21C) Collins. P. M.. Carbohydrates Serles: Chapman and Hall Chemistty Sourcebooks; Chapman and Hall, 1986. (22C) Deifel, A., Dtsch. Lebensm., 1985, 81, 209. CA103(21):177026j. (23C) Den Drijver, L.; Holzapfel. C. W.; Van der Linde. H.,J. Agric. Food Chem., 1986, 34, 758. CA 105(5):41348z. (24C) Dziedzic, S. Z.; Ireland, P. A., Anal. Food Carbohydr., 1985, 225. CA 103(25):213454h. (2%) Englyst, H. N.; Cummings, J. H., Frog. Biotechnoi., 1985, 373 CA 103(1):5213b. '
FOOD (26C) Fauks, Rlchard M.; Timms, Stephen E., Food Chem., 1985, 77, 273. (75C) Scherz, Heimo, 2. Lebensm. Forsch., 1984, 779, 17. CA701CA 703(11):86808j. (23):209 1681. (27C) Folkes, D. J.; Brodtes, A., Wucose Syrups: Sci. Technol., 1984, 197. (76C) Scherz, H., Lebensmitteichem. Gerichfl. Chem. 1985, 39, 32. CA 702(17): 147595f. CA 703(1):5083j. (77C) Scherz, Heimo, Z. Lebensm. Forsch., 1985, 181, 40. CA103(28C) Folkes, D. J., Anal. Food Carbdrydr., 1985, 91. CA 703(25):213452f. (29C) F m i , E.; Rizzoio, A.; Gargano, A., Tecnol. Aliment., 1984, 7, 38. (13): 10355Od. CA 707(15):128984v. (7%) Senkaiszky Akos. Eva; Petres, Joian; Czukor, Balint, Nelmiszervizsga (3OC) Fozy. Istvan; Horvath, Eva, Edesipar, 1988, 37, 38. ~ ~ 1 0 5 lsti Kozl., 1984. 30, 119. CA 703(7):52789d. (13): 113778n. (79C) Shallenberger, R. S. Anal. Food Carbohydr., 1985, 41. CA103(25):213450d. (31C) Frank, J. F.; Christen, G. L., J. Food Sci., 1984, 49, 1332. CAIOI(25):228584h. (8OC) Shidlovskii, V. P.; Verbitskaya, E. M., Molochn. Prom 1984, 29. CA 707( 17):149950w. (32C) Garcia, Eiisabeth; Cordenunsi, Eeatriz R.; LaJoio, Cienc. Tecnol. Aliment.. 1985. 5, 39. CA 705(3):23187k. (8lC) Simon, P. W.; Freeman, R. E., HorfScience, 1985, 20, 133. CA702(17): 147632r. (33C) Giangiacomo, Roberto; Duii, Gerald G., J. Food Sci., 1986, 57, 679. CA 705(7):59532q. (82C) Sjoberg, A. M.; Pyysaio, H., J. Chromatogr., 1985, 319, 90. CA102(1 1):94427u. (34C) Goetz, Heinz. Tec. Lab., 1985, 9, 236. CA703(23):195030k. (83C) Sumida, Mariko; Imoto, Hisae, Kenkyu Kiyo Konan Joshi Daigaku, (35C) (lossl, M.; Micco, C.; Chirico, M.; Arnoldi, C., Riv. SOC. Ita/. Sci. 1985. 576. CA 704(15):128264x. Aliment ., 1985, 74, 429. CA 704(25):223703y. (84C) Tamate, Jerry; Bradbury, J. Howard, J. Sci. Food Agric., 1985, 36, (3%) He, Zhaofan; Dan, Youliang; Miu, Aizhen, Shengwu Huaxue Yu Sheng1291. CA 704(13):108026t. wu Wull Jinzhan, 1985, 67, 74. CA103(1):5071d. (85C) Tawfik. Ahmed M.; Mardon, Christopher J., J. Sci. Food Agric., 1985, (37C) Hili, R. D., Munck, L., Eds.; New Approaches to Research on Cereal 36, 621. CA703(19):156727y. Carbohvdrates: Proa. In bio.. 1. Eisevier. 1985. CA 10317k52928v. (86C) Thier, H. P., Gums Stab. Food Ind. Appl. Hydrocoiloids, Proc. Int. (38C) Hob, J.; Bjoerck, I.; Drews, A.; Asp, N. G., Starch;Staerke: 1988, Conf., 1984. CA 707(23):209152z. 38, 224. CA705(13):113755e. (87C) Tsujisawa, Hiroshi; Yokoyama. Tsuyoshi, Wakayama Eisei Kogai (39C) Hughes, A.; Lindsay, R. C., J. Food Sci., 1985, 50, 1862. CA 704Kenkyu Senta Nenpo, 1984, 30, 66. CA 103(23):195026p. (3):18845e. (88'2) U, Zang. Kual; Kang, Soon Seon; Koh, Jeong Eun; Kim, Y. S.,Non(40C) Karkaias, John, J. Sci. Food Agric., 1985, 36, 1019. CA704munjip Cheju Taehk, 1985, 27, 33. CAf05(7):59519r. (9):67597j. (89C) Valdehita, Maria T.; Tenorio, Maria D.; Lequerica, E. M., An. Broma(41C) Kearsiey, M. W., Anal. Food Carbohydr., 1985, 75. CA103tol., 1984, 35,255. CA 702(5):44494t. (25):213449k. (9OC) Van Riel, J. A. M.; Oiieman, C., J. Chromatogr. 1986, 362, 235. (42C) Kbyn, Dick H., J. Dairy Scl., 1985, 68, 2791. CA703(23):195048x. CA 705(13):113736z. (43C) Knudsen, Ida M., J. Sci. Food Agric., 1986, 37, 560. CA705(91C) Voragen, A. G. J.; Schois, H. A.; Clement, A. J.; Piinick, W., J. (7):59533r. Gumsstab. Foodnd. Appl. Hydrocolloids, 1984. CA f07(21):189793d. Kobayashi, Shoichi; Schwartz, Steven J.; Lineback, D. R., J. Chroma(92C) Walter, Erhard, Z. Lebensm. Forsch., 1984, 179, 210. CAIOIfogr., 1985, 379, 205. CA702(13):111596t. (23):209224z. (45C) Koerner, Cathy A.; Nieman, Timothy A., Anal. Chem., 1986, 58, 116. (93C) Walter, Erhard; Kohier, Peter, 2.Lebensm. Forsch., 1985, 780, 121. CA 704(9):67582a. CA 702( 17):147637~. (46C) Kunerth, W. H.; Youngs, V. L., Cereal Chem., 1984, 67, 344. (94C) Wang, Tieiiang; Yang, Guangqi, Yingyanag Xuebao, 1985, 7, 157. CA lOl(15): 128965q. CA 103(25):213470k. (47C) Lanza, E.; Li, B. W., J. Food Sci., 1984, 49, 995. CA707(95C) Watanabe, E.; Endo, H.; Ikeda, Y.; Shibamoto, N., Nlppon Suisan (19): 169198k. Gskkaishi, 1988, 52, 711. CA105(5):38420m. (48C) Lawrence, James P.; Lyengar, Jagannath R., J. Chromatogr., 1985, (96C) Watanabe, Noriyuki, J. Chromatogr., 1985, 330, 333. CA703350, 237. CA 104(7):49933m. (17):137930t. (49C) Lercker, G.; Savioii, S.;Vecchi, M. A.; Sabatinl, A. G.; Nanetti, A,; Bachmann, M., Gums Stab. Food Ind. (97C) Wedlock, D. J.; Phillips, G. 0.; Plana, L., FoodChem., 1988, 79, 255. CA704(21):184971n. Appl. Hydrocolbids, 1984. CA 101(21):189794e. (50C) Macrae, R., Anal. Food Carbohydr., 1985, 61. CAI03(25):213451e. (98C) Wenbck, Robert W.; Siveii, Lorna M.; Agater, I., J. Sci. Food Agric., (5%) Mardai, V. N.; Lyashenko, A. A.; Petrenko, A. A.; Lipets, A. A,, Sakh. 1985.36. 113. CA 702(15):130548v. Prom, 1985, 4, 34. CA 702(25):219708v. (99C) Xie. 0.; Zheng. P.; Han, L.; He. Y., Yuzhen, Fenxi Huaxue, 1986, 74, 134. CA 705(7):59506j. (52C) Matsumoto, K.; Hamada, 0.; Ukeda, H.; Osajima, Y., Anal. Chem., 1986, 58, 2732. CAI05(19):170695j. (1OOC) Yasui, Takeshi, J. Sci. Food Agric., 1986, 37, 491. CA105(3):23 17 lg. (53C) Matsumoto, K.; Hamada, 0.; Ukeda, H.; Osajima, Y., Agric. Bioi. Chem., 1985, 49, 2131. CA703(17):140423k. (101'2) Zheng, Shengiian; Guo, Liqing, Zhongguo Niangzao, 1985, 1 , 32. CA 703(19): 159 188j. (54C) Medlicott, Andrew P.; Thompson, Anthony K., J. Scl. Food Agric., 1985, 36,561. CA103(19):159352h. (102C) Zhu, An; He, Yuzhen; Hania; Sha, Yixian; He, Huizhu, Shengwu Huaxue Y Shengwu Wuli Jinzhan, 1984, 60, 41. CAf02(25):219744d. (55C) Melton, L. D.; Laas, A. M., N. 2.J. Technol., 1985, I , 191. CA704(17): 147263n. Saito, M.; Okuda, J.; Ishihara, H.; Tejima, S.,Eisei Kagaku, (56C) Miwa, I.; COLOR 1984, 30, 238. CA 102(3):22961r. (57C) Moinar-Perl, I.; Pinter-Szakacs, M.; Kovago, A,; Petroczy, J., J. Chro(1D) Amakawa, A.; Hirata, K.; Ogiwara, T.; Ohnishi, K., Buneseki Kagaku, 1964, 33. 586. CA 102(3):22932g. matogr., 1984, 295, 433. CA 707(21):189795f, (2D) Bailey, John E., Jr.; Bailey, Catherine J., Talanfa, 1985, 32, 875. (58C) Nebytov, V. G.; Davydov, V. Ya.; Zinchenko, V. A., S Biol., 1984, 12, CA10413k18694e. 104. CA 102(9):75107y. --- (3D) Iversen, Arve J.; Palm, Torgny, Appl. Spectrosc., 1985. 39, 641. (59C) Ohtsuki, KOZO; Kawabata, Makoto; Taguchi, Kuniko, Kyoto Daigaku CA 703(11k86607h. Gakujufsu Hokoku, 1985, 36,31. CA 705(11):96128h. (4D) Kamiku;al Mieko; Nakazato, Keiko, Shokuhin Eiseigaku Zasshi, 1985, (6%) Ohtsuki, Kozo; Kawabata, Makoto; Taguchi, Kuniko, Kyoto Daigaku 26, 150. CA103(21):177142u. Gskkujufsu Hokoku, 1984, 35,21. CA 703(3):21326w. (5D) Kanda, Hiroshi, Shokuhin Eisei Kenkyu, 1985, 35, 813. CA104(61C) Paynter, Valerie A.; Neubauer, Debbie; Ladenburg, Kurt, J. Chroma(11):87199). togr. Sci., 1986, 24, 170. CA704(23):205630t. (6D) Khachik, Frederick; Beecher, G. R.; Whittaker, N., J. Agric. Food (62'2) Petrzika, M.; Linow, F., Nahrung, 1985, 29, 927. CA103Chem ., 1988, 34, 603. CA 105(5):41487u. (25):2 134851.1. (7D) Kobayashi, F.; Ozawa, N.; Hanai. J.; Isobe, M.; Watabe, T., Anal. (63C) Picha, David H., J. Food Sci., 1985, 50, 1189. CA103(9):69892e. Chem., 1986, 58, 3048. CAfO5(21):189554). (64C) Pigman, W., Woiffrom. M. L., Eds.; Advances in Carbohydrate Chem(ED) Mader, Pavel; Chiadova, Jarmiia, Proc. Int. Symp. Capillary Chromaistry and Biochemistry; Voi. 42 Ser. Publication Ser., Acad. Pr., 1984. togr., 1985, 6th, 555. Edite, CA 103(17):140644h. CA 702(20):168599a. (9D) Puttemans, Marc L.; Dryon, Louis; Massart. Desire, J. Assoc. Off. (65'2) Pirisino, James F., Food Scl. Techno/., 1984, 71 (Food Const. Food Anal. Chem., 1984, 67, 880. CA707(23):209199~. Residue), 159. CA 707(17):149859y. (1OD) Rahmani, M.; Csaiiany, A. Saari, Rev. Fr. Corps Gras, 1985, 32(61), (66C) Podgorska, Zofia, Przem. Spozyw., 1986, 40, 29. CAIO5257. CA 703(23):195025n. (17): 151614r. (11D) Ushiyama, H.; Nishijima, M.; Yasuda, K.; Kamimura, H.; Tabata, S.; (67C) Praznik, W., Ernaehrung (Vienna), 1985, 9, 843. CA704Matsumoto, S.; Nishima, T., Kenkyu Nenpo, 1984, 219. CAfO2(15): 128281a. (23k2027 16v. (68C) Rathbone, Einer B., Anal. Food Carbohydr., 1985, 149. CA103(12D) ' Yang, hying; Gao, Hejuan, Shipin Yu Fajlao Gongye. 1985, 9. (25):213453g. CA 704(5):33115k. (69C) Reimerdes, E. H.; Reisewitz, I., Fresenlus' 2.Anal. Chem., 1984, (13D) Ye, Shibai; Han, Huixin; Chem., Yanhua; Qui, Hai, Shipin Kexue (Bei318, 283. CA701(15):128972q. iino). 1985. 67. 48. CA 10417):49896b. (70C) Reimerdes, E. H.; Rothkitt, K. D., Fresenius' 2.Anal. Chem., 1984, (14D)"'Yin. P&yu;'Chen, Libing,' Sepu, 1985, 2, 201. CA 104(7):4991IC. 378, 220. CA701(15):128912v. (15D) Zioch, Zdenek, Kvasny Prum., 1985, 3 1 . 58. CAf03(5):36273a. (71C) Reimerdes, Ernst H.; Rothkitt, K. D., GIT Fachz. Lab., 1984, 28, 97. CA IOZ(lk4539e. ENZYMES (72C) Rekerdes,Ernnst H.; Rothkitt, K. D., 2. Lebensm. Forsch., 1985, 781. 408. CA 10413k187030. (1E) Bergmeyer, H. U., Bergmeyer, J., Grassi, M., Eds., Methods of Enzy(73C) Ruggeri, P.; 'Fonseca: G., Latte, 1985, 70, 1050. CAf04matic Analysis, 3rd ed.; Veriag Chemie: Weinheim, Deerfield Beach, FL, (13): 107999a. 1984; Voi. 5. (74C) Saucerman. Janice R.; Winstead, Charles E., J. Assoc. Off. Anal. (2E) Birkeiand, Stein Erik; Stepaniak, L.; Soerhaug, T., Appl. Environ. MicroChem., M84, 67, 899. CA 707(25):228587m. biol.. 1985, 49, 382. CAfO2(13):108539w.
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ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
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FOOD (3E) Carlson, Alfred; Hill, Charles G., Jr.; Olson, N., J. Dairy Sci., 1985, 68, 290. CA102(19):165332x. (4E) Carlsson, M.; Larsson-Razniklewicz, M., Salamonsson, L., Cafa Chem. Scand., Ser. 8.1988, 840(5), 394. CA705(11):93303a. (5E) Cartier, P.; Chiiliard. Y.; Chazal, Marie Paule, Lait, 1984, 64(640) 340. CA 70217k60863t. , (6E) Cinco, F. J.: Freis, J. M ; Holt, D.; Rupnow, J., J . Food Sci., 1985, 50, 533 CA 102(17):147766n. (7E) Dalling, M. P., Ed., Plant Proteolytic Enzymes; CRC Press: Boca Raton, FL. 1986: Vol 1. (8E) De Palozzo, Aura Lopez; Caliejas, Antonio, Acta Client. Venez.. 1984, 35(5-6), 448. CA 702(23):202710s. (9E) Demmer, W.; Werkmeister, K., Arch. Lebensmifteihyg., 1985, 36, 15. CA 702(21):183913s. (IOE) Finney, P. L., Cereal Chem. 1985, 62, 258. (11E) Fretzdwff, Barbara, Veroeff. Arbeitsgem. Getreideforsch. 1985, 798(Ber. Tag. Getrldechem., 35th, 1984). 179-81. CA703(17):140404e. (12E) Fukal, Ladislav; Kas, Jan; Kasafirek, Evzen, Sb. Vys. Sk. Chem. Praze, Potraviny, 1985, €58, 103. CA105(3):23165h. (13E) Gottesmann, Peter; Hamm, Reiner, Fleischwlrtschaff, 1985, 65, 591. CA 103(7):52850s. (14E) Haslbeck, Franz; Senser, Friedrich; Grosch, Werner, Z.Lebensm.-Unters. Forsch., 1985, 181, 271. CA703(25):213525g. (15E) Herrmann, Heinrich; Krause, Wolfgang, Patent, 1984. CA 103131: \ , 19094a. (16E) Jensen, S. A.; Munck, L.; Kruger, J. E., J. Cereal Sci., 1984, 2(3), 187-201. CA 701(17):147140h. (17E) Kwee, W. Seng, Aust J . Dairy Technol. 1985, 40, 27. CA103(211:177029n. (l8E) 'Linfield, Warner M.; Serota, Samuel; Sivieri, L., JAOCS, J. Am. Oil Chem. SOC. 1985, 62, 1152. CA703(11):83886n. (19.9 Majeed, G. H.; Ernstrom, C. A., J. Dairy Sci., 1985. 68, 1936. CA 703( 17): 140419p. (20E) Meckeljar, Robin C.: Cholette, Hilaire, J . Dairy Res., 1986, 53, 301. CA 704 (19):167017p. (21E) Murthy, Gopala K.; Peeler, James T.,J . Assoc. Off. Anal. Chem., 1988, 69, 658. CAl05(11):96134g. (22E) Paggi, G.; Pancini, R.; Giannelli, R.; Barbaro, D.; Gentiii, S . , Sci. Tec. Latt.-Caseria, 1984, 35, 201. CA707(23):209227c. (23E) Paggi. G.; Panclni, R.: Sbernini, F.; Barbaro, D.; Gianelli, R., Latte, 1985, 10, 214, 218. CA102(21):183850u. (24E) Paquette, G. J.; McKellar, R . C. J . Food Sci.. 1988, 51, 655. CA705( I 1):96112y. (25E) Saunders, R. M.; Heltved, F.. J. Cereal Sci., 1985, 3, 79. CA703(3):21320q. (26E) Stead, Donald, J. Dairy Res., 1984, 57, 623. CA101(23):209171e. , I.; Zemek, J., Lebensmitfeiindustrie, (27E) Taeufel, A.; Gabor, R 1986, 33, 65. CA705(9) (28E) Van den Noortgaete, C. H.. Cerevisiae, 1986, 11, 45, 49. CA 105(9):77634d. (29E) Wasserman, Bruce P.; Wagner, Jeffrey D., Biochem. Educ., 1985, 13, 84. CA703(5):36767q. (30E) Yada, Rickey Y.; Nakai. Shuryo, J . Agric. Food Chem., 1986, 34, 675. CA 705(5):37964e.
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FATS, OILS, AND FAlTY ACIDS
(IF) AbdeCMoety, E. M.; Ahmad, A. K. S.; Sharaf El-Din, M., J. Assoc. Off. Anal. Chem., 1988, 69, 67. CA104(11):87240r. (2F) Adolf, R. 0.; Emken, E. A., JAOCS, J . Am. OiiChem. Soc., 1985, 62, 1592. CA703(25):213529m. (3F) Agienko. K. S.; Nikitina, L. I . ; Kukota, G. N. Moiochn. Prom, 1986, 6 , 28. CA 705(21):189683a. (4F) Ajana, H.; Perrin, J. L.; Prevot, A., Rev. F r . Corps Gras, 1988, 33, 19. CA 104(25):223708d. (5F) Arai, Fumitada; Osada, Chiaki; Katsuyama, Shunkai, Cienc. Technol. Aliment., 1988. CA 104(23):203480v. (6F) Araulo, Julio M. A.: Pratt. Dan E., Cienc. Technol. Aliment. 1985, 5 , 57. CA 705(1):5254g. (7F) Arens, M.; Kroll, Edith, Fetfe, Seifen, Anstrichm., 1985, 87, 467. CA 10419k67603h. >-, - --(8Fj Asano, Ichiro; Matsushita, Setsuro, Nippon €~YO, Shokuryo Gakkaishi, 1984. 37. 273. CA7011151:128963n. (9F) Athnasios, A. K.; Heaiy, E. J.; Gross, A. F.; Templeman, G. J., J. Assoc. Off. Anal. Chem., 1986, 69, 65. CA104(11):87239x. (IOF) Bannon, Cecil D.; Craske, John D.; Hilliker, A. E., JAOCS, J . Am. Oil Chem. SOC.,1985, 62, 1501. CA103(25):213487w. (11F) Bengtsson, Lena, Fette, Seifen, Anstrichm., 1985, 87, 262. CA703(11):86612f. (12F) Bhati. A.; Benbouzid, M.; Hamilton, R . J.; Sewell, P. A,, Chem. Ind. (London). 1986, 2 , 70. CA104(11):87225a. (13F) Bianchini, J. P.; Gaydou. E. M.; Slgoillot,'J. C., J. Chromatogr., 1985. 329, 23 1. CA 1O3(13): 10 1430r. (14F) Bird, R.; Evans, M. 6. Chromatographia, 1984, 79, 180. CA102f23k202709v. (156 ~ ~ U & n t t k l ,Michael Mark; Stockler, Jerry Ronald, JAOCS, J. Am. Oil Chem. SOC., 1985. CA704(17):147479n. (16F) Blumenthal, M. M.; Stockler, J. R.; Summers, P. J., JAOCS, J. Am. Oil. Chem. Soc., 1985, 62, 1373. CA103(19):159214q. (17F) Boniforti, L.; Lorusso, S.;Chlaccherini, E.; Mariani, C.; Fedeli, E.. Riv. Ital. Sostanze Grasse, 1985, 62, 455. CA104(13):107997y. (18F) Bradley, Robert L., Jr., J. Assoc. Off. Anal. Chem. 1986, 69, 831. CA 705(21):189576t. (19F) Brumely, W. C.; Sheppard, A. J.; Rudolf, T.S.; Shen, C.: Shang, J.; Yasei. P.: SDhOn. J. A.. J. Assoc. Off. Anal. Chem.. 1985. 68. 701 CA m ( 2 3 ) :i95021h (20F) Cao, Xide, Dai, Chaozheng. Sepu, 1985, 2. 42. CA103(3):21297n
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(21F) Chaouch, A.; Michel, M.; Dordonnat, J. M.; Tisse, C.; Lesgards, G., Ann. Falsif. Expert. Chim. Toxicol., 1985, 78, 383. CA704(23):205635y. (22F) Chaveron, Henri; Verdola, Christlne. Ann. Faisif. Expert. Chim. Toxicol., 1984, 77, 401. CA702(19):165324w. (23F) Chaveron, H.; Verdola, C.; Meili, M., Ann. Falsif. Expert. Chim. Toxicol., 1984, 77, 571. CA703(13):103547h. (24F) Christie, William W.; Noble, Raymond C., Food Sci. Technoi., 1984, 71 (Food Const. Food Residues), 1. CAlO7(17):149857w. (25F) Christie, William W.; Connor, Kevin; Noble, Raymo, J. Chromatogr., 1984, 298, 513. CA701(17):147094w. (26F) Chriistopoulou, Constantha N.; Perkins. Edward G., JAOCS, J. Am. Oil Chem. SOC., 1988, 63, 679. CA705(1):5272m. (27F) Conway, J.; Ratnayake, W. M. N.; Ackman, R. G., JAOCS, J. Am. Oil Chem. SOC., 1985, 62, 1340. CA703(19):159212n. (28F) Cotton, Robyn M., N. 2. J. Dairy Sci. Technol., 1984, 19, 267. CA 102(16):137462w. (29F) Croon, L. B.; Rogstad, Astri; Leth, T.; Kiutamo, T., Fetfe, Seifen, Anstrichim., 1986, 88, 67. CA704(21):184973q. (30F) Croon, L. B.; Kiutamo, T.; Leth, T.; Rogstas, A., Proc. Scand. Symp. Lipids, 72th, 1983, 1984, 53. CA703(25):213536m. (31F) Crudglngton, D. R., J. Assoc. Pubiic Anal., 1985, 23. 103. CA104(15):1 2 8 3 3 5 ~ . (32F) Davies, Anthony M. C.; Brocklehurst, Timothy F., J. Sci. Food Agric., 1986. 37, 310. CA704(21):184969t. (33F) De Koning, A. J.; Evans, A. A.; Heydenrych. C.; Wessels, P. H., J . Sci. Food Agric., 1986, 36, 177. CA702(23):20284lk. (34F) Defour, J., Chem. Mag. (Ghent), 1985, 71, 32, 35. CA104(9):67602g. (35F) Deman, J. M.; Gupta, S.;Kloek, M.; Timbers, G. E.; JAOCS, J. Am. Oil Chem. SOC., 1984, 61, 1569. CAlO7(21):189831q. (36F) Demirbas, Ayhan, Kim. Sanayi, 1984, 27, 77. CA702(17):146161z. (37F) Dupuy, H. P.; Flick, G. J., Jr.; Balley, M. E.; St. Angelo, A. J.; Legendre, M. 0.; Sumrell, G., J. Am. Oil Chem. SOC., 1985, 62, 1690. CA104(7):49913e. (38F) Fiebig, H. J., Fefte, Seifen, Anstrichim., 1985, 87, 53. CA702(20):168633g. (39F) Fischer, K. H.; Grosch, W., Lipid Oxid.: Biol. Food Chem. Aspects, Contrib. LIPIDFORUMISIK Symp., 7985, 1986, 125. CA104(25):223769z. (40F) Fischer, Karl Heinz; Laskawy, Gudrun; Grosch, W., 2.Lebensm. Fors ch., 1985, 787, 14. CA103(13):103548j. (41F) Fletcher, D. L.; Brltton, W. M.; Cason, J. A,, Poult. Sci., 1984, 63, 1759. CA 10l ( 2 1):189814m. (42F) Fozy. Istvan, Mrs.; Horvath. Eva, Desipar, 1985, 36, 97. C A W (11):87250u. (43F) Frankel, E. N.; Neff, W. E.; Selke, E., Lipids, 1984, 79, 790. CA101(25):228756r. (44F) Fraser, M. S.; Franki, G., JAOCS, J. Am. Oil Chem. Soc., 1985, 62, 113. CA1021131:111553b. (45F) Frede, E;'Precht, D.; Timmen, H., Milkfat its M o d i f . . Contrib. LIPIDFORUM Symp., 1984, 1985, 32. CA103(23):195139c. (46F) Frsde, E., Chromatographia, 1986, 27, 29. CA705(13):113726w. (47F) Frega, N.; Lercker, G., Riv. Itai. Sostanze Grasse, 1984, 67, 385. CA . 10217k60817f. (48F) Jujimoto, Nobukunl; Katai, Masaaki; Meguri, Haruo, Bunseki Kagaku , 1988, 35, 482. CA 105(19):170693g. (49F) Gambhir, P. N.; Agarwala, A. K. JAOCS, J . Am. Oil Chem. SOC., 1985. 62. 103. CA102f9):77350w. (50F) &era&, E.; De Schepper, D., Anal. Chem. Symp. Ser., 1984, 21. 287. CA701125k228595n. (51F) Geeraert.' E.: Sandra, P., Proc. I n f . Symp. Capiilary Chromatogr.. 1985, 6. 174. CA104(21):184945g. (52F) Geeraert, E.; Sandra, P., HRC CC, J. High Resoiut. Chromatogr. Chromatogr. Commun., 1985, 8, 415. CA704(3):18699k. (53F) Gegiou, D.; Staphylakis, K., JAOCS, J . Am. Oil Chem. Soc., 1985. 62. 1047. CA103(13k103518z. (54F) 'Gere, Anna; Gekz,' C.; Morin, Odile, Rev. Fr . Corps Gras . 1984, 3 7 , 34 1. CA 102(13):111588s. (55F) Gildenberg, Lawrence; Firestone, David, J. Assoc. Off. Anal. Chem., 1985, 68, 46. CA102(21):183835t. (56F) Goh,S.H.; Tong, S.L.; Gee,P. T..JAOCS, J. Am. Oil Chem. SOC., 1984, 67, 1597. CA101(23):209222x. (57F) Goh, S. H.; Choo, Y. M.; Ong, S.H., JAOCS, J. Am. Oil Chem. Soc. 1985, 62. 237. CA702(15):130493y. (56F) Gomes. T.; Catalano, M., Agrochimica, 1985, 29, 281. CA105191:776461 . - .(59F) Graciin Tous, J.; Pocklington, W. D.; Hautfenne, A,, Pure Appl. Chem. 1986, 58, 1023. CA105(11):96123c. (60F) Gray, J. I., AOCS Monogr., 15 (Flavor Chem. Fats Oils), 1985, 75, 223. CA105113~:113670v. (61F) Grover, M: R.'; Sarma,*N. V.; Mathew, T. V., Res. Ind., 1985, 30, 40. CA 103U7):140405f. (62F) &n, Janqiu; Xiao, Yanwen; Zhang, Jle, Fenxi Huaxue, 1984, 12, 484. CA 102(3):22965v. (63F) Hall, Ounnar, Lipidoxid.: Bbl. FoodChem. Aspects, Contrib. LIPIDFORUM/SIK Symp., 7985, 1986, 96. CA705(1):5215v. (64F) Hall, G.; Lingnert, H., Dev. Food Sci., 1986, 72, 735. CA105(15): 132412g. (65F) Hamilton, R. J., Rossell. B. A., Eds.. Analysis of Fats and Oils; Elsevier: England, 1986. CA 705(3):23341n. (66F) tiara, Setsuko; Yamawaki, Hideki; Totani, Yoichiro, Yukagaku, 1984, 33. 594. CA 102f21:8563f. (67F) Herslof, Bengi; 'Kindmark. Gunilla, Lipids, 1985, 20, 783. CA104(5):33130m 3
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FOOD (68F) Hibino, Hidehiko; Fukudo, Nobuo; Kudo, Kiyoshi, Yukagaku, 1985, 34, I. 1. 1. .. CA - . . 702123):200532m. . .(69F) Hibino, H.; Makino. T.: Maeno, T.; Ozawa, A., Yukagaku, 1985, 34, 371. CA 103(7):52778z. (70F) Hirata, H.; Hguchi, K.; Ishikawa, K.; Nakasato, S., Kagaku GJustu k Enkyusho Hokoku, 1986, 87, 7. CA105(14):126461f. (71F) Hoien. Boerge, JAOCS. J. Am. Oil Chem. SOC., 1985, 62, 1344. CA 703 ( 19): 159213~. (72F) Homberg, Eifriede, Dtsch. Lebensm., 1985, 8 1 , 12. CA102(15):130522g. (73F) Homer, David, Proc. Scand. Symp. Lipids, 12th, 1983, 1984, 213. CA 104(5):33119q. (74F) Homer, David Milkfat its Modif ., Contrib. LIPIDFORUM Symp ., 1984, 1985, 172. CA103(23):195047w. (75F) Horstrnann, P.; Montag, A., Fette, Selfen, Anstrichm., 1986, 88, 262. CA 105(15): 1322563. (76F) Hurst, W. Jeffrey; Martin, Robert A,, Jr., JAOCS, J. Am. Oil Chem. SOC., 1984, 61, 1462. CA 707(23):209179p. (77F) Hurst, W. Jeffrey: Aieo, M. D.; Martin, Robert A,, J. Agric. Food Chem., 1985, 33, 820. CA103(19):159173a. (78F) Hwang, K. S.; Mawer, W. S . ; Nam, Y. J.: Min, B. Y., Han'guk Sikp'um Kwahakhoechi, 1984, 16, 348. CA 102(1):4528a. (79F) Indyk, H.; Wooilard, D. C., J. Chromatogr., 1988, 356, 401. CA104(25):223709e. @OF) Ishiguro, Masataka; Namba, Shigeru; Nakatsu, A., Kanzei Chuo Bunsekishoho, 1985, 25, 95. CA103(13):103538f. (81F) IUPAC Commission on Oils, Fats and Derivatives; Appl. Chem. Div., IUPAC, Pure Appl. Chem., 1985, 57, 899. CA103(9):69871x. (82F) IUPAC Commission on Oils, Fats and Derivatives; Appi. Chem. Div., IUPAC, Yukagaku, 1986, 35, 472. CA705(11):96123c. (83F) IUPAC Commission on Oils, Fats and Derivatives; Appi. Chem. Div., IUPAC, Pure Appl. Chem., 1986, 58, 1419. CA 105(21):189567r. (84F) Jaky, Miklos, Olaj, Szappan, Kozmet., 1984, 33, 97. CA703(2):7982a. (85F) Jonker, D.; Van der Hoek, G. D.; Glatz, J. F.; Homan, C.; Posthurnus, M. A.; Katan, M. B., Nutr. Rep. Inc., 1985, 32, 943. CA 704(7):49899e. (86F) Kamata, Tsuneo, Yukagaku, 1985, 34, 1017. CA104(19):166975n. (87F) Kamata, Tsuneo, Yukagaku, 1985, 34, 36. CA102(11):94430q. (88F) Kato, Tokinobu; Iwamoto, Kazuro, Kanzei Chuo Bunsekishoho, 1985, 25, 9. CA103(11):86611e. (89F) Kawai, Nobuko; Nakayama, Yukuho; Sasaki, Kiyoshi, Yukagaku, 1985, 34, 921. CA 104(5):33157a. (9OF) Kershaw, Stephen J., J. Sci. FoodAgric., 1966, 37, 267. CA104(19):167027s. (91F) Kihara, Kazuko; Rokushika, Souji; Hatano, Hiroyuki, Bunseki Kagaku, 1984, 33, 674. CA102(17):147624q. (92F) Kikugawa. K.; Nakahara, T.: Taniguchi, Y.; Tanaka, M., Lipids, 1985, 20, 475. CA103(13):103529d. (93F) Koiarovic, L.; Traitier, H.; Ducret, P., J. Chromatogr., 1984, 314, 233. CA - 702(51:44480k. .(94F) Kopp, J.; Ronnet. M.: Renou, J. P., Spectra, 1988, 710, 37. CA105f13k113677i -(95F) Korynova, I.N.; Lur'e. I. S., Khlebopek, Konditer. Prom 1985, 3, 35. CA 102(25):219687n. (96F) Kou. I Ling; Holmes, Ross P., J . Chromatogr., 1985, 330, 339. CA 103(17):140424m. (97F) Krishnamurthy, Mahishi, N.; Rajaikshmi, S.; Kapur, J. Assoc, Off. Anal. Chem., 1985, 68, 1074. CA104(7):49916h. (98F) Kroli, Edith; Seher, A,, Fette, Seifen, Anstrichm., 1986, 88, 357. CA 105(19):170742x. (99F) Lambeiet, P.; Desarzens, C.f Raemy, A., Lebnsm. Technol.. 1986, 19. 77. CA705(11):96125e. (IOOF) Lang, Johanna; Ceiotto, Claude; Esterbauer, H., Anal. Biochem ., 1965, 150, 369. CA703(23):192547y. (101F) Lee, Ken; Herian, Anne M.; Richardson, T., J. FoodProt., 1984, 47, 340. CA 101(21):189782z. (102F) Lee, Theresa W., JAOCS, J . Am. OilChem. SOC.,1986, 63, 317. CA 104 (17):147295z. (103F) Lercker, G.; Caboni. M. F., Riv. Ital. Sostanze Grasse, 1985, 62, 193. CA 104(15): 1282774. (104F) Leung, H. K.; Anderson, G. R.; Norr, P. J., J. Food Sci., 1985, 50, 942, 950. CA 103(9):69888h. (105F) Lin, K. C.; Marchello, M. J.; Fischer, A. G., J. Food Sci., 1984, 49, 1521. CA 102(1):4622b. (106F) Linfield, Warner M.; Serota, Samuel; Sivieri, L., JAOCS, J. Am. Oil Chem. SOC., 1985, 62, 1152. CA103(11):83886n. (107F) Lu, Hannan; Yang, Luoquing; Qiu, Zeguang, Shipin Yu Fajiao Gongye. 1985, 22. CA103(17):140416k. (108F) Luf, W., Milchwirtsch. Ber. Sundesanst. Wolfpassing Rotholz. 1984, 80, 247. CA102(1):4506s. (109F) Maerker, G.; Unruh, J., Jr., JAOCS, J. Am. Oil Chem. SOC.,1986, 63, 767. CA 105(9):77649n. (llOF) Magak'yan, D. T.; Shishkin, N. I., Tr. Erevan. Zoovet. Inst., 1984, 56, 34. CAIO2(13):111756v. (111F) Mallet, G.; Dimitriades, Catherine; Ucciani, E., Rev. F r . Corps Gras., 1985, 32, 439. CA 104(21):184949m. (112F) Mariani, C.; Fedeli, E., Riv. Ital. Sostanze Grasse, 1985, 62, 3. CA 103(15):121946s. ( I 13F) Marjanovic, Nikola; Jankovits, Istvan; Sagorac, M., Techno/. Mesa, 1985, 26, 70. CA 103(17):140434q. (114F) Marjanovic, N.; Jankovits, I.; Turkulov, J.; Kariovic. G.; Caric, M.; Milanovic, S.; Zagorac, M., Mljekarstvo, 1984, 34, 87. CA101(17):149958e. (11%) Martinez-Castro, I.; Alonso, L.; Juarez, M., Chromatographia, 1986, 21, 37. CA105(11):96118e. .--I
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(116F) Martovshchuk, V. I.; Mgebrishviii, T. F.; Martovshchuk, E., Maslo Prom, 1986, 7, IO. CAI05(17):151838b. (117F) Maruyama, Kazushige; Yonese, Chizuo, J A W S , J Am. Oil Chem . SOC. 1986. 63. 902. CA105(13):113734x. (1 18F) Masoom, M.; Townshend,'Alan, Anal. Chlm. Acta, 1985, 174, 293. CA 103(25):2 10139y. (119F) Masson, Lilia; Martinez, MarRza, Bull. Fed. Int. Lait.. 1984, 177, 157. CA 103121): 177028m. (120F) Matsui, Masami; titsuwa, Takaharu; Hine, Takashi, Shlmadzu Hyoron. 7983, 1984, 40, 235. CA104(2):14284y. (121F) Matsumoto, K.; Yoshida. H.; Ohta, K.; Tsuge. S , Org. Mass Spectrom., 1985, 20, 777. CA104(7):49932k. (122F) Maxwell, Robert J.; Mondimore, Donna; Tobias, J., J Dairy Sci., 1986, 69, 321. CA104(19):167010f. (123F) Mikuia, Mario; Khayat, Aii, JAOCS, J. Am. Oil Chem SOC., 1985, 62, 1694. CA104(5):33158b. (124F) Misir, R.; Laarveid, B.; Blair, R.,J. Chromatogr., 1985, 331, 141. CA 103(17):140422j. (125F) Miteva, E., Vet. Nauki, 1984, 21, 94. CA102(11):94411j. (126F) Monaceiii, R.: Dei Giovine, L., Rass. Chim. 1984, 36, 285. CA102(19):165306s. (127F) Moneam, N. M. A.; Ghoneim, T., J. Chromatogr., 1986, 361, 391. CA 105(9):77660j. (128F) Mordret, F.; Coustille, J. L.; Taconne, L., Rev. F r . Corps Gras, 1984, 31, 503. CA702(21):183817p. (129F) Mordret, F.; Morin, 0.; Coustiile, J. L., Rev. F r . Corps Oras. 1985, 32, 193. CA103(15):121806w. (130F) Morisaki, S.; Tsubone, N.; Fuchi, Y.; Mizokoshi, T.; Yamada, K., Oifa Kogai Eisi Senta Nenpo, 1985, 12, 23. CA 104(25):223772v. (131F) Mrugasiewicz, K.; Mscisz, A,, Herba Pol., 1984, 30, 97. CA10419):65 157s. (132F) Murata, Takeshi; Takahashi, Seiji, Shimadzu Hyoron, 1985, 42, 213. CA 105(7):59521k. (133F) Nagao, A.: Uozumi, J.; Iwamoto, M.; Yarnazaki, M., Yukagaku, 1985, 34, 257. CA102(25):219697r. (134F) Nasiruilah; Kapur, 0. P., J. Oil Technoi. Assoc. India (Bombay), 1965, 17, 37. CA104(16):131906p. (135F) Naudet, M.; Hautfenne, A., Rev. F r . Corps Gras, 1986, 33, 167. CA 105(15):130129w. (136F) Nazer, Jamii M. A.; Young, Clyde T.; Giesbrecht, F. G., J. Food Sci., 1985, 50, 1095. CA103(9):69890c. (137F) Netting, A. G., JAOCS, J. Am. Oil Chem. SOC., 1986, 63, 1197. CA105(21~189571n. (138F) Park, S. Won; Addis, P. B., J. Food Sci., 1985, 50, 1437. CA 103(2i):177044p. (139F) Petersson, B., Fette, Seifen, Anstrichm., 1986, 88, 128. CA105(3):23169n. (14OF) Petersson, B.; Anjou, K.; Sandstroem, L., Fette, Seifen, Anstrichm., 1985, 87, 225. CA 103(9):69884d. (141F) Phillips, F. C.; Erdahi, W. L.; Schmit, J. A,; Privett, 0. S., Lipids, 1984, 19, 880. CA 102(3):22951n. (142F) Pisareva, N. A,; Zhakevich, M. L.; Vasiievskii, B. S.; Sergeeva, T. V.; Kharenko, E. N., Tekhnol. Rybn. Prod., 1984, 94. CA104(1):4714z. (143F) Pocklington, W. D.; Hautfenne, A,, Pure Appl. Chem., 1985, 57, 1515. CA 103(19): 159198n. (144F) Podiaha, Oidrich; Toeregaard, Bengt; Pueschi, B., Lebensm. Techno I . , 1984, 17, 77. CA101(21):189965m. (145F) Pokorny, J.; Vaientova, Helena; Davidek, J., Nahrung, 1985, 29, 31. CA 102(19): 165320s. (146F) Pyysaio, H.; Enqvist, J.; Sandholm, J.; Sunila, P., Proc. Scand. Symp. Lipids, 12th, 1983, 1964, 12, 11. CA104(11):87192b. (147F) Ratnayake, W. M. N.; Ackman, R. G.,Can. Inst. Food Sci. Technol. J., 1985, 18, 284. CAl04(9):67615p. (148F) Recseg, Kataiin; Jeranek, Maria, O&j, Szappan, Kozmet., 1986, 35, 45. CA105(11):96145m. (149F) Reineccius, Gary A,, AOCS Monogr., 1985, 15, 263. CA105(13):113672a. (150F) Renou, J. P.; Kopp, J.; Valin, C., J. Food Technol., 1985, 20, 23. CA lOZ(13):111609z. (151F) Ritchie, A. S.; Jee, M. H., J. Chromatogr., 1985. 329, 273. CA103(13): 101184p. (152F) Robinson, J. L.; Macrae, R., J. Chromatogr., 1984, 303, 386. CA 10 1(24):221799y. (153F) Rosenthal, Ionei; Merin, Uzi; Popei, G.; Bernstein, S., J. Assoc. OM. Anal. Chem., 1985, 68, 1226. CA104(5):33161x. (154F) Rosseli, J. 8.; King, B.; Downes, M. J., JAOCS, J. Am. Oil Chem. SOC., 1985, 82, 221. CA102(13):111769b. Errnakova, T. P.; Kieshko, G. M.; Andronov, V. F.; (155F) Ryseva, L. I.; Burkov. G. I., Khlebopek, Kondlter, Prom-st., 1986, 3, 37. CA104(2333205763~. (156F) Sato. Tomonobu, Arch. Jpn. Chir.. 1984, 53, 33. C A l O l (19):166528g. (157F) Shiefer, Sigbert; Beutler, Hans Otto, Methods Enzym. Anal. 1985, 8, 87. . . CA1041111:84464f. .. . , (158F) Schwarz, Heimuth, Milchwirtsch. Ber. Bundesanst. Wolfpassing ROfholz, 1985, 84, 217, CA104(9):67567z. (159F) Sebedio, J. L.; Farquharson, T. E.; Ackman, R. G., Lipids, 1985, 20, 555. CA103(17):140414h. (160F) Seneit, Serpil; Gurturk, Feyza; Erguven, A,; Bozkurt, M., Turk HU, Denesel Siyol. Derg., 1986, 43, 23. CA105(19):170735x. (161F) Sheeley. Douglas Marf Sheeley, Richard M.; Hurst, J., Spectroscopy (Spingfield, Oreg.), 1986, 1 , 38. CA704(13):108030q. (162F) Shibahara, A,; Yamamoto, K.; Nakayama, T.; Kajimoto, G., Yukagaku, 1985, 34, 618. CA704(1):4697w.
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FOOD (163F) Shukia, V. K. S.; Schioetz, Nielsen, W., Proc. Scand. Symp. Lipids, 12th, 7983, 1984, 12, 27. CA104(3):18705j. (164F) Slover, Hal T.; Thompson, Raymond H., Jr., Bbl. Ref. Mater. Symp. Meeting Date 7983, 1985, 239. CA702(13):111561c. (165F) Smidovnik, Andrej; Perdih, Anton; Vitez, Ljubka. Nova Proizvod., 1985, 36, 107. CA 104(23):205633w. (166F) Smiljanic, D., Hrana Ishrana, 1985, 25, 171. CA103(21):177051p. (167F) Smurygina, N. V.; Andrianov, Yu. P.f Eremina, V., Molochn. Prom 1986, 5,33. CA105(15):132271k. (168F) Snyder, J. M.; Frankei, E. N.; Warner, K., JAOCS, J. Am. Oil Chem. SOC., 1988, 63, 1055. CA 105(19):170867s. (169F) Soliman, Mervat A.; Younes, N. A,, JAOCS, J. Am. OilChem. SOC., 1986, 63, 248. CA 704(15):128536n. (170F) Sotirhos, N.f Ho, Chi Tang; Chang, Stephen S., fette. Seifen, Anstrichm., 1988, 88, 6. CA704(15):128353a. (171F) Sotirhos, N.; Ho, Chi Tang: Chang, Stephen S., fette, Seifen. Anstrichm., 1986, 88, 45. CA104(17):147292w. (172F) Sotirhos, N.; Ho, C. T.; Chang, S. S., Dev. foodsci., 1986, 12(Sheif Life Foods Beverages), 601. CA 105(3):23168m. Svensen, A.; Abrahamsen, R. K., J . Dairy (173F) Spangelo, A.; Karijord, 0.; Sci., 1988, 69, 1787. CA105(13):113774k. (174F) Stack, Jeanette B.; Joe, Frank L., Jr.; Cunningham, D.; Fazio, T.; Roach, A. G., J. Assoc. Off. Anal. Chem.. 1986. 69, 551. CA105(3):23189u. (175F) Stolyhwo, Andrzej; Colin, Henri; Guiochon. George, Anal. Chem ., 1985. 57, 1342. CA 102(23):202675j. (176F) Strocchi, A.; Mariani, C.; Camurati, F.f Fedeli, E.; Baragli, S.; Giro, L.; Motta, L., Riv. Ital. Sostanze Grasse, 1984, 61, 499. CA102(17): 147625r. (177F) Strocchi, A., Riv. Ital. Sostanze Grasse, 1988, 63, 99. CA105(19):1706652. (178F) Sugino, K.; Terao, J.; Murakami, H.; Matsushita, S., J. Agric. food Chem. 1986, 34, 36. CA104(11):87195e. (179F) Sumimoto, Tatsuo; Yoshida, Ayako; Tanaka, Ryoichi, Osaka Koshu Eisei Kenkyusho Kenkyu Hokoku, Shokuhin, 1985. 16, 35. CA 105113H 13718~. (18OFf Szumilak, Krystyna; Gudaszewski. Tadeusz, Tluszcze Jadalne , 1985. 23. 1. CA10413k187160. (181F) Takagi, Tofu; Itabaihi. Yutaka, Yukagaku, 1984, 33, 600. C101(21):189827t. (182F) Toeregaard, B.; FribergJohansson, I., Proc. Scand. Symp. Lipids, 12th, 1983, 1984, 37. CA 104(5):33118p. (183F) Totani, Yoichior, Yukagaku, 1988, 35, 337. CA 105(9):77607x. (184F) Traitier, H.; Nikiforov, A., Anal. Chem. Symp. Ser., 1984, 21, 299. CA 101(25):228596p. (185F) Tsuda. T.; Nakanishi, H.; Kobayashi, S.; Morita, T., J. Assoc. Off. Anal. Chem., 1984, 67, 1149. CA102(13):111587r. (186F) Usuki, Riichiro, Nippon Shokuhin Kogyo Gakkaishi, 1985, 32, 74. CA 102(19): 165304q. (187F) Vaientova, Helena; Davidek, Jiri; Pokorny, Jan, Sb. Uvfiz, Potravin, Vedy, 1986, 4 , 1. CA105(17):151647c. (188F) Vicente, Thelma, S.; Waysek, Edward H.; Cort, W.. JAOCS, J. Am. Oil Chem. SOC.. 1985, 62, 745. CA102(21):183854y. (189F) Vioque, E.; Maza, M. P.; Miiian;F., J. Chromatogr., 1985, 331, 187. CA 103(19):159189k. (19OF) Wada. S.; Isoda, Y.; Arima, T.; Sangai, T.; Maekawa, Y.; Tamura, T. Sanga, Yukagaku, 1986, 35,647. CA 105(21):189555k. (191F) Wang, Changium; Zhang, Yi, fenxi Ceshi Tongbao, 1985, 4, 25. CA 104(13): 108008~. (192F) Wang, Wen Tang; Hou, Ke Quin; Mayinur, Y., U/jarstvo, l985., 22, 303. CA 105(7):59513]. CA103(193F) Ward, D. D., Milchwissenschaff, 1985, 40, 583. (25):213413u. (194F) Wei, Runyun; Song, Fengying; Gao, Hejuan, Shipin Yu faiao Congye. 1985, 5, 32. CA 104(7):49904c. (195F) Woestenburg, W. J.; Zaaiberg, J., fette, Seifen, Anstrichm., 1986, 88, 53. CA104(17):147293x. (196F) Woo, A. H.; Kollodge, S.; Lindsay, R. C., J. Dairy Sci., 1984. 67, 1517. CA 101(15): 128961k. (197F) Wood, Randall, Biochem. Arch ., 1988,2, 63. CA 105(9):77633c. (198F) Yabe, Yoshie; Tan, Shigeru; Ninomiya, T.; Okada, T., Nippon Shokuhin Kogyo Gakkaishi, 1984, 25, 264. CA 702(3):22948s. (199F) Yagi. K.; Kiuchi, K.; Saito, Y.; Miike, A,; Kayahara, N.; Tatano, T.; Ohoshi, N., Biochem. Int., 1988, 12, 367. CA 104(21):184960h. (200F) Yamamoto, Y.; Niki. E.; Tanimura, R.; Kamiya, Y., JAOCS, J. Am. Oil Chem. SOC., 1985, 62, 1248. CA103(25):214617a. (201F) Yamazaki, Megumi; Nagao, Akihiko; Tamori. Jyunji, Shokuhin Sogo Kenkyusho Kenkyu Hokoku, 1986, 48, 79. CAlO5(17):151647d. (202F) Yomota, Chikako; Toyoda, Masatake; Ito, Yoshio, Shokuhin Eiseigaku Zasshi, 1986, 27. 37. CA 104(25):223714c. (203F) Yoshida. Hiromi; Murata, Kazuhiko; Kajimoto, Goro. Ntur. Rep. Int ., 1985, 32. 707. CA 103(21):177069a. (204F) Yunusova. S. G.; Gusakova, S.D.; Giushenkova, A. I.; Shcherbakov, V.. I z v . Vyssh. Uchebn. Zaved.. 1965, 17, 2. CA103(11):86556r. (205F) Zhou. Yingtian; Zhao, Zhijie. Yingyang Xuebao. 1985. 7, 47. CA 103(7):50657k. (206F) Zimniak. Andrzej. Tluszcze Jadlne, 1984, 22, 30. CA102(21):183774~. FLAVOR
(1G) Abraham, V.; Deman, J. M.. J . Am. OilChem. SOC.. 1985, 62, 1025. CA 103(17):140394b. (2G) Adam, S., Anal. Chem. Symp. Ser., 1984, 67-77. CA102(1):4518x. (3G) Aishima, I., Dev. Food Sci.. 1986, 12 (Sheif Life Foods Beverages), 755. CA 105(7):59586k.
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ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
(4G) Badings, H. T.; De Jong, C.; Dooper, R. P. M.; DeNijs, R. C. M., Dev. Food Sci., 1985, 45, 523. CA703(15):12181lu. (5G) Badings. H. T.; De Jong, C., Anal. Vdetiles: Methods Appl., Proc. Int. Workship, 1984. CA 707(21):189789g. (6G) Badings, H. T.; De Jong, C.; Dooper, R. P. M., J. Hlgh Resolut. Chromatogr. Chromato@. Common., 1985, 8. CA704(16):141496u. (7G) Beutler, Hans Otto, Methods Enzyme. Anal. Ed., 1984, 6, 606. Edited by Bergmeyer, H. U. CA 702(9):75027x. (8G) butler, Hans Otto, Methods Enzym. Anal. Ed., 1984, 6 , 598. Edited by Bergmeyer, H. U. CA 102(9):73631r. (9G) Borek, Vladimir; Hubacek, Jaromir; Rehakova, Vera, Chem. Lisfy, 1985, 79, 984. CA 104(1):4703v. (100) Busch, Kenneth L.; Kroha, Kyle J., ACS Symp. Ser., 1985, 289 (Charact. Meas. Flavor Compd.), 121. CA 104(13):10796Of. (11G) Carpenter, R. S.; Burgard, D. R.; Patton, D. R.; Zwerdling, S., Instrum. Anal. Foods, 1983, 2, 173-86. CA 707(21):189986u. (12G) Chamblee, T. S.;Clark, B. C., Jr.; Raadford, T.; Iacobucci, G., J. Chromatogr., 1985, 330, 141. CA 103(16):128789b. (13G) Chang. Yueh Ing; Reineccius, Gary A,, J. Agric. food Chem., 1985, 33, 1168. CA 104(7):49894z. (14G) Chen, Chu Chin; Ho, Chi Tang, J. Chromafogr., 1986, 356, 455. CA 104(23):205643z. (15G) Chiang, Grace H., J. foodsci. 1986, 57,499. CA104(23):205616v. (16G) Collinge, A.; Hermesse, 8 . ; Noirfaiise, A,, Be@. J. food Chern. Biotechno/., 1985, 40, 143. CA105(1):5268q. (17G) De Pooter, H. L.; Coolsaet, B. A.; Dirinck, P. J., Essent. Oils Aromat. Plants, 1985, 67-77. CA 703(23):195045u. (18G) Dirinck. P.; De Pooter. H.; Wiiiaert, G.; Schamp, N., Anal. Volatlles: Methods Appl., 1984, 381-400. CA 101(23):209151y. (19G) Dirks, Uwe; Herrmann, Karl, Z.Lebensm. forsch., 1984, 779, 12. CA 102(1):4516v. (20G) Dunn, H. C.; Lindsay, R. C., J. Dairy Sci., 1985, 68, 2853. CA 104(5):33132p. (21G) Dupuy, H, P. Flock, G. J., Jr.; Bailey, M. E.; St. Angelo. A.; Legendre, M.; Sumreii, G., J. Am. Oil Chem. SOC., 1985, 62, 1690. CA104(7):499 13e. (22G) Eberhardt, Reinhlld; Pfannhauser, Werner, 2. Lebensm. forsch ., 1985, 181, 97. CA 103(23):195097n. (23G) El-Obeid, H. A.; Madani, A. E.; Mossa, J. S.; Rashed, M.; Ibrahim, A,. Pharmazie, 1984, 39, 778. CA102(14):119404z. (24G) Geroge, Gerard, Lab0 Probl. Tech., 1984, 343, 479. CA101(19):169217r. (25G) Gonzalez. L.; Gra. R., Rev. Cienc. Quim. 1984, 15, 275. CA104(9):67599m. (26G) Guarino, Phippip A.; Brown. Susan M., J. Assoc. Off. Anal. Chem. 1985, 68(6), 1198-201. CA f94(7):49925k. (27G) Hardin, Joyce M.; Stutte, Charles A,, f o o d Sci. Technol., 1984, 71 (Food Const. Food Residue) 295. CA 101(17):149861t. (28G) Hayashi, Tateki; Reece, Clayton A,; Shibamoto, Ta, ACS Symp. Ser., 1985, 289 (Charact. Eas. Flavor Compd.), 61. CA 704(17):147253j. (29G) Horita, Hiroshi; Hara, Toshio, Chagyo Gyutsu Kenkyu, 1984, 41. CA 103(15): 121842e. (30G) Hutt, Terrence F.; Herrington, Mark E.,J . Sci. Food Agric., 1985, 36, 1107. CA 104(9):67617r. (31G) Idstein, Heinz; Schreier, Peter, ACS Symp. Ser., 1985, 289 (Charact. Meas. Flavor Compd.), 109 CA104(13):107959n. (32G) Izquierdo, L.; Aristoy, M.; Navarro, J. L., Int. fruchtsaff Wiss. Komm., 1984, Flavor. CA703(17):140582m. (33G) Janssen, A.; Gole, T., Chromatographica, 1984, 18, 546. CA 102(1):4541z. (34G) Jansz, E. R.; Pathirana, I.C.; Packiyasothy, E., J. Natl. Sci. Counc. S r i h n k a , 1983, 11, 129. CA103(17):140401b. (35G) Kato, T.; Sekikawa, Y., Kanzei Chuo Bunsekishoho, 1985, 25, 1. CA 703(11):86679h. (36G) Kawada, T.; Watanabe, T.; Katsura, K.; Takami. H.;Iwai, K., J. Chromatogr., 1985, 329, 99. CA 103(9):69886f. (37G) Kernik, K.; Reineccius, G. A.; Scire, J. P., Dev. Food Sci., 1985, 10 (Prog. Flavour Res.), 477. CA103(13):103515w. (38G) Kolb, E., Essent. Oils Aromat. Plants, 1985, 3-21. CA103(23):195044t. (39G) Krajewska, Anna M.; Powers, John J., J. Chromafogr., 1986, 367, 267. CA 105(21):189585v. (40G) Kubeczka, Karl Heinz; Formacek, Viktor, Anal. Volatiles: Methods Appl., 1984, 219-30. CA701:(20)177241j. (41G) Lang. Johanna; Celotto, Claude; Esterbauer, H., Anal. Biochem ., 1985, 150, 369. CA 703(23):192547y. (42G) Leahy, M. M.; Reineccius, G. A., Anal. Volatiles: Methods Appl., 1984, 19-47. CA 701(21):189786d. (43G) Liddie, P. A. P.; Bossard, A., Dev. foodsci., 1985, 10(Prog. Flavour Res.), 467. CA 103(13):103485m. (44G) Liddle, P. A. P.; Bossard, A., HRC CC, J. High Resolut. Chromafogr. Chromatogr. Commun ., 1984, 7. CA 102(5):44486s. (45G) Lin, J. C. C.; Jeon, I. J., J. food Sci., 1985, 50, 843, 846. CA 102(23):2027172. (46G) MacLeod, Glesni; Ames, Jennifer M.,J. Chromafogr.. 1988. 355, 393. CA 704(26):236590j, (47G) Mayfieid, H. T.; Mar, T.; Bertsch, W.; Staroscik, J. A,, R o c . Int. Symp. Caplllaty Chromatogr., 1985, 6th, 555-67. CA 103(23):195037t. (480) Mills, 0. E., N . 2. J. Dairy Sci. Technol., 1988, 21, 49. CA105(9):77647k. (49G) Moeilering, Hans; Bergmeyer, Hans Uirich. Methods Enzyme. Anal., 1984, 6, 220. Edited by Bergmeyer, H. U. CA 102(9):74993x. Pinter-Szakacs, M.; Wittmann, R.; Reutter, M.; Eichner, (50G) Moinar-Perl, I.; K. J. Chromafogr., 1986, 361, 311. CA105(9):77659r.
FOOD (51G) Mati, Yutaka; Kluchi, Ken, Nippon Jozo KyokaiZasshi, 1985, 80, 274. CA 703(7):5279&d. (52G) Mounie, J.; Santona, L.; Truchot, R.; Escousse, A., Ann. Falsif. Expert. Chlm. Toxicol. 1985, 78, 271. CA104(11):87217p. (53G) Nitz, S.,Top. Flavour Res., R o c . Int. Conf., 1985, 43. CA704(9):67594f. (540) Nunez, A. J.; Maarse, H., Chromatographia, 1988, 21, 44. CA 705(9):7766 1k. (55G) RavM, U.; Putievsky, E.; Weinstein, V.; Ikan, R., Essent. Oils Aromaf. Plants, 1985, 135-8. CA103(23):195046v. (56G) Reineccius, G. A.; Liardon, R., Top. Flavour Res., R o c . Int. Conf., 1985, 125. CA 704(9):67595g. (57G) Reineccius, Gary A.; Anandaraman, S., Food Sci. Technol., 1984, 11 (Food Const. Food Residue), 195. CA 101(17):149860s. (58G) Rousoff, Russoil F., Semiochem.: Flavors fhormones, 1985, 275-84. CA 7O2(25):2 19681f. (59G) Schreier, Peter; Idstein, Heinz; Herres, Werner, Semiochem.: Flavors fhermones, 1985, 251-64. CA 102(23):202838q. (60G) Shahidi, Fereidoon; Rubin, Leon J.; D'Souza, L., CRC Crit. Rev. Food Sci. Nutr., 1988, 24, 141. CA105(17)151600h. (61G) Shaw, Philip E.; Moshonas, Manuel G., Mass Specfrom. Rev., 1985, 4, 397. CA 704(5):33094c. (62G) Shibamoto, Takayuki, Anal. Volatiles: Methods Appl., 1984, 233-500. CA 701(20):177242k. (63G) Smith, Roger M., Electrochem. Defect., Kwahakhoechi, 1984, 17. CA 702(17):147636v. (64G) Spiro, Michael; Price, William E., Analyst (London), 1988, 11 7 , 331 CA 705(5):41331p. (65G) Suzuki, Jun; Bailey, Milton E., J. Agric. Food Chem., 1985, 33, 343. CA 702(23):202676k. (66G) Tateo, F.; Chizzini, F.; Cunlai, P., Mtf. Geb. Lebensmitfelunte Hug., 1985, 76(4), 563-9. CA 704(15):128345Z. (67G) Toulemonde, B.; Beauverd, D., Dev. Food Sci., 1985, 10 (Prog. Fiavour Res.), 533. CA 703(13):103659w. (68G) Trugo, Luiz C.; Macrae, Robert, Food Chem., 1988, 79, 1. CA 104( 13): 108020m. (69G) Van der Greef, J.; Nijssen, L. M.; Maarse, H.; TenNoever de Brauw, M.; Games, D.; Alcock, N., Dev. Food Sci., 1985, 603. CA103(15): 1218 12v. (70G) Vernin, G.; Metzger, J.; Fraisse, D.; Scharff, C., Planta M e d . , 1988, 96. CA 105(6):48808h. (71G) Voiiley, A.; Bosset, J. O., Lebensm. Technol.. 1988, 79, 47. CA105(13):113733w. (72G) Wadhwa, B. K.; Jain, M. K.. Indian J. Dairy Sci., 1984, 37, 254. CA 703( 1):5093n. (73G) Weinstein, V.; Ikan, R.: Ravid, U.; Putievsky, E., Essent. Oils Aromat. Plants, 1984, 139-43. CA 704(25):224793q. (74G) Whiffield, F. 6.; Shaw, K. J., Dev. Food Sci., 10 1985, 70 (Prog. Flavour Res.), 221. CA 703(11):86549r. (75G) Wyiie, P. L., Chromatographia, 1988, 21, 251. CA 105(12):107670g. IDENTITY
(IH) Acton, J. C.; Clay, D. L.; Robinson, K. E.; Dick, R. L.; Acton, W. C., J. FoodSci., 1988, 51, 524. CA704(19):167013). (2H) Akimoto. Koichi, Lectins: Biol., Biochem., Clin. Biochem., 1988, 5, 95. CA 101(171:150190e. (3H) Andersen,~Mette M.; Ebbesen, Kirsten, Lectins: Biol., Blochem., Clin. Biochem., 1988, 5, 95-108. CA705(13):113721r. (4H) Barroga, Charlene F.; Laurena, Antonio C.; Mendoza, E. T., J. Agric. Food Chem., 1985. 33, 1006. CA703(19):159332b. (5H) Bianchini, Jean Pierre; Gaydou, E. M.; Sigoillot, J. C., J. Chromafogr., 1985, 329, 231. CA103(13):101430r. (6H) Blru, Geresu; Seeger, Horst; Gemmer, Helmut; Voik, Klaus, Fieischwirtschaft, 1985, 65, 862. CA103(11):86616k. (7H) Boegl, W.; Heide, L., Radiat. fhys. Chem., 1985, 173. CA103125k213517f -- . . .. (8H) Boegl, W.; Hekle, L., Anal. Appl. Biolumin. Chemilumin., 1984, 173. CA 702(21):183812h. (9H) Carman, A. S., Jr.; Kuan, S. S.;Francis, 0.J., Jr.; Ware, G. M., Anal. Lett., 1985, 78(B9), 1167. CA103(19):159199p. (10H) Casas, C.; Tormo, J.; Hernandez, P. E.; Sanz, B., Meat Sci., 1985, 72. 31. CA102115k130539t. (11H) 'Casas, C.; Tormo, J.; Hernandez, P. E.; Sanz, B., J. Food Technol., 1984, 79, 283. CA701(17):149935v. (12H) Chaveron, H.; Verdoia, C.; Meili, M., Ann. Falsif. Expert. Chlm. Toxicol., 1984, 77, 571. CA103(13):103547h. (13H) Chen, Ching Jiang; Lin, Yu Ming, Ho Tzu K ' o Hsueh, 1985, 21, 251. CA 703(13):100898n.(14H) Cows, U.; Montag, A., Fetfe, Seifen, Anshichm., 1985, 87, 177. CA 103(3):21337a. (15H) Croon. Lars Boerje; Kiutamo, Tuomo; Leth, Torben; Rogstad, A,, R o c . Scand. Symp. Lipids, 1984, 53. CA103(25):213536m. (16H) De Freitas, Claudia Jose; Graner, C. A. F.. Zuanon, N., Rev. Cienc. Farm. (Araraquara, Braz.). 1984, 8 , 23. CA104(1):4717c. (17H) Demmer. W.: Werkmeister. K., Arch. Lebensmittelhvo., .- 1985. 36. 15. CA m ( 2 I): 183913s. (18H) Derbesy, Michel, Labo-Pharma-frob/. Tech ., 1984, 343, 467. CA 7Oi~19k169160s. (19H) Dyszel. SusG-M., Therrnochim. Acta, 1985, 87, 89. CA103(11):86588c. (20H) Farag, R. S.;Hewedi, M. M.; Abo-Raya, S. H.; Khalifa, H. H., Grasas Aceifes (Seville), 1984, 35, 181. CA107(23):209193p. (21H) Fedenko, V. S.; Vinnichenko, A. N.; Mirosh, 0. G., Fiziol. Blokhim. Kul'f. Rast., 1985, 77, 501. CA703(25):213504z. (22H) Fritsch. Rudolf, Ernaehrung (Vienna), 1984, 8, 532. CA104(5):33 123m. 1--,.-
(23H) Garrone, W.; Antonucci, M.; Bona, U., Milchwissenschaff, 1984, 39, 464. CA 107(17):149964d. (24H) Gegiou, D.; Staphyiakis, K., J. Am. OilChem. SOC., 1985, 62, 1047. CA 103(13): 103518~. (25H) Geilinger, Irene: Amado, Renato; Neukom, Hans; Kleinert, J., Lebensm. Technol., 1984, 77, 195. CA 101(23):209454z. (26H) Gomez Gomez, R.; Vazquez Rocero, A,, Grasas Aceites (Seville), 1985, 36, 250. CA704(3):18721m. (27H) Gottesmann, Peter; Hamm, Reiner, Fleischwirtschaft, 1985, 65, 591. CA 103(7):52850s. (28H) Graciani Constante, E.; Gomez Gomez, R.; Vazquez. Grasas, Aceites (Seviiie), 1985, 36, 254. CA 104(3):18722n. (29H) Greenberg, Rae; Dower, Harold J., J. Agric. Food Chem., 1988. 34, 30. CA104(11):87194d. (30H) Griffiis, Neil M.; Billington, M. J.: Crimes, A. A,; Hitchcock, C., J. Sci. Food Agric., 1984, 35, 1255. CA 102(5):44466k. Gaponenko, V. G., Maslo from 1985, (31H) Gubman, I.I.; Askinazi, A. I.; 21. CA 704(3):18707m. (32H) Hamann, Y.; Tisse, C.; Estienne, J., Ann. Falsif. Expert. Chim. Toxicol., 1984, 77, 271. CA702(9):77343w. (33H) Hariand, Barbara F.; Oberieas, Donald, J. Assoc. Off. Anal. Chem ., 1988, 69, 667. CA105(13)113751a. (34H) Heide, Lydia; Boegl, Werner, Z.Lebensm, Forsch ., 1985, 787, 283. CA 703(25):213526h. (35H) Hili, Susan H. A.; Gasson, Michael J., J. Dairy Res., 1986, 53, 625. CA 105(21):189676a. (36H) Hoilingworth, T. A., Jr.; Throm. H: R.; Wekell, M.; Trager, W.; O'Donnell, M. J., J. Assoc. Off. Chem., 1988, 69, 524. CA105(5):41346x. (37H) Huebner, F. R.; Bietz, J. A., J. Chromatogr., 1985, 327, 333. CA 103(5):36399w. (38H) Hurst, W. J.; Snyder, K. P.; Martin, R. A,, Jr., J. Chromafogr., 1985, 378, 408. CA 102(11):94419t. (39H) Hyde, W.; Stahr, H. M., f r o c . Annu. Meet. Am. Assoc. Vef. Lab. Diagn., 1983. CA 103(15):121817a. Tur'yan, Ya. I.; Arutyunyan, A. N., Gavrilenko, S.A.. Izv. (40H) II'ina, L. I.; Vyssh. Uchebn. Zaved., 1986, 82. CA104(19):167023n. (41H) Jamais, Gilberte; Clemencet, M. C.; Baron, C., Ann. Falsif. Expert. Chim. Toxicol., 1985, 78, 467. CA 705(3):23173j. (42H) Janssen, Frederik W.; Voortman, G.; De Baaij, J., Z. Lebensm. Forsch., 1988, 782, 479. CA 705(11):96138m. (43H) Jones, Shelia J.; Patterson, Ronald L. S., J. Sci. Food Agric., 1988. 37, 767. CA105(15):132272m. (44H) Kamarei, A. R.; Karel, M., J. Food Sci., 1984, 49, 1517, 1524. CA 702(1):4543b. (45H) Kaminski, E.; Przybylski, R.; Wasowicz, E., J. Cereal Sci., 1985, 3, 165. CA 703(9):69862v. (46H) Ke, P. J.; Cervantes, E.; Robles-Martinez, C., J. Sci. Food Agric., 1984, 35, 1248. CA 702(3):22940h. (47H) Kiei, Jonathan L., Lipids, 1985, 20, 475. CA105(9):75424m. (48H) Kikugawa, Kiyomi; Nakahara, Takami; Tanuguchi, Yasumichi; Tanaka, M., Mas, Lipids, 1985, 20(7). 475-81. CA103(13):103529d. (49H) Kneifel, W.; Uiberth, F., Milchwissenschaff, 1985, 40, 265. CA703(5):36336y. Belitz, H. D., Lebensmitfeichem. Gerichti. Chem., 1985, (50H) Krause, I.; 39, 33. CA102(25):219693m. (51H) Krueger, Dana A.; Krueger, Harold W., J. Agric. FoodChem., 1985, 33, 323. CA 102(23):202885n. (52H) LeBlanc, R. J.; Gill, T. A., Can. Inst. FoodSci. Technol. J., 1984, 77, 195. CA 702(3):22984u. (53H) Lee, Hyoung S.; Rouseff, Russell L.; Nagy, Steven, J. Food Sci., 1988, 51, 1075. CA705(13):113773j. (54H) Lemieux, L.; Amiot, J.; Brisson, G. J., Can. Inst. FoodSci. Technol. J., 1985, 18, 29. CA102(19):165349h. (55H) Lever, Michael; May, Philip C.; Andre, Claude M., Anal. Biochem., 1985. 144. 6. CA702(151:128160u. , (56H) Lin, H.'H.; Cousin, M. A., J. Food f r o t . , 1985, 48, 671. CA104(131: 10801l i . ( 5 7 b ' Lindberi Waiter; Oehman, J.; Wold, S.; Martens, H., Anal. Chim. Acta, 1985, 777, 1. CA103(11):86590~. (58H) Loeliger, Juerg; Saucy, Francoise, J. Lumin., 1984, 31, 908. CA102f17): 147645~. (59") ' Manz, Jakob, Fleischwirtschaft, 1985, 65, 497. CA 703(1):5107v. (60H) Marcy, Joseph E.; Rouseff, Russell L., J. Agric. Food Chem., 1984, 32, 979. CA107(15):128955m. (61H) Mazzola, E. P.; Phiiiippy, B. Q.; Harland, B.; Miller, T.; Potemra, J., Katsimpiris, E. W., J. Agric. Food. Chem., 1988. 34, 60. CA704(11):87 191a. (62H) Minkowski, Karol; Schubert, Irena, Tluszcze Jadahe, 1984, 22, 16. CA 103(11):86609k. (63H) Morgan, M. R. A.; McNerney, R.; Coxon, D. T.; Chan, H. W., Immunoassays Food Anal., 1985, 16. CA103(19):159184e. (64H) Morishita, H.; Iwahashi, H.; Osaka, N.; Kido, Ryo, J. Chromatogr., 1984, 315, 253. CA702(11):94403h. (65H) Muuse. B. G.; Van der Kamp, H. J., Nefh. Milk Dairy J., 1985, 39, 1. CA 10311 - , ik86579a. --- -(66H) Nakhost, 2.; Karel, M., J. Food Sci., 1984, 49, 1171. CA 707(191: 169203h. (67H) Nazer, Jamil M. A.; Young, C. T.; Giesbrecht, F. G., J. Food Sci., 1985, 50. 1095. CA 703(9):69890c. (68H) Northeved, Allen, Rapid Methods Autom, Microbiol. Immunol., 1985, 1. CA703(3):2148Os. (69H) Notermans, S., Rapid Methods Autom. Microbiol. Immunol, 1985, 649-55. CA 103(23):195049y. (70H) Ohhashl, Minoru, Kagaku Gijufsushi Mol. 1985, 23, 63. CAiO3(13):103487p.
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FOOD (71H) Palagyi, S., Isotopenpraxis, 1985, 27, 130. CA702(24):214317g. (72H) Patel, P. D., Immunoassays Food Anal., 1985, 23. CA703(19): 159140n. (73H) Patel, A. M.; Dave, J. M.; Sannabhadti, S. S., Indian J. Dairy Sci., 1984, 37, 396. CA 703(5):36255w. (74H) Ravestein. P.; Driedonks, R. A., J . Food Technol., 1986, 27, 19. CA 704(15):128374h. (75H) Rogstad, Astri, Proc. Scand. Symp. Lipids, iZth, 7983, 1984, 47. CA 703(25):213535k. (76H) Salfi, Vincenzo; Fucetola, F.; Pannunzio. G., J. Sci. Food Agric., 1985, 36, 811. CAi04(3):18737w. (77H) Schafer, M. L.; Peeler, J. T.; Bradshaw, J. G.; Hamilton, C.; Carver, R., J. Assoc. Off. Anal. Chem., 1985, 68, 626. CA703(11):86597e. (78H) Takahashi, M.; Wakabayashi, K.; Nagao, M.; Yamamoto, M.; Masui, T.; Goto. T.; Kinae, N., Carcinogeneisis, 1985, 6 , 1195. CA703(13):103558n. (79H) Tan, E. K.; Siew, W. L.; Oh, Flingoh, C. H.; Berger, K.. Palm Oil Prod. Techrtol. Eighties, 1983, 165-81. CA 707(25):228739n. (80H) Tanner, H.; Limacher, H., Fluess. Obst. 1984, 768. 182. CA707(17):149921n. (81H) To, Kar Chun; Rack, Edward, P., Anal. Chem.. 1985, 57, 1490. CA 702(23):200343a. (82H) Tsunoda, K.; Inoue, N.; Aoyama. M.; Ito, H.; Tachiban, M.; Hasebe, A., Shokuhln Eiselgaku Zasshi, 1985, 26, 229. CA 704(3):18728u. (83H) Wieneke, Antonnette A., Gilbert, R. J., J. Hyg., 1985, 95, 131. CA 703( 17): 140415j. (84H) Wrigley, C.; Campbell, W.; DuCros, D.; Margolis. J.. J. Electrophor., 1984, 95. CA 707(17):149815f. (85H) Yehchen, Shih Ling; Hsu, Chin Tan, J . Assoc. O f f . Anal. Chem.. 1985, 68, 618. CAiO3(11):86595c. (86H) Yiu, S. H.; Collins, F. W.; Fulcher, R. G.; Altosaar, I., Can. J. Plant Sci.. 1984, 64, 869. CA 702(11):92347u. MINERALS
(IJ) AI Hitti, I.K.; Thomas, J. D. R.. Anal. Lett.. 1985, 78(A8), 975. CA 703( 15): 121843f. (2J) Alvarez de Eulate, M. J.; Montoro, R.; Ybanez, N.; De La Guardia, M., J. Assoc. Off. Anal. Chem.. 1988, 69, 871. CA 705(2t):189579w. (3J) Alvarez, Robert, Fresenius' 2.Anal. Chem., 1986, 324, 376. CA705( 14):126031r. (4J) Andersen, Jan Rud, Analyst (London), 1985, 770, 315. CA703(3):2 129 1f. (5J) Anderson. C.: Warner, C. R.; Daniels, D. H.; Padgett, K., J. Assoc. Off. Anal. Chem., 1986, 69, 14. CAi04(11):87230n. (6J) Aziz-Alrahman, A. M., I n t . J. fnviron. Anal. Chem., 1984, 79, 55. CA 702(113394422~. (7J) Aznarez, Jose; Mir. Jose M., Analyst(London), 1985, 770, 61. CA702(26):230953s. (8J) Aznarez, J.; Rabadan, J. M.; Ferrer, A.; Cipres P., Talanta , 1986, 33, 450. CA 705(6):53715e. (9J) Baluja-Santos, C.; Gonzalez-Portal, A,; Bermejo-Martinez, F., Analyst (London), 1984, 709, 797. CA 70 7 (25):228454r. (IOJ) Balulescu, Lano. FooU Technol. (Chicago), 1985, 39, 38. CA 703(2 1): 177023f. (1 1J) Barbera, Reyes; Farre, Rosaura; Montoro, Rosa, J. Assoc. O f f . Anal. Chem., 1985, 68, 511. CA703(1):5102q. (12J) Beljaars, Paul R.; Horwitz, William, J . Assoc. Off. Anal. Chem., 1985, 68, 480. CA 703(3):21317u. (13J) Benzo, Z.;Schorin, H.; Velosa, M., J. Food Sci., 1986, 57, 222. CA 704(13):108028v. ( 1 4 ) Bettoli, M. G.; Orlandi, G.; Tubertini, O., Inorg. Chim. Acta, 1985, 98, 29. CA iOZ(21):18156 1b. (15J) Boyer, Kenneth W.; Horwitz. William; Albert, R., Anal. Chem., 1985, 57,454. CA 702(6):55204z. (16J) Coles, L. E.; Guthenberg, H.; Kato, T.; Kojima. K., Pure Appi. Chem ., 1985, 57, 1507. CA703(19):159197m. (17J) Cook, Joanne M.; KareHtz, Richard L.; Dalsis, D., J. Chromatogr. Sci., 1985. 23, 57. CA702(13):111607x. (18J) Dabeka, Robert W.; McKenzie. Arthur, D., Can. J. Spectrosc., 1988, 37, 44. CA705(9):77671p. (19J) Dabeka, Robert W.; Lacroix, Gladys M. A,, Can. J. Spectrosc.. 1985, 30, 154. CA 705(5):41357b. (20J) Demura, Reiko; Tsukada, Shiro: Yamamoto, Ikuo, Eisei Kagaku, 1985, 37, 405. CA 705(1):5260f. (21J) Evans, William H.; Caughlin, Dorothy, Analyst (London), 1985, 770, 681. CA 703( 19): 159176d. (22J) Evans, William H.; Read, John I., Analyst (London), 1985, ifO(6). 619-23. CA 703(19):159175C. (23J) Farre, Rosaura; Lagarda, M. Jesus: Montoro, Rosa, J. Assoc. O f f . Anal. Chem.,' 1986, 69, 876. CA 705(21):189580q. (24J) Fernandez, P.; Perez-Conde. C.; Gutierrez, A. M.; Camara. C., J. Mol. Struct., 1986, 743, 549. CA 705(1):5238e. (25J) Fischer, Peter W. F.; L'Abbe, Mary R.; Giroux, A., J. Assoc. Off. Anal. Chem.. 1986. 69, 687. CA705(11):96136j. (2W) Fulton, B. A.; Meloan. C. E.: Wichman, M.: Fry, R., Anal. Chem., 1984, 56, 2919. CA707(23):209155c. (27J) Gharaibeh, A. A. R.; Eagles, J.; Self, R., Biomed. Mass Spectrom., 1985, 72(7), 344-7. CA 703(13):103560g. (28J) Gharlb. A.; Rahimi, H.; Pyrovan, H.; Raoffi, N. J.; Taherpoor, H., J. Radloanal. Nucl. Chem., 1985, 89. 31. CA702(13):111608y. (29J) Gillain, G.; Rutagengwa. J.. Analusis, 1985, 13, 471. CA704(7):49937r. (30J) Goewie, Cherie E.; Van den Broek, Huub H., Meded. Fac. Landbouww et Rijksuniv. Gent, 1985, 50(3B), 1315-18. CA 704(9):67610h. (31J) Grobecker, K. H.; Kluessendorf, E., Fresenius' Z . Anal. Chem. 1985, 322, 673. CA704(11):87252w.
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(32J) Grobenski, 2 . ; Erler, W.; Voellkopf, U., At. Spectrosc., 1985, 6, 91. CA 703(18):152913h. (33J) Guinon, Jose L.; Garcia-Anton, Jose, Anal. Chim. Acta, 1985, 777, 225. CA 704(16):141302c. (34J) Gutierrez, A. M.;Perez-Conde, C.; Rebollar, M. P.; Polo Diez, L. M., Talanfa, 1985, 32. 927. CA704(1):4702u. (35J) Harniey, James M., J . Anal. At. Spectrom., 1986, 7 , 287. CA705(16):145276R. (36J) Herrador, M. A.; Jimenez, A. M.; Navas, M. J.; Troncoso, A. M., Z . Gesamte Hyg. Ihre Grenzgeb., 1986 32, 285. CA705(11):96092s. (37J) Hidaka, T.; Tanaka, Y.; Nakamura, K.; Takarai, T.; Kirigaya, T.; Kamijo, M.; Suzuki, Y.; Kawamura, T., Shokuhin fiseigaku Zasshi, 1985. 26, 465. CA 704(5):33166c. (38J) Hill, A. D.; Patterson, K. Y.; Veillon, C.; Morris, E. R., Anal. Chem., 1986, 58, 2340. CA 705(11):93926f. (39J) Hocquellet, P., At. Spectrosc., 1985, 6 , 69. CA 703(10):81045p. (40J) Huijbregts, A. W. M.; Hibbert, D.; Phillipson, R.; Schiweck, H.; Steinle, G., Zuckerindustrie (Serlin), 1985, 770. 797. CA704(1):4716b. (41J) Hunt, John; Seymour, Deborah J., Analyst(London), 1985, 770, 131. CA 702(23):202678n. (42J) Irsch, B.; Schaefer, K., Fresenius' Z . Anal. Chem., 1985, 320, 37. CA 702(13): 109251h. (43J) Ishii, Yuuko, Mukogawa Joshi Daigaku Kiyo, Shokumotsu-hen, 1984, 32, 1. CA 703(9):69881a. (44J) Johnson, Mark E.; Olson, N. F., J. Dairy Sci., 1985, 68, 1020. CA 702(25):219711r. (45J) Khammas, Z. A.; Marshall, J.; Littlejohn, D.; Ottaway, J.; Stephen, S. C.. Microchim. Acta. 1985, 7(5-6), 333. CAi04(9):67618s. (46J) Kindstedt, P. S.; Kosikowski, F. V., J. Dairy Sci., 1985, 68, 806. CA 702(25):21 9 7 0 9 ~ . (47J) Kluessendorf, B.; Rosopulo, A,; Kreuzer, W., Fresenius' 2. Anal. Chem., 1985, 322. 721. CA704(11):87253x. (48J) Knezevic, G.; Kurfuerst, U., Fresenius' Z. Anal. Chem., 1985, 322, 7 17. CA 704( 18):151 104d. (49J) Kohiyama, M.; Maruyama, T.; Niiya, I.; Matsumoto, T., Yukagaku, 1986, 35, 653. CA705(15):132275q. (50J) Koops, J.; De Graaf, C.; Westerbeek, D., Neth. Milk Dairy J., 1984, 38, 223. CA702(13):11598v. (51J) Krull, Ira S.; Panaro. Kenneth W.. Appl. Spectrosc., 1985, 39, 960. CA 704(5):33134r. (52J) Kruse, Reinhard, Fortschr. Atomspektrom. Spurenanal., 1984, 7 , 403. CA 703(1):5056c. (53J) Lawrence, J. F.; Chadha, R. K.; O'Brien, R.; Conacher, H. B., Microchem. J., 1985, 37, 237. CAi02(25):219705s. ( 5 4 ) List, D.; Ruwisch, I.; Langhans, P., Fluess. Obst, 1986, 53, 10. CA 704(21):184947j. (55J) Louie, H. W.; Go, D.; Fedczina, M.; Judd, K.; Dalins, J., J . Assoc. Off. Anal. Chem., 1985, 68, 891. CA703(17):140443s. (56J) Lyons, David John; Spann, K. P.; Roofayel, R. L., Analyst (London), 1985, 7 IO, 955. CA 704(1);4699y. (57J) Mannino, Saverio; Bianco, Mariagrazia, J. Micronutr. Anal., 1985, 7 , 47. CA 704(5):33147x. (58J) Mannino, Saverio, Rlv. SOC.Ital. Sci. Aiimont., 1986, 75(1-2), 11. CA 705(7):59495e. (59J) Matsumoto, Kiyoshi; Ishida, Kohichi, Osajima, Y.. Nippon Shokihin Kogyo Gakkaishi, 1986, 33, 61. CA 704(23):205644a. (60J) McCabe, S.; Ottaway. J. M., Anal. Proc. (London), 1986, 23, 16. CA 704(19):166979s. (61J) Meloni, S.; Nogara, G.; Queirazza, G., J . Trace Microprobe Tech., 1985, 3, 221. CA103(20):171141w. (62J) Miller-Ihli, Nancy, J.; Wolf, Wayne, R., Anal. Chem., 1986, 58, 3225. CA 705(21):189570m. (63J) Mingorance. M. D.; Lachica, M., Anal. Lett., 1985, 78(A12), 1519. CA 703(21):177071v. ( 6 4 ) Mori, T.: Nishioka, C.; Ishikawa, H.; Kuroda. H.. Shokuhin Eiseigaku Zasshi, 1985, 26, 260. CA704(1):4721z. (65J) Muenz. H.; Lorenzen, W., Fresenius' Z . Anal. Chem., 1984, 379, 395. CA 702(5):44490p. (66J) Murphy, L. C.; Almeida. M. C.; Dulude, G.; Sotera, J., Lebensm.-Biotechno/., 1985, 2, 54. CA 704(15):128343x. (67J) Nangniot. P.; Agneessens, R.; Zenon-Roland, L.; Beriemont-Frennet. M., Analusis, 1984, 72, 197. CA 702(7):60868y. (68J) Narasaki, Hisatake, Anal. Chem., 1985, 57, 2481, CA703(19):159178f. (69J) Narres, Hans Dieter; Mohl, Carola; Stoeppler, M., Z. Lebensm.-Unters. Forsch., 1985, 787, 111. CA703(17):140440p. (70J) Narres, Hans Dieter; Valenta, Pavel; Nuernberg, H., Z. Lebensm.-Unters. Forsch., 1984, 779, 440. CA 702(9):77379n. (71J) Nikdel, S.; Barros, S. M., R o c . Fla. State Hortic. SOC., 7984, 1885, 97, 79. CA703(17):140566r. (72J) Ochiai. S.;Ogawa, H.; Suzuki, J.; Nishijima, M.; Nishima.'T.. Kenkyu Nenpo Tokyo-ToritsuEisei Kenkyu, 1985, 36, 180. CA 704(21):184980q. (73J) Okubo. N.; Kawabata, N.; Koshida, K.; Miyazaki, M., Eisei Kagaku, 1985, 37, 274. CA704(15):128364e. Haswell, S. J.; Grzeskowiak, R., J . Anal. At. Spec(74J) Olayinka, K. 0.; trom., 1986, 7 , 297. CA705(19):170727w. (75J) Oyamada. Noritaka; Ueno, Seiichi; Kubota, Kaoru; Ishizaki. Mutsuo, Shokuhin Elseigaku Zassh 1985, 26, 13. CA 703(21):177066x. (76J) Peinado, Jose; Toribio, Fermin; Perez-Bendito, E., Anal. Chem ., 1986, 58, 1725. CA 705(1):5237d. (77J) Penchuk, Ya.; Haldna, U.; Ilmoja, K., J. Chromatogr.. 1986, 364, 189. CA 705(21):189568s. (78J) Puchyr, Richard, F.; Shapiro, Rubin, J. Assoc. OM. Anal. Chem., 1986, 69. 868. CAi05(21):189578v. (79J) Rubio, Soledad; Gomez-Hens, A.; Valcarcel, M.. Analyst (London), 1985, 170, 43. CA703(7):52768w.
FOOD (8OJ) Salinas, F.; Jlmenez Sanchez, J. C.; Gaieano Diaz, T., Anal. Chem., 1986, 58, 824. CA704(14)122077s. (81J) Sailsbury, Craig D.; Chan, Wayne, J. Assoc. Off. Anal. Chem., 1985, 68, 218. CA702(19):165348g. (82J) Schindlrneier, Wiihelm; Heumann, Klaus, G., Fresenius' 2 . Anal. Chem., 1985, 320, 745. CA103(3):21323t. (83J) Schindler, Erwin, Dtsch. Lebensm.-Rundsch., 1985, 87, 250. CAlO3(15):121857p. (84J) Schmuckler, G.; Roessner, 6.; Schwedt, G., J. Chromaragr., 1984, 362, 15. CA 101(23):209229e. (85J) Semu, E.; Seimer-Olsen, A. R.; Singh, B. R.; Steenberg, K., Fresenlus' ,?.Anal. Chem., 1985, 322, 440. CA 104(7):49902a. (86J) Shiralshi, Kunio; Kawamura, Hisao; Tanaka, G., Anal. Scl., 1985, 7 , 321. CA 104(9):67614n. (87J) Singer, Leon; Ophaug, Robert H., J. Agric. Food Chem., 1988, 34, 510. CA 104(23):205607r. (EN) Singh, Ishwar; Poonam, J. Indian Chem. SOC., 1988, 63, 259. CA 705( 19): 1707 1Ok. (89J) Singh, Ishwar; Poonam; Kadyan, P. S., Talanta, 1985, 32, 387. CA 703(7):50693u. (9OJ) Sinram, Roger D., JAOCS, J. Am. Oil Chem. Soc., 1988, 63, 667. CA 705(1):5271k. (9lJ) Srinlvas, 6.; Rao, V. R. S.; Kuriacose, J. C., J . Radloanal. Nucl. Chem., 1988, 703,347. CA 704(23):205610m. (92J) Stephen, Sharon C.; Littlejohn, David Ottaway, J., Analyst (London), 1985, 770, 1147. CA 704(9):67586e. (93.J) Stlive, T., Dtsch. Lebensm .-Rundsch ., 1985, 87, 321. CA 103- (25):213518g. (94J) Suddendorf, Ronald, F.; Cook, Kathleen K., J . ASSOC.Off. Anal. Chem., 1984, 67, 985. CA 707(21):189826s. (95J) Takeo, Tadakazu, JARQ, 1985, 79, 32. CA703(19):159190d. (96J) Tsukada. Shiro; Demura, Reiko; Yamamoto, Ikuo, Else/ Kagaku, 1985, 3711\. \.,, 37-41. - . . . . CA70315k36266a (97J)' Unger, Martina; Heumann, Klaus G., Fresenlus' 2 . Anal. Chem., 1985, 320, 525. CA 702(23):202703s. (98J) Vaessen, Hubert, A. M. G.; Van Oolk, A.; Zuydendrop, J., 2 . Lebensm .-Unters . Forsch., 1985, 787, 189. CA 703(19): 159221q. (99J) Vaeth, E.; Holz, E., Fefte, Seifen. Anstrichm., 1985, 8 7 , 97. CA702(22): 187038h. (1OOJ) Van Betteray-Kortekaas, A. M. G.; Vos, G., Fresenius' 2. Anal. Chem., 1986, 323, 493. CA 704(23):205639c. (101J) Van Eeden, C. H. Peter; De Jong, Alex W. J., 2 . Lebensm. Forsch., 1985, 187, 412. CA704(3):18704h. (102J) Viladrich Gonzalbez, E.; Forcadell Berenguer, M.; Buxaderas Sanchez, s.; Merine-Font, A,, Grasa Aceltes, (Sevllle), 1988, 37, 77. CA 705(9):77645h. (103J) Viacil, F.; Vins, I., Nahrung, 1985, 29, 467. CA103(11):86580u. (104J) Warner, C. R.; Daniels, D. H.; Joe, F. L.; Fazio, T., J. ASSOC.Off. Anal. Chem., 1988, 69, 3. CA704(11):87228t. (105J) White, R. Thomas, Jr.; Douthit, Garnett E., J. Assoc. Off. Anal. Chem., 1985, 68, 766. CA703(13):101265r. (106J) Wlchman, M. D.; Fietkau, R.; Fry, R. C., Appi. Spectrosc., 1988, 40, 233. CA 704(15):128359g. (107J) Wlechen, A.; Kock, B., Fresenius' 2 . Anal. Chem., 1984, 379, 569. CA 702(5):44475n. (ION)Yan, Daren; Stumpp, E.; Schwedt, G., Fredsenius' 2 . Anal. Chem., 1985, 322,474. CA704(5):33137u. (109J) Yan, Daren; Schwedt, Georg, Fresenius' 2. Anal. Chem., 1985, 320, 252. CA702(16):142487n. ~
MOISTURE
(IK) Bussiere, G.; Serpeiloni, M., NATO A S I Ser., 1985, Ser. E, 9O(Prop. Water Foods), 627. CA103(15):121828c. (2K) Chin, H. 6.; Kimball. J. R.; Hung, J.; Allen, B., J. Assoc. Off. Anal. Chem., 1985, 68(6), 1081-3. (3K) Chirife, Jorge; Resnlk, Slhria L., J. Food Scl., 1984, 49, 1486. CA707(2533228633~. (4K) Gambhir, P. N.; Agarwaia, A. K., JAOCS, J. Am. Oil Chem. Soc., 1985, 62, 103. CA102(9):7735Ow. (5K) Gerschenson, Lia; Favetto, Guillermo; Chirife, J., Lebensm Wiss . Techno/., 1984, 77, 342. CA 702(9):77352y. (6K) Kitic, D.; Pereira Jardlm, D. C.; Favetto. G.; Resnick, S.; Chirife, J., J. FoodSCl., 1988, 57, 1037. CA705(13):113772h. (7K) Koizumi, Hideo; Yasui, Akemi; Tsutsuml, Chiuchi, Nippon Shokuhin KOgyo Gakkaishi, 1984, 31, 465. CA 707(21):189822n. (8K) Labuza, T. P., Moisture Sorption: Practical Aspects of Isotherm Measurement and Use; Am. Assoc. of Cereal Chem. (AACC): St. Paul, MN, IQRA (SKj-Rueegg, M.; Steiger, G.; Moor, Ursula, Mlff. Geb. Lebensmiffelunters. Hyg., 1988, 77, 139. CA705(31):113718t. (10K) Rueegg, M.; Moor, Ursula, Mlft. Geb. Lebensmirtelunters.wg.,1988, 77. 131. CA105113k113715s. (11K)' S a n k Louis' A., J. Assoc. Off. Anal. Chem., 1988, 69, 834. CA 105(21):189577u. (12K) Smith, D. M.; Mitchell, J., Aquametry Pari 2. Electrical and Electronic Methods; Wiley: Chicester, Sussex, 1984. (13K) Stamp, J. A.; Linscott, S.; Lornauro, C.; Labuza, T. P., J. Food Scl., 49, 1139. CA101(19):169202g. (14K) Ueda, Masafuml; Shiba, Kamekichl, Moisture HurnMty, R o c . Int. Symp., 1985. 751. I S A Research Trlangle Park, NC. CA104(4):27977b.
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ORGANIC ACIDS
(1L) Ali, M. Sher, J. Assoc. Off. Anal. Chem., 1985, 66, 488. CA103(1):51OOn.
(2L) Ashoor, Sarny H.; Welty, Jim, J. Assoc. O f f . Anal. Chem., 1984, 67, 885. CA 701(23):209200p. (3L) Ashoor, Samy H.; Knox, M. J., J. Chromatogr., 1984, 299, 288. CA 707(19): 169219t. (4L) Badoud, R.; Pratz, G., J. Chromatogr., 1988, 360, 119. CA105(9):77637g. (5L) brgmeyer, Hans Ulrich; Moellering, Hans, Methods Enzym. Anal.. 1984, 6, 628. CA 102(11):92289b. (6L) Beutier, Hans Otto; Tischer, Wilhelm, Methods Enzym. Anal., 1985, 8, 80. CA704(5):33136t. (7L) Beutler, Hans Otto. Methods Enzym. Anal.. 1984, 6, 639. CA102(11):92290v. (EL) Boehme, Wolfgang; Oehme, Uirike; Steinwand, Micha, Lebensmiftelchem. Gerlchtl. Chem., 1984, 38, 88. CA101(17):149951x. (9L) Cereda, M. P.; De Almeida Lima, U., Turrialba, 1985, 35, 19. CA104(3): 18834a. (IOL) Chikamoto, Takeji; Maitani, Takeshi, Shokuhin Elseigaku Zasshi, 1984, 25, 342. CA 702(7):60874x. (11L) Chonan, Takao; Rakuno Kagaku, Shokuhin no Kenkyu, 1985; 34, A7. CA 103(7):52780u. (12L) Coppola, Eiia D.; Starr, Martin S., J . Assoc. Off. Anal. Chem., 1988, 69. 594. CA705(13):113743z. (13L) Engelhardt, Ulrich; Maler, Hans Gerhard, Fresenius' Z.Anal. Chem., 1985, 320, 169. CA 702(15):130552s. (14L) Fujlta, Shuji; Kawasaki, Hirotaks; Tono, Tetsuzo, Saga Daigaku Nogakobo Iho, 1985, 59. 27. CA704(15):128367h. (15L) Gancedo. M. Crlstlna; Luh. B. S., J. Food Sci., 1988, 51, 571. CA 105(7):59670h. (16L) Giffhorn, Freidrlch; Beutler, Hans Otto,Methods Enzym. Anal., 1985, 7, 78. CA703(19):158796v. (17L) Goto. Yuri; Liang, Zu Yu; Inoko, M.; Matsuno, T., Yokohama Kokuritsu Daigaku Kankyo Kagaku Kenkyu Senta Kiyo. 1984, 7 1 , 47. CA102(21):183808m. (18L) Hayakawa, KO; Shimazu, Kunihiko, Methods Enzym. Anal., 1986, CA - 104125k221668s. . , (19L) Healey, Kevin, W.; Carnevale, Joseph, J. Agric. Food Chem. 1984, 32, 1363. CA707(28):20898lg. (20L) Heinz. Fritz; Kohibecker, Guenther, Methods Enzym. Anal.. 1984, 6, 649. CA 702(9):75031u. (21L) Joex, E.; Pletzsch, W.; Froede, M., Lebensmiffelindustrie, 1986, 33, 79. CA 705(7):59525q. (22L) Katagirl, Mltsuakl; Shimizu, Sumio; Kaihara, Hiromichi, Nippon Nogei Kagaku Kalshi. 1988, 60, 385. CA105(11):96108b. (23L) Kayahara, Hlsataka; Yasuhara, Hitomi, Miso no Kagaku to Guutsu, 1984, 32, 242. CA707(15):128962m. (24L) Kikunaga, Shigeshl; Takahashi, Masayuki, Nippon Eiyo, Shokuryo Gakkaishi, 1985, 38, 123. CA103(17):140393a. (25L) Kogure, Kyoichi; Enomoto, Yasunori; Shibata, H., Patent, 1985. CA 704(13):108203y. (26L) Kok, W. T.; Groenendijk, G.; Brinkman, U. A. T.; Frei, R. W., J. Chromatogf., 1984, 315, 271. CA 702(9):75060c. (27L) Lagemann, M.; Graef, V.; Anders, D., Dtsch. Lebensm .-Rundsch, 1985, 87, 140. CA703(13):103523x. (28L) Lamkin, W. M.; Luginsland, N. D.; Pomeranz, Y., Cereal Chem., 1985, 62, 6. CA 702(21):183829u. (29L) Lamkin, W. M.; Unruh, N. C.; Pomeranz, Y., CereaiChem., 1988, 63, 372. CA 705(21):189558p. (30L) Lin, L.; Tanner, H., HRC CC, J. High Resolut. Chromatogr. Chromatogr. Commun., 1985, 8, 126. CA102(19):165344c. (31L) Littmann, S.,Dtsch. Lebensm. 1985, 87,345. CA104(5):33146w. (32L) Maimberg, Alf G.; Theander, Olof, J. Agric. Food Chem., 1985, 33, 549. CA 102(23):202686p. (33L) Matsumoto, K.; Ishida, K.; Nomura, T.; Osajima, Y., Agric. Bioi. Chem.. 1984, 48, 2211. CAI01(23):209213v. (34L) Matsuo, T.; Yorimitsu, A.; Kanehiro, M.; Kanamori, H.; Sakamoto, I., Hiroshima EiseKenkyusho Kenkyu Hokoku, 1984, 37. 47. CA 103(23): 195038~. (35L) Mattiuz, Edward L.; Perone, Ruth A,, LC, 1986, 4 , 552. CA 705(5):41355z. (36L) Mazzola, E. P.; Phillippy, 8. Q.; Harland, 6.; Miller, T.; Potemra, J.; Katslmpiris, E., J. Agric. Food Chem., 1988, 3 4 . 60. CA104(11):87191a. (37L) Mentastl, E.; Gennaro, M. C.; Sarzanini, C.; Baiocchi, C.; Savigilano, M., J. Chromatogr., 1985, 322, 177. GA702(21):183689y. (38L) Moellerlng, Hans, Methods Enzym. Anal., 1985, 7, 2 CA703(2 1):174758~. (39L) Moilica, Joseph N.; Morselli, Maria Franca, J. Assoc. Off. Anal. Chem., 1984, 67, 1125. CA702(13):111585p. (40L) Murakaml, R.; Yamamoto, K.; Kamiya, T.; Komuro, M.; Kakefuda, S.; Takai, K., Shokuhin Elseigaku Zasshl, 1984, 25, 360. CA707(25):228616v. (41L) Oen, Haakon; Vestrheim. Sigbjoern, Acta Agric. Scand., 1985, 35, 145. CA 103(19):159329f. (42L) Ohkawa, Hironori, J. Assoc. Off. Anal. Chem., 1985, 68, 108. CA 102(21):183841s. (43L) Otsuka, K.; Hori, M.; Sugltani, A,; Yamada, F.. GIFU N S E I KENKYUSHOHO. 1985, 30, 67. CA105(17):151616T. (44L) Panari, G., Mlichwlssenschaff, 1988, 4 7 , 214. CA 105(1):5246f. (45L) Picha, David H.,J. Agric. Food Chem., 1985, 33, 743 CA103(5):36256x. (46L) Procharka, Lubos; Kvasnicka. Frantisek; Stechova, Alena , Kvasny Prum., 1988, 32, 33. CA 705(7):59529u. (47L) Puttemans, Marc L.; Dryon, Louis; Massart, Desire, J. Assoc. Off. Anal. Chem., 1984, 67, 880. c~701(23):209199v.
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ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
249R
FOOD (48L) Puttemans, Marc L.; Branders, Chris; Dryon, Louis; Massart, Desire, J. AsSOC. Off. Anal. Chem., 1985, 68,80. CA102(21):183839x. (49L) Rabe, E., Veroeff. Arbeitsgem. Getreideforsch., 1984, 35, 114. CA f03( 17): 140403d. (50L) Rocklin, Roy D.; Slingsby, Rosanne, W.; Pohl, C. A., J. Li9. Chromatogr., 1988, 9 , 757. CA 104(23):203300m. (51L) Schaller, Karl Heinz; Triebig, Gerhard, Methods Enzym. Anal., 1984. 6, 668. CA 102(9):75032v. (52L) Spahis, Khira; KuzdzaCSavoie, Simone, Lait, 1984, 64, 579. CA 103(15): 121852h. (53L) Tsuda, T.; Nakanishi, H.; Morita, T.; Takebayashi, J.. J. Assoc. Off. Anal. Chem., 1985, 68, 902. CA 703(19):159201h. (54L) Tsuji, Masao; Harakawa, Mamoru: Komiyama, Y., Nippon Shokuhin Kogyo Gakkaishi, 1985, 32, 661. CAf04(13):108143d. NITROGEN
(1M) Abd El-Sahm, M. H.; AI-Khamy, A. F.; El-Etriby, H., FoodChem., 1988, 19, 213. CA104(19):167011g. (2M) Aiyar, K. R.; Greig, R. I.W.; Sangrouber. M. J. Food Sci., 1988, 51, 856. 858. CA 105(9k77653i. (3M) Andrews, A. T.: Taylor,-'M. D.; Owen, A. J., J. Chromatogr., 1985, 348, 177. CA 104(5):33126q. (4M) Arneth, Wolfgang, Fleischwirtschaft, 1984, 64, 1086. CA 101(25):2286 1Op (5M) Arnstadt, Klaus, Bangladesh J. Sci. Ind. Res., 1984, 191, 210. CA 104( 13): 108225g. (6M) Banu, Laila Arjumand; Ahmed, M. Kabir; Gomes, Joseph, Beng/adesh J. Sci. Ind. Res., 1984, 19(1-4), 210-19. CA 704(23):205777w. (7M) Barnett, Don: Howden, Marlin E. H., Food Technol. Aust., 1984, 36, 510. CA 702(3):22937n. (8M) Beattie, I.G.; Games, D. E.; Startin, J.; Gilbert, J., Biomed. Mass Spectrom., 1985, 12, 616. CA 103(25):213521c. (9M) Bender, A. E., Kiel. Milchwirtsch. Forschungsber., 1983, 35, 267, CA 103(11):86568w. (10M) Bengtsson, Lena, Fette, Seifen, Anstrichm., 1985, 87, 262. CA103(11):86612f. (11M) Bergmeyer. Hans Ulrich; Beutler, Hans Otto, Methods Enzym. Anal., 1985, 8, 454. Edited by Bergmeyer, H. U. CA 704(9):65052d. (12M) Beutler, Hans Otto, Methods €nzym. Anal.. 1985, 8, 369. Edited by Bergmeyer, H. U. CA 104(9):65045d. (13M) Beveridge, T.; Harrison, J. E., Can. Inst. Food Sci. Technol. J . , 1985. 78, 259. CA103(21):177052q. (14M) Blcan, P., Experientia 1985, 41, 958. CAf03(13):103562j. (15M) Bueser, W.; Erbersdobler, H. F., J. Chromatogr., 1984, 303, 234. CA 101(25):228820s. (16M) Burns, B. Garth; Ke. Paul J.. J . Assoc. Off. Anal. Chem., 1985. 68, 444. CA 103(1):5097s. (17M) Carisano, A., J. Chromatogr., 1985, 318, 132. CA f02(7):60872v. (18M) Carpenter, Robert N.; Brown, Rodney, J., J. Dairy Sci.. 1985, 68. 307. CA 102(19):165333y. (19M) Chang. Shyi Feu: Ayres. James W.; Sandine, W., J. Dairy Sci., 1985, 68,2840. CA104(5):33131n. (20M) Chong, C. S.; Kostalas, H.; Jervis, R. E., J. Radioanal. Nucl. Chem., 1988, 99, 359. CA 705(6):53869h. (21M) Chung, Siyin; Swaisgood, Harold E.; Catignani, G., J. Agric. Food Chem., 1985, 33, 201. CA102(13):111548d. (22M) Constantinescu, B.; Ivanov, E.; Plostinaru. D.; Popa-Nemoiu, A,; Pascovici, G., J. Radioanal. Nucl. Chem., 1985, 91, 389. CA103( 13):103561h. (23M) Csiba, A., Acta Aliment., 1984, 73, 189. CA 101(23):209183k. (24M) Cuq, J. L.; Cheftel, J. C.. Cah. Nutr. Diet., 1985, 20, 373, 377. CA 104(5):33079b. (25M) Dennison, C.; Gous, R. M., S. Afr. J. Anim. Sci., 1984, 14, 64. CA 70 I (17):149934u. (26M) Eka, 0. U.; Oyeieke, O.,Nlger, J. Biochem., 1984, I , 56. CA704(7):49914f. (27M) Ekstrand, B.; Larssondaznikiewicz. M., Milchwissenschaf?, 1984, 39, 591. CA 102(7):60853q. (28M) Eikin, Robert G.; Griffith, Joseph, E., J. Assoc. Off. Anal. Chem., 1985, 68,1117. CA104(5):33160w. (29M) Eikin, Robert, G.; Griffith, Joseph E., J. Assoc. Off. Anal. Chem., 1985, 68.1028. CA103(17):140444t. (30M) Elkin, Robert G., J. Assoc. Off. Anal. Chem., 1984, 67, 1024. CA - . 101 . (23k20921 ,--,----i t (31M) Findiay, C. J.; Parkin, K. L.; Stanley, D. W., J. FoodBiochem., 1988, 10. 1. CA104117k147357w. . , (32M) Fischer, Beatrice; Luethy, Juerg; Schiatter. C., Z.Lebensm. Forsch .. 1984, 179, 218. CA101(23):209225a. (33M) Friedman, Mendei; Noma, Amy T., J . Agric. Food Chem., 1988, 3 4 , 497. CA 104(23):205612p. (34M) Fritschy. F.; Windemann, H.; Baumgartner, E., Z. Lebensm. Forsch., 1985, 187, 379. CA103(25):213522d. (35M) Gavineili, M.; Airoldi, L.f Fanelll, R., HRC CC, J. High Resolut. Chromatogr. Chromatogr. Commun ., 1988, 9. CA 704(25):223723e. (36M) Gehrke, C. W.; Wail, L. L.; Absheer, J.; Kaiser, F.; Zumwait, R., J . AsSOC. Off. Anal. Chem., 1985, 68,811. CA103(17):140442r. (37M) Grassl, Mariannae; Supp, Martin, Methods Enzym. Anal., 1985. 7, 426. Edited by Bergmeyer, H. U. CA 103(21):174786q. (38M) Green. Marie R., J. Histochem. Cytochem., 1988, 34, 147. CA104(13k108120u. (39M) Greiner, Steven P.; Kellen, G. J.f Carpenter, D.,J. Food Sci., 1985, 50. 1106. CA 703(9):698916. (40M) Grimmer, Gernot; Naujack, Klaus Werner, J. Assoc. Off. Anal. Chem., 1988, 69, 537. CA105(3):23188r. (41M) Grivas, Spiros; Nyhammar, Tomas, Mutat. Res., 1985, 742, 5. CA 102( 19):1653 12r. ~~
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ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 19
(42M) Gustine, David L., J. Chromatogr., 1985, 319, 450. CA102(15): 130537r. (43M) Hach, Clifford, C.; Brayton, Scott V.; Kopeiove, A,, J . Agric. Food Chem., 1985, 33, 1117. CA103(25):210255h. (44M) Hayashi, Riklmaru; Suzukl, Fukuko, Anal. Biochem ., 1985, 749, 521. CA f03( 17):140410d. (45M) Heppell, L. M. J., Immunoassays Food Anal., 1985, 527. CA103(19):159181b. (46M) Honigs, D. E.; Hieftje, Gary M.; Mark, H. L.; Hirschfeld, T. B., Anal. Chem., 1985, 57, 2299. CA703(15):121814x. (47M) Horvath, L.; Norris, K.; Horvath-Mosonyi, M., Acta Aliment., 1985, 14, 113. CA 103(25):213508d (48M) Huet, Jean Claude; Pernollet, Jean Claude, J. Chromatogr., 1988, 355, 451. CA104(21):184964n. (49M) Ihekoronye, A. I., J. Food Technol., 1986, 21, 81. CA104(17):147276~. (50M) Ihekoronye, A. I.,J. Sci. Food Agric., 1985, 36, 1004. CA104(7):4993 l j . (51M) Ingles, D. L.; Black, J. F.; Gallimore, D.; Tindale, R., J. Sci. Food Agric., 1985, 36, 402. CA 703(7):52784y. (52M) Ingles, David L.; Gallimore, David, J. Chromatogr., 1985, 325, 346. CA 103(3):21332v. (53M) James, N. A.; Ryley, Janice, J. Sci. Food Agric., 1988, 37, 151. CA 104(17):147291v. (54M) Kaffka, K. J.; Martin, A. P., Acta Aliment., 1985, 14, 309. CA 704(15):128365f. (55M) Kane, Peter F., J. Assoc. Off. Anal. Chem.. 1986, 69, 664. CA 705(11):96135h. (56M) Keller, Ronald P.; Neville, Margaret C., Clin . Chem. (Winston N.C .), 1988, 32(Pt. I), 120. CA 704(11):87221k. (57M) Klrst, E.; Tschop, J.; Jahn, D.; Jacobi, U.. MF Milchforsch., 1985, 27, 12. CA 703(3):21300h. (58M) Kojima, Misao; Hamada, Hiroshi; Toshimitsu. Norik, Nippon Shokuhln Kwvo Gakkaishi. 1986. 33. 155. CA105(13~:113713a. (59M)-Kuninori, T.; khiyama, J., J. Chromato& 1986, 362, 255. CA 705f13k 113737a. (60M)' Lei, Mei Guey; Reeck, Gerald R., Cereal Chem., 1986, 63. 111. CA 104(23):20580lz. (61M) Lei, Mei Guey; Reeck, Gerald R., Cereal Chem.. 1988, 63, 116. CA 104(23):204040p. (62M) Lookhart, George L.; Jones, Berne L., Cereal Chem., 1985, 62, 97. CA 103(7):52788c. (63M) Lookhart, G. L.; Cooper, D. 8.; Jones, B. L., CerealChem., 1985, 62, 19. CA 102(21):183830n. (64M) MacDonald, John L.; Krueger, Mark W.; Keller, J., J. Assoc. Off. Anal. Chem., 1985, 68, 826. CA103(19):159200g. (65M) Mack, D. 0.; Reed, V. L.; Smith, L. D., J. Li9. Chromatogr., 1985, 8 , 591. CA 303(5):34377p. (66M) Manji, B.; Hill, A.; Kakuda, Y.; Irvine, D. M., J. Dairy Sci., 1985, 68, 3176. CA f04(13): 108019t. (67M) Matschiner, Hermann; Heberer, Henning; Guennel, G., Dev. FoodSci., 1988, 120. CA 105(2):17616q. (68M) Matsuda, Tsukasa; Kato, Yasuko; Watanabe, Kenji; Nakamura, Ryo, Dev. Food Sci., 1986, 13, 411-19. CA105(15):132239f. (69M) Mayanna, S.M.; Jayaram, B., J. Indian Chem. Soc., 1988, 63, 329. CA 105(18):164220j. (70M) McKillop, D. F.; Gosling, J. P.; Stevens, F. M.; Fotreli, P. F., Biochem. SOC. Trans.. 1985, 466-7. CA 703(3):21324u. (71M) Menger, Anita; Baudner, S.;Guenther, H. O., Getreide, Mehl Bot, 1985, 39, 149. CA703(11):8659ly. (72M) Moellering, Hans, Methods Enzym. Anal., 1985, 8, 350. Edited by Bergrneyer, H. U. CA 704(11):84573r. (73M) Moinar-Perl. I.; Pinter-Szakacs, M.; Kovago, A.; Petroczy, I.; Krab vanszky, U.; Matyas, J., Food Chem.. 1988, 20, 21. CA104(25):2237 12a. (74M) Nadirov, B. T., Vestn. SNaukiKaz.. 1985, 30. CAf03(15):119268d. (75M) Nguyen, T. T.; Sporns, P.; Hadziyev, D., J. Chromatogr., 1988, 363, 361. CA 705(19):170732u. (76M) Nielsen, Henrik K.; Hurrell. Richard F., J. Sci. FoodAgric.. 1985, 36, 893. CA 104l3):18740s. (77M) Oitner, Roland; Bengtsson, Staffan; Larsson, Kjel, Acta Vet. Scand., 1985, 26, 396. CAf04(13):108004j. (78M) Osborne, B. G., Dev. Food Proteins, 1988, 4 , 247. CA105(21):189509~. (79M) Overley, J. C., I n t . J. Appl. Radiat. Isot., 1985, 36. 185. CA103(3k21301i. (80Mj Pare&-Lopez, 0.; Guevara, L. F., Tecnol. Allment. (Mexico City), 1985. 20. 10. CA303115):121854k. (81M) Patterson, P. L., Lipus, 1985. 20, 503. CA103(17):140412f. (82M) Peleran, J. C.; Bories, G. F., J. Chromatogr., 1985. 324, 489. CA 10313k21307r. (83M) Perl, I.M.; Szakacs. M. P.; Kovago, A.; Petroczy, J., Food Chem.. 1985 16, 163. CAfOZ(19):165314t. (84M) Popineau, Y.; Pineau, Florence, Lebensm. Technol., 1985, 18, 133. CA 103(3k21305~. (85M) Poiras, 0.; Carisson. 6.; Faellstroem, S. P.; Hanson. L., Int. Arch. Allery Appl. Immunol., 1985, 78, 30. CA103(21):177113k. (86M) Raghavan, Sree K.; Ho, Chi Tang; Daun, Henryk, J. Chromatogr., 198s. 351, 195. CA104(11):87220j. (87M) Ray, P. K., Indian J. Nub. Diet., 1985, 22, 201. CA104( 17):147283~. (88M) Ribarova. F.; Shishkov, S., NAHRUNG, 1986, 303, 449. CA105(15):132236c.
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FOOD (89M) Ryder, John M., J. Agric. Food Chem., 1985, 33, 678. CA103(5):36250r. (90M) Samei, M. 8. A.; Elshafie, M. A.; Hanna, M.; Cskai, J.; Juhasz, M., J. Radioanal. Ncl. Chem., 1988, 103, 81. CA 104(17):147455b. (91M) SauraCalixto, F.; Cannellas Lourdes Soler, J., An. Bromatol., 1984, 1985, 36, 89. CA 103(9):69874a. (92M) Sen, Nrisinha P.; Seaman, Stephen W.; Kushwaha, S., Analyst (London), 1988, 111, 139. CA 104(25):223685u. (93M) Sjaunja. L. 0.; Andersson, I.,Acta Agrlc. Scand., 1985, 35, 345. CA 104(25):223694w. (94M) Skerritt, John, H.; Diment, John A.; Wrlgley, C., J. Sci. Food Agric., 1985, 36, 995. CA 104(7):49930h. (95M) Skerritt, John H., J. Sci. Food Agrlc., 1985, 36, 987. CA104(7):49929q. (96M) Skerritt, John H.; Smith, Robyn A., J. Sci. Food Agrlc., 1985, 36, 980. CA 104(7):49928p. (97M) Slump, P.; Bros, K. D., Poult. Sci., 1985, 64, 705. CA103(1):5087p. (98M) Tomareili, R. M.; Yuhas, R. J.; Fisher, A.; Weaber, J., J. Agrlc. Food Chem., 1985, 33, 316. CA102(13):111590m. (99M) Tuffnell, Janet M.; Payne, J. W., J. Appl. Bacterlol., 1985, 58,333. CA 102(25):21969 1j. (100M) Tummuru, M. K.; Sastry, C. S. P., J. Inst. Chem. (Indla), 1985, 57, 167. CA 104(11):87222m. (101M) Ukeda, H.; Miyazaki, E.; Matsumoto. K.; Osajima, Y., Anal. Chem., 1988, 58,2975. CA705(21):189548k. (102M) Valdes, E. V.; Summers, J. D., Poun. Sci., 1986, 65,485. CA705(1):5236c. (103M) Venter, B. G.; Scheepers, H. P.; Floor, J.; Snymaman, J., S . Afr. J. Dairy Technol.. 1985, 17, 107. CA105(1):5249]. (104M) Viroben, G., Rev. Aliment. Anim., 1985, 385, 45, 47. CA103(15):121836f. (105M) Wahlefekl, August Wilhelm; Sledei, Joachim. Methods Enzym. Anal., 1985, 8, 486. Edited by Bergmeyer, H. U. CA104(9):65054f. (106M) Wakabayashi, K.; Takahashi, M.; Nagao, M.; Sato, S.; Kinaa, N.; Tomita, I.; Sugimua, T., Dev. Food Sci., 1988, 363-371. CA105(19): 170696k. (107M) White, W. J. P.; Lawrie, R. A., Meat Sci., 1985, 72, 117. CA102(17): 147631q. (108M) Williams, Philip C.; Mackenzie, S. L.; Starkey, P., J. Agric. Food Chem.. 1985, 33, 811. CA103(25):213497z. (109M) Zee, J. A.; Simard, R. E.; L'Heureux, L., Lebensm. Technol., 1985, 18, 245. CA103(17):140437t. (llOM) Zomborszky, Kovacs Melinda, Magy. Allatorv. Lapja, 1985, 40, 539. CA 104(5):33097f. VITAMINS (1N) Aki, Hideml; Miyamoto, Teljiro, Kaseigaku Zasshi, 1985, 36, 929. CA 104(17):147281s. (2N) Ashoor, S. H.; Knox, M. J.; Oisen, J.; Deger, D. A,, J. Assoc. Off. Anal. Chem., 1985, 68, 693. CA703(11):86599g. (3N) Augustin, Jorg, J. Assoc. Off. Anal. Chem., 1984, 67, 1012. CA101(23):209208x. (4N) Augustine, J., Klein, B. P., Becker, D., Venugopal, P. B., Eds.; Methods of Vnamln Assay-Fowth Ednion; Wiley: New York. 1985. (5N) Ayi, Benjamin K.; Yuhas, David A.; Moffett. K. S.; Joyce, D.; Deangelis, N. J., J. Off. Anal. Chem., 1985, 68, 1087. CA704(7):49918k. (6N) Ayi, Benjamin K.; Yuhas, David A.; Deangelis, N. J., J. Assoc. Off. Anal. Chem., 1988, 69, 56. CA104(11):87237v. (7N) Bitsch, R.; Salz, I.; Hoetzei, D., Dtsch. Lebensm.-Rundsch., 1988, 82, 80. CA 104125k223700v. , (EN) Bognar, Antal, 2. Lebensm. Unfers. Forsch., 1985, 181, 200. CA 703123k195029s. (9N) Bogna;, Antal, 2. Lebensm. Unters. Forsch., 1986, 182, 492. CA 105(11):96139n. (10N) Brubacher, G.; Mueller-Muiot, W.; Eds., Elsevier: London, UK, 1985; I66 pp. CA103(19):159399d. (11N) Coburn, Stephen P.; Mahuren, J. Dennis, Mefhods Enzymol., 1988, 122(Vltam. Coenzymes, Pt. G), 102. CA 105(11):93896w. (12N) Colugnati, Luigi, Boll. Chlm. Ig., Parfe Sci., 1985, 36(S2), 65. CA 703(21):177038n. (13N) Coverly, Stephen C., J. Mlcronufr. Anal., 1985, 1, 65. CA104(7):49910b. (14N) Davidek. Jirl; Vellsek, Jan, J. Mlcronutr. Anal., 1988, 2, 61. CA105( 13): 113699q. (15N) DeLeecher, A. P.; Lambert, W. E.; DeRuyter, M. G. M., Eds., Modern ChromafographlcAnalysis of Vnamins; Marcel Dekker: New York, 1985. (16N) Echois, Richard E.; Miller, Robert H.; Thompson, L., J. Chromatogr., 1985, 347, 89. CA 703(25):213502x. (17N) Echols, Richard E.; Miller, Robert H.; Foster, Wllllam, J. Dairy Sci., 1986, 69(5), 1246-1249. CA 105(7):59511g. (18N) Ekanayake, Athula; Nelson, Philip E., Br. J. Nufr., 1986, 55, 235. CA 104117k147266r. (19N) Esaka, Muneharu; Suzuki, Kanlchi; Kubota, Klyoshi, Agric. Bioi. Chem., 1985, 49, 2955. CA 103(25):213510y. (20N) Finglas, P. M.; Faulks, R. M., Food Chem., 1984, 15, 37. CA10112 1I: 1898100. (21N) ' Ge, Ho& Oman, Gary N.; Ebert, Frank J., J. Assoc. Off. Anal. Chem., 1986, 69, 560. CA 105(5):41347y. (22N) Gerstenberg, Holger, Lebensmlffelchem, Gerichfl. Chem ., 1985, 39, 1. CA 102(15):130543q. (23N) Grace, Margaret L.; Bernhard, Richard A., J. Dairy Sci., 1984, 67, 1646. CA101(21):189807m. (24N) Greaorv, Jesse F., 111. J. Assoc. Off. Anal. Chem.. 1984, 67, 1015. . CA 101~23j209131s. (25N) Gregory, Jesse F., 111; FeMstein, Debra, J. Agric. Food Chem.. 1985, 33(3), 359-63. CA 702(23):202672f.
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(26N) Guilarte. Tomas R., Nuh. Rep. Inf., 1985, 32, 037. CA104(3): 18726s. (27N) Hernandez-Mendez, J.; Alonso Mateos, A.; Almendral Parra, M. J.; Garcia de Marla, C., Anal. Chim. Acta, 1986, 184, 243. CA105(18): 164225q. (28N) Holz, Friedhelm, 2. Lebensm. Unters. Forsch., 1984, 779, 29. CA 107 (23):209169k. (29N) Hwang, Shie Ming, J. Assoc. Off. Anal. Chem , 1985, 68(4), 684-9. CA103(11):86598f. (30N) Jaumann, G.; Engelhardt, H., Chromafographia, 1985, 20, 615. CA 104(3):18718r. (31N) Knelfel, W.; Sommer, R., Ernaehrung (Vienna), 1986, 10, 459. CA 105(19): 170741w. (32N) Kneifel. Wolfgang; Sommer, Regina, 2 . Lebensm. Unfers , Forsch., 1985, 181, 107. CA 103(19):159191e. (33N) Kneifel, W., Dtsch. Molk. Zig., 1986, 107, 212, 216. CA104(25):223720b. (34N) Kobayashi, Tadashi; Okano, Toshlo; Takeuchi, Atsuko, J. Micronub, Anal., 1988, 2, 1. CA105(3):23134x. (35N) Kodaka, Kaname; Inagaki, Setsuko; Ujiie, Takashi; Ueno. Toshio; Suda, Hiroyuki, Bifamln, 1985, 59, 451. CA 103(25):213475r. (36N) Lambertsen, Georg, Roc. Scand. Symp . Lipids, 12fh, 1983, Maruse, R. Ed., Llpidforum: Goeteborg, Swed, 1984. CA 104(1):4720y. (37N) Landen, Willlam O., Jr., J. Assoc. Off. Anal. Chem., 1985, 68, 183. CA 102(21): 183823n. (38N) Lau, 01 Wah Luk. Shiu Fai; Wong, Kit Sum, Analyst (London), 1988, 117 , 665. CA 705(17):151620q. (39N) .Law 01 Wah; Shlu, Kwok-Keung; Chang, Shu Ting, J. Sci. Food Agr/C., 1985, 36(8), 733-739. CA 103(25):213491t. (40N) Lazaro, F.; Rios, A.; Luque de Castro, M.; Valcarcel, M., Analyst (London), 1988, 111, 163. CA104(24):213343s. (41N) Mauro, D. J.; Wetzel, D. L., J. Chromatogr., 1984, 299(1), 281-7. CA 10 1(19):1692 18s. (42N) Mills, Robert S., J. Assoc. Off. Anal. Chem.. 1985, 68, 56. CA702(2 1):183836~. (43N) Oesterdahl. B. G.; Janne, K.; Johansson, E.; Johnsson, H., Int. J. Vifam. Nufr. Res.. 1988, 56,95. CA105(1):5257k. (44N) Pachia, Lawrence A,; Reynolds, D. L.; Kissinger, P., J. Assoc. Off. Anal. Chem., 1985, 68, 1. CA 102(23):202632t. (45N) Rammell, Coiin G.; Hoogenboom, Jacobus J. I., J. Liq. Chromatogr., 1985, 8, 707. CA 103(9):67656g. (46N) Rychener, M.; Walter, P., Mift. Geb. Lebensmiftelunters. Hyg., 1965, 78, 112. CA103(1):5086n. (47N) Schiaffer, Gary W.; Wheeler, Glenn P.; Cimino, C., J. Liq. Chromafogr., 1984, 7, 2659. CA 102(5):44491q. (48N) Seki, Tokuichiro; Yamaguchi, Yoshihisa; Noguchi, Kohji; Yanagihara, Y.. J. Chromafogr., 1985. 332, 283. CA703(19):159217t. (49N) Sell, U., Fresenius' 2.Anal. Chem., 1984, 318(3-4), 287. CA101(15): 128973r. (50N) Sertl. David C.; Molltor, Bruce E., J. Assoc. Off. Anal. Chem., 1985, 68, 177. CA102(21):183822m. (51N) Shen, C. S. J.; Sheppard, A. J., J. Micronutr. Anal., 1986, 2, 43. CA 705(3):23166j. (52N) Speek, A. J.; Schrijver, J.; Schreurs, W. H. P.,J. Food Sci., 1985, 50, 121. CA702(13):111765x. (53N) Speek. A. J.; Temalilwa, C. R.; Schrijver, J., food Chem., 1986, 19, 65. CA704(13):108021n. (54N) Stancher, Bruno; Zonta, Fabio, J. Chromatogr., 1984, 312, 423. CA 102(7):60644n. (55N) Trugo, L. C.; Macrae, R.; Trugo, N. M. F., J. Micronutr. Anal., 1985, 7 , 55. CA 704(7):49909h. (56N) Vandersiice. J. T.; Brownlee, S. R.; Cortissoz, M. E., J. Assoc. Off. Anal. Chem., 1984, 67, 999. CA 701(25):228589p. (57N) Vanderslice, Joseph T.; Higgs, Darla J., J. Chromafogr. Sci.. 1984, 22. 485. CA10213k22934i. (58N) 'Veiisekl Jan;DaCidek, Jii; Mnukova, J.; Pistek, T., J. Micronufr. Anal., 1988. 2. 73. CA705115k132231x. (59N) Velisek, Jan; Davidek: Jiri, J. Micronutr. Anal., 1986, 2 , 25. CA105(3):23135y. (60N) Watada, Alley E.; Tran, Tony T., J. Liq. Chromatogr., 1985, 8, 1651. CA 103(17):140432n. (61N) Wills, R. B. H.; Wimalasiri, P.; Greenfield, H., J . Micronutr. Anal., 1985, 1, 23. CA 104(7):49906e. (62N) Wlmalaslrl, P.; Wills, R. 8. H., J. Chromafogr., 1985, 318, 472. CA 702(11):94420m. (63N) Wooliard, D. C.; Blott, A. D., J. Micronutr. Anal., 1986, 2 , 97. CA 105(15): 132232~. (64N) Zonta, Fabio; Stancher, Bruno, J. Chromafogr., 1985, 329, 257. CA 103(11):86567b. MISCELLANEOUS (1P) Allen, J. C., BNF Nutr. Bull. 1988, 11, 46. CA104(23):205599q. (2P) Bernardini, M.: Fedell, E.: Baroni, D., Riv. Ital. Sostanze Grasse, 1985, 62, 357. CA104(9):67550p. (3P) Boppel, B.: Fischer, E.; Frindik, 0.; Kalus, W.; Mueller, H.; Schelenz, R., Report, 1984. CA104(13):105094c. (4P) Charalambous, G.,Analysis of Foods and Beverages, Modern Techniques; Academic: Orlando, FL, 1985. (5P) Cox, D.; Harrison, G.; Jandlk, P.; Jones, W., Food Techno/. (Chicago), 1985, 39, 41. CA103(17):140400a. (6P) Davies, A. M. C.; Grant, A.; Gavrel, G.; Steeper, R.. Analyst (London) 1985, 110, 643. CA 104(13):108041u. (7P) Frankhuizen. R.: Van der Veen, N. G., Neth. Milk Dairy J. 1985, 39, 191. CA 104(11):87209n. (8P) Giacin, Jack R.; Brzozowska, Anna, J. flast. Film Sheeting. 1985, 7 , 292. CA 104(23):205583e. ANALYTICAL CHEMISTRY, VOL. 59,
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Anal. Chem. 1987, 5 9 , 252R-280R (9P) Hischenhubr, Cladla, Lebensrn. Biotechnol., (Sonderh .), 1985. 4 , 7. CA 104(15):128282b. (1OP) King, R. D., Ed., Developments in Food Analysis Technques-3; Elsevier:1985. (11P) Kress-Rogers. Erika, J . Phys. E : Scl. Instrum., 1986, 19. 13. CA 10415):128283~. (12P) Miebs, Angelfka; Kirst, Eberhard, Mf -MP, MHchtorsch.-Milchprax ., 1986, 28, 47. CA 105(7):59500c. (13P) Morris, €3. A.; Clifford, M. N., Eds., Immunoassay in Food Analysis; Elsevier:1985. (14P) Nadai, B. T.; Mihalyi-Kengyei, V.. Acta Aliment., 1984, 13, 343. CA 102( 19): I6531 7w. (15P) Nakaoka, A.; FukuSMma, M.; Tsukamto, M.; Taka@,S., J . Radloanal. Nucl. Chem., 1986, 99, 203. CA104(25):221377w. (16P) Raemy, A.; Mlchel, F.; Lambelet, P., Calorlm. Anal. Therm., 1984, 15, 11. CA 102(25):219688p.
(17P) Ronalds, John A.; Miskelly, Diane, Chem. Aust., 1985, 5 2 , 302. CA 105(17): 151604n. (18P) %to, Tetsuo; Iwamoto, Mutauo; Hashizume. Karumot; Yoshino, Masazumk Furukawa, S. Someya, Yuklo; Yano, N., Nlppon Chkusan Gakkaiho, 1985, 56, 878. CA14(17):14726Oj. (19P) Schwedt, Georg; Attkofer, Werner, GIT fachz. Lab ., 1985, 29, 369, 373, 377. CA103(3):21327x. (20P) Valdes, E. V.; Summers, J. D., Poult. Sci., 1986, 6 5 , 485. CA105( 1):5 2 3 6 ~ . (21P) Wernimont, G. T., Spendiey, W., The Use of Statistics to Develop 8 Evaluate Analytical Methods; Assoc. Offic. Anal. Chem.: Arlington, VA, 1985.
(22P)WOolerd, David C., food Techno/. N . Z . , 1986, 21(3), 36-37, 39, 55. CA 105(1):5219z. (23P) Yeransian, James A.; Sloman, Katherine G.; Foltz, Authur K.. Anal. Chern., 1985, 5 7 , 278R. CA 102(17):147589g.
Petroleum F.C. Trusell Consulting Analytical Chemist, 6910 South Prince Way, Littleton, Colorado 80120
This is the 18th review in a series dating back to 1953. Complete bibliographic references to previous articles will be found in the 1985 review (1A). Abstracts of papers covered in this present work appeared in Chemical Abstracts, Analytical Abstracts (London), and the American Petroleum Institute Refining Literature Abstracts during the period July 1984 through June 1986. Reviews of this scope are the work of many hands. Each author is named at the beginnin of their section. Two significant contributors, however, wor in relative anonymity. C. H. Simpson, a t Mobil, and D. K. Albert, at Amoco, search the abstract literature during the biennium between reviews to provide the references reported herein. The authors’ tasks are made much easier by their work. Frequently a paper appears to fit, with equal validity, into either of two (or more) categories. The decision about where to place it is made thus: If the principal thrust of the paper seems to be to characterize the sample, the paper goes in Section B-Crude Oil Section C-Fuels, Gaseous and Liquid Section D-Lubricants, Greases, and Specialty Oils Section E-Asphalts, Bitumens, Tars, Pitches, and Waxes If the principal thrust of the paper seems to be to analyze the sample for a particular element, compound, class of compounds, or physical pro erty, the paper goes in Section F-Hydrocar ons Section G-Physical Properties Section H-Metals in Oil Section I-Nonmetal Elements and Compounds If the paper appears to emphasize the method or equipment used, it goes in Section J-Analytical Methods and Apparatus
E
E
CRUDE OILS T. Yonko Marathon Oil Company, Littleton, Colorado 80 160
The petroleum industry has seen considerable changes over the past several years affecting all areas of the industry. However, analytical testing in support of the petroleum industry has not waned. Although analytical developments for oil shale and shale oil have decreased, new methods and techniques for petroleum and coal flourish The following section is divided into three major subsections (Crude Petroleum, Coal Oil, and Shale Oil). Major topics and advances over the last few years are presented.
CRUDE PETROLEUM Exploration. General. Mironova, Rostotskaya, and Naumov developed a pyrochromatographic technique for 252 R
detecting HzO, COz, CHI, and hydrocarbons during oil and gas prospecting (1B).Colling and colleagues used multidimensional pyrolysis gas chromatography for studying organic geopolymers found in sedimentary rocks (2B).Pyrolysis GC techniques on kero ens, rocks, asphaltenes, and petroleum were used by Behar &B). Schaefer trapped and analyzed gases from heated rock samples on an SE-54 fused silica column using a commercial thermodesorption unit as an injection device (a, 5B).Shang studied the geochemical characteristics and ap lications of aromatics in crude oil (6B,7B). The course of biofegr adation was followed by gas and liquid chromatography detection on crude oil from the Gifhorn trough, Lower Saxony region. The work was done by Teschner and Wehner (8B). Seifert et al. found that surviving biomarkers in biodegraded oils could be used for source correlation (9B). G h o u r , Swart,and Pillinger used GC and stable isotope mass spectrometry to investigate the carbon isotope composition of individual petroleum alkanes (IOB).Killops and Readman determined aromatic hydrocarbons from oils and sediments by HPLC fractionation and GC/MS ( I I B ) . GC/MS was used to analyze volatiles in fluid and gas inclusions, which provided information on process history (12B). Gurko and colleagues found that petroleums diffusing through geological strata fractionated (13B, 14B). Rullkoetter, Spiro, and Nissenbaum examined the biological marker characteristics of oils from carbonate source rocks in the Dead Sea, Israel (15B). Curiale and associates studied biomarkers in oils and rocks of the Monterey Formation, California (16B), and Li and associates studied the biomarken in source rocks of Nanyang, Damintun, and Liaohe Basin in China (17B).Meyer, Christie, and Brooks used GC/MS with selective metastable-ion monitoring to obtain biomarker information (184 19B). Similar work was also done by Philip and Gilbert (20B). Srivastava characterized petroleum crudes of Indian origin by NMR (22B).Kvalheim and Telnaes also used NMR to characterize Norwegian North Sea oils (22B). Zav’yalov and Razumova geochemically compared petroleums and natural bituminoids by inrared spectroscopy (23B). Tezuka and colleagues characterized Abu Dhabi and Japanese domestic crudes by using NMR and IR (24B). IR and X-ray diffraction helped in the analysis of insoluble organic matter in Domanik rock of the Tman-Pechora region from depths
