P., Massart, D. L., Fresenuis’ Z.Anal. Chem., 208 (I), 21-3 (1976)(Eng.); Chem. Abstr., 85, 56230. (126)Van Rosmalen, H. A,, Soil Sci. Soc. Am. Proc., 39 (4),809 (1975);Fert. A, 9, 409. (127)Verigina, K. V., Dobritskaya, Y. I., in “Me-
tody Opred. Mikvelem. Pachvakh, Rast Vodakh”. I. G. Vazhenin, Ed., Koios, Moscow, USSR, 1974, 25-145 (Russ.); Chem. Abstr., 84, 120275. (128)Wall, L., Sr., Gehrke, C., scheduled for publication in May 1977, J. Assoc. Off. Anal. Chem. (129)Warner, D. A., Paul, J., Microchem. J., 20 (3),292-98 (1975);Ferf. A, 9, 598. (130)Wherley, S.K.. Jones, C. E., J. Assoc. Off.
Anal. Chem., 58 (5),928-36 (1975). (131)Williams, C.,J. Sci. Food Agric., 27 (6), 561-70 (1976);Ferf. A, 9,2104. (132)Wise, W., Anal. Lett., 7 (IO), 637-46 (1974);Chem. Abstr., 82, 67914. (133)Wiseman, B. F. H., Bedri, G. M., J. Radioanal. Chem., 24 (2),313-20 (1975);Fert. A, 8, 1549. (134)Woodls, T., Jr., Hunter, G., Johnson, F., J. Assoc. Off. Anal. Chem., 59 ( I ) , 22-5 (1976). (135)Yamasaki, S.,Yoshino, A,, Kishita, A,, Soil sci. Piant ~ u t r(rokyo), . 21 (I), 63-72 (1975)(Eng.); Chem. Abstr.. 83. 77467.
dova, N. A., Agrokhimiya., 4, 131-4 (1975);Chem. Abstr., 83, 26763. (137)Zemel’man, V. B., Sov. Chem. ind., (Eng. Transl.), 7 (6),1260-1 (1975);Fert. A, 9, 246. (138)Zhemaituk, L. N., Kamrads, A,, Nauchn, Konf. Khim-Anal. Pribalte. Resp. 6. SSR (Yezisy Koki.), 118-24 (1974)(Russ.); Chem. Abstr., 85,
106227.
Contribution Of the Missouri Agricultural Experiment Station. Journal Series No. 7770. Amroved bv the Direc-
Food Arthur K. Foltz,” James A. Yeransian, and Katherine G. Sloman General Foods Technical Center, White Plains, N.Y. 10625
This review attempts to encompass the advancements and refinements in the analysis of foods that have occurred or come to the authors’ attention within the period October 1974 to October 1976. Its structure is similar to that of the previous one (22P) and space considerations dictated that selectivity be exercised. Where similar work has appeared in domestic or widely circulated journals as opposed to obscure ones, the former citations have been made. A new edition, the Twelfth, of the “Official Methods of Analysis of the Association of Official Analytical Chemists” (16P)appeared in 1975. Lees (12P)authored a text on food analysis. The Society of Soft Drink Technologists published their “Quality Control Methodology” (18P).
ADDITIV ES Procedures for additives have kept pace with analytical technology but consist for the most part of refinements since new allowable additives are minimal. A standard procedure of qualitative analysis for food additives using thin-layer chromatography was published by the International Organization of the Flavour Industry (17A).Mordret (32A)used a solvent partition-colorimetric test to detect 10 ppm BHT in suet. Singh et al. (50A)estimated BHA and B H T in meat using gas chromatography after extraction and alumina column clean-up. Kaito et al. (20A) studied a fluorimetric detection method for BHA using Fe ( C N ) G ~ -oxidation. Hurtubise (14A) selectively measured propyl gallate by quenching the fluorescence of other antioxidants with chloroform. Gallic acid esters in fats were correlated to bathochromic absorbance effects upon addition or alkaline buffer to the 80% MeOH solution in a method by Cuzzoni et al. (4-4). An automated analysis based on hydroxylation, and color formation with 4-aminoantipyrine was described by Van Gend (58A) that also incorporated a continuous initial volatile separation. Zonneveld (62A)eliminated interferences in an ultraviolet spectrophotometric method for benzoic and sorbic acids by acid dichromate oxidation. Procedures for extraction and determination by GLC of TMS derivatives for benzoic, sorbic, and 4-hydroxybenzoic acids in cheese and other foods were described by Larsson et al. (29A).Gutfinger et al. (IOA) steam distilled benzoic and sorbic acids from orange juice before separate spectrophotometric determinations. Fogden et al. ( 8 A )directly injected “Tris” salts of sorbic and benzoic acids onto a Porapak column after extraction from food. Errors in sorbic acid determination by reaction with p-hydroxybenzaldehyde were discussed by Iioka (26A) and attributed to ginger and spice components. Volatile interferences from wines and fruits were minimized by alkaline evaporation of the distillate in a sorbic acid method by Mandrou et al. (30A). Roy et al. (44A) used a gas diffusion membrane instead of steam distillation for separation in their automated sorbic acid 194R
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procedure. A rapid UV method for sorbic acid in prunes was published by Stafford (53A).Van Bronswijk (57A)corrected UV interferences to measure sorbic acid in wines by subtracting absorbance at another wavelength. Franco et al. (9A) used emission spectroscopy to measure boric acid in caviar. The hydrolysis rate of diethyl dicarbonate was studied by Drozd et al. ( 5 A ) .A variety of preservatives in wine were detected by acid-ether extraction followed by direct as well as gas chromatography after methylation in the work by Revuelta et al. (43A).The interference of phenoxyacetic acid herbicides in colorimetric assay for monohaloacetic acids was detailed by Baluja et al. ( 1 A ) .Kaneshima e t al. (22A) employed TLC, colorimetric, and GLC methods to detect phthalic acid esters in, e.g., soy, laver, and sake. Sontag et al. (52A) used steam distillation, thiourea formation, CdS separation, and final titration or colorimetry to determine isothiocyanate in samples. EDTA in pickled vegetables was extracted, methylated, and measured using GLC by Williams (60A).The preservative furylfuramide was solvent extracted from food, cleaned up on florisil, reacted with (C4F7CO)O and measured by GLC in the procedure of Tanaka e t al. (40A). Sakai et al. (45A)used TLC for this species and measured it on the plates. Yoshikawa et al. (61A) after their TLC separation, developed the color from reaction of the spot eluate with sulfamine and naphthylethylenediamine. Reductones added to beer were precipitated and separated by TLC as their 2,4-dinitrophenylhydrazonederivatives in the work of Jerumanis et at. (19A).Hils (13A)applied a fluorescein procedure for Br- to the microdetermination of brominated vegetable oils in soft drinks. A review on the analysis of nitrate and nitrite in foods was published by Usher et al. (56A).Weisz et al. (59A) employed a ring oven technique for nitrite and nitrate a t nanogram levels. The nitrate selective electrode was investigated as a tool for analysis of baby food and reported to correlate to the AOAC xylenol method by Pfeiffer et al. (41A).Karlsson et al. (23A)coulometrically titrated nitrite from meat products with iodine generated in a cell. These same authors (24A) also measured nitrate after reduction by coppered cadmium. An automated procedure for nitrite and nitrate using a Technicon apparatus was reported by Hauser et al. (11A).The errors introduced from filter paper used in nitrite analysis were described by Fiddler e t al. ( 7 A ) in their paper. An improved canned food method employing tin removal and a larger sample but based on Kamm’s method was reported by Eipeson et al. ( 6 A ) .Coppola et al. (3A)measured nitrite indirectly in meats by fluorometric measurement of excess sulfanilic acid reacted with fluorescamine after a diazotization. Monoglyceride emulsifiers were separated by TLC after butanol extraction from alimentary pastes in the procedure of Schmid et al. (48A).Sodium steroyl-lactate was detected in the presence of other emulsifiers on a TLC plate by Regula
Aurthur K. Foltr, a Research Specialist at General Foods Central Research Analytical Laboratories has a background of analytical methodology encompassing techniques for major and trace components in food and biological systems as well as related areas, e.g., environment and packaging. instrumental applications including realtime laboratory computer automation of chromatographic and wet chemical methods best describes his recent specialization.
James A. Yeranslan, Senior Laboratory Manager, General Foods Central Research Department (B.A., Cornell University and M.S., Adelphi College), is the supervisor of the Corporate Analytical Laboratories. He was employed as an analytical chemist by National Dairy Research Laboratories from 1948 to 1955 before joining General Foods. He has held positions in both the Corporate and Jell-0 Research Areas. His work experience includes analysis of foodstuffs and natural flavors and development of analytical methods and instrumental capabilities for both research and oualitv control. He is an associate referee of the Association of Official Analytical Chemists and a member of the American Chemical Society and AAAS. He serves as a member of the US. delegation of the Codex Alimentarius Committee on Analysis and Sampling.
Katherine G. Sloman, Senior Research Specialist, Analytical Chemistry, General Foods Central Research (B.A.. Smith College and M.A., Columbia University), has specialized in the application of analytical procedures to foods. She has had wide experience with the standard methods of food analysis and with the problems encountered both in methad development for specific problems, and for the needs of quality control. Recently she has worked on special methods required for the determination of food additives, for other trace components in foods, and on automation of methods applicable to foods.
(42A).Kroller (27A)reported a general colorimetric method for detecting lactic and acetic glyceride-based emulsifiers. Nishijima et al. (38A)employed DEAE-cellulose and carbon columns to clean up ether extracts before atomic absorption measurement of dimethylpolysiloxane in foods. A short column method followed by a fluorescamine fluorimetric measurement enabled Coppola et al. ( 2 A )to detect 0.05% of MSG in foods. Marine Font e t al. (31A) read the ninhydrin color after ion exchange for monosodium glutamate in baby foods. Kalinowski (21A) potentiometrically titrated MSG with HCHO present in his method. The artificial sweetener saccharin was methylated by action of diazomethane before gas chromatography by Unterhalt (%A) who reported other products formed also in the reaction. Nagai et al. (33A)used dimethyl sulfate to derivatize saccharin before GLC of the N-methyl product. Tanaka et al. (54A) monitored the absorption at 254 nm in their HPLC method for saccharin in foods. Ultraviolet absorbance measurement after Zn-HC1 reduction and alumina clean up was described as a saccharin method by Nakamura et al. (34A).Preliminary extraction and correction a t another UV wavelength enabled Hussein et al. (15A)to measure saccharin in chewing gum and other foods. Nakamura (35A)measured saccharin fluorimetrically in alkaline solution after removal of interferences with permanganate. Smyly et al. ( 5 I A )simultaneously separated saccharin, caffeine, and benzoate in beverages by HPLC. Sigematsu et al. (49A) prepared electrodes responsive to saccharin and some antiseptics that, however, had limited
selectivity. Hazemoto et al. (12A) described their electrode that functioned in the presence of other sweeteners to measure saccharin. Kodama e t al. (26A) reduced saccharin with ZnHCI before TLC to increase sensitivity. Different TLC solvent and coating systems were examined by La Rotonda e t al. (28A) in their saccharin and cyclamic acid separations. A fluorimetric determination of cyclamate with 1,2-naphthoquinone-4-sulfonic acid was published by Sakai et al. (46A) and applied to foods (47A). An electron capture GC micromethod for cyclamates as N-heptafluorobutrylcyclohexylamine derivatives was described by Nagasawa et al. (36A).The trifluoroacetyl counterparts were measured previously using flame ionization by Nagasawa e t al. (37A). L-Aspartyl-Lphenylalanine methyl ester was determined by Nishijimi et al. (39A)by dialysis from a food sample followed by TLC or HPLC. Ishiwata (18A) determined this sweetener with an amino acid analyzer and showed good recovery from foods. A simple method for polysaccharides by precipitation after enzymic hydrolysis of lipids and proteins was shown by Klostermeyer et al. (25A).
ADULTERATION, CONTAMINATION, DECOMPOSITION Many publications continue to appear that report the ability to detect adulteration in very specific cases, e.g., two widely dissimilar fats in admixture being differentiated by fatty acid methyl ester analysis. Many of these have necessarily been omitted for the sake of brevity and because the techniques employed are routine laboratory practice a t this time. Nissenbaum et al. (118B)employed mass spectrometric techniques to measure the l80to l60ratios in the water phase of orange juices and the 13C to 12C ratio in the solids phase which data allowed them to project utility in detecting added water or cane sugar. Tugetes extracts in orange juices and oils were separated and detected by Wild et al. (189B) using an alumina column and final HPLC separations of xanthophyll esters. Atomic absorption of a methyl ethyl ketone oil solution permitted Gegiou (53B)to measure olive oil adulteration with soap as sodium from soap. An extensive analytical scheme including determination of sterols, fatty acids, and triglycerides by as chromatography was used by Imai et al. (74B) to define etection limits for adulteration of various oils with others. Datura alkaloids in millet were determined by TLC in the test of Bose et al. (8B).Gyromitrin in false morels was extracted and characterized by Schmidlin-Meszaros (155B). Chand et al. (13B) detected 3% mineral oil in edible oil with AgNOB-plate TLC. Farmer (31B)separated mineral oil and vegetable oil in furfural-dioxane solvent phases. Contributions to the techniques of analyzing traces of mycotoxin contaminants in foods have continued to proliferate since the last review. Durackova et al. (25B)described their scheme for systematic chromatography of 37 mycotoxins by TLC. Hagan et al. (62B)found they could avoid streaking of ochratoxin by choosing proper solvent systems for double development TLC in their mycotoxin in oil procedure. Heathcote et al. (68B)tested adsorbants and solvent systemawith an Aspergillus fluvus extract to determine the best TLC system. El-Nawaway (27B) reported quantitative recovery in his aflatoxin in meat method that employed silica gel column clean-up before TLC. Bencze et al. ( 6 B )studied procedures needed to identify aflatoxins a t levels below 50 ng using mass spectroscopy. A pulsed Nz laser was used by Berman et al. ( 7 B )to induce fluorescence on TLC plates, 0.2 ng of aflatoxin B1 having been detected. The use of dialysis as a cleanup method before TLC analysis was investigated for 12 mycotoxins by Roberts et al. (140B). The relative merits of four different extraction systems for aflatoxins in coconut were given by Samarajeewa et al. (151B).Beljaars et al. (5B)surveyed spices for aflatoxins wherein positive results were found for ground nutmegs and a bay leaf sample. Velasco et al. (183B)recommended blending water slurries of larger samples to give more precise aflatoxin analyses. Zinc acetate/AlCls solution was found to give a better cleanup from interferences by precipitation of cottonseed product extracts in a paper by McKinney (106B).Leistner (98B)purified aflatoxins B1, B 2 , GI, and Gz with a thin layer on an aluminum sheet employing a multiple solvent-multiple direction procedure. Several columns were examined for effectiveness of aflatoxin separation in the high pressure liquid chromatographic
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work of Seitz (156B).Garner (50B)reported HPLC separation of aflatoxins B1, B2, GI, and G2 within 10 min with 0.3% methanol in wet dichloromethane eluent. Pons (130B) achieved the same separation with a wet CHCl3/cyclohexane/CH&N solvent system. Aflatoxins B1 and B2 were differentiated from G1 and G2 by NaBH4 reduction before TLC separation where the former gave one fluorescent derivative spot and the latter two, as reported by Ashoor et al. (3B). Przybylski (134B)confirmed aflatoxins B1 and G1 by forming derivatives with (F),CCOOH before TLC. A collaborative study by Stack et al. (165B)showed the method to be valid for peanut butter. T h e adsorptive tendencies of chyrysotile asbestos in some filter paper types was studied with respect to aflatoxin B1 by Postel e t al. (131B). T h e identification of compounds formed by ammonia treatment of aflatoxin B1 was accomplished by mass spectroscopy after fractional sublimation in a paper by Stanley et al. (166B). Romer (141B)made use of silica gel mini-columns to screen and concentrate aflatoxins before further analysis of positive samples. The results of a collaborative effort to test such a procedure were published by Romer et al. (142B). Collaborative tests results for a modified official AOAC method for aflatoxins in cottonseed products were reported by Pons (129B) and showed a faster analysis with equal precision. Rhein wines were examined for aflatoxins by Drawert et al. (22B) but their TLC procedure showed none. Lafont et al. (96B) found interferences with the same TLC-Rf values as aflatoxin B1 when they examined apricot extracts. Shannon e t al. (159B)applied a green coffee method with slight modifications to analyze for aflatoxin B1 in roasted corn. A single development was found sufficient to separate aflatoxins from corn lipids in an extract when Trucksess (176B) used the proper silica gel and solvent TLC system. Velasco (182B) described the use of adapted filter fluorimeters to measure the intensity of bands on mini-columns used for aflatoxin screening. An extraction-partition method before TLC analysis for aflatoxin M1 in milk was published by Fonseca et al. (38B). Stubblefield et al. (168B)conducted a collaborative study on a TLC/confirmatory method for aflatoxin M1 in dairy products and found interferences from blue cheese. Sensitivity to the part per trillion range was claimed by Tuinstra e t al. (178B) in a procedure for M1 in milk that involved both column and two-dimensional TLC. Trifluoroacetic acid derivatization was found useful for a confirmatory test for aflatoxin MI by Trucksess (177B).Wilson et al. (194B) showed an expanded screening method applicable to aflatoxin, ochratoxin, zearalenone, penicillic acid, and citrinin. Penicillic acid was determined by electron capture gas chromatography of its trifluoroacetate derivative in a procedure by Thorpe e t al. ( 173B).Trimethylsilyl derivatives were also found amenable to such a measurement technique in the method of Suzuki et al. ( I 70B) where both patulin and penicillic acid were measured. Patterson et d. (125B)improved a method for aflatoxin M1 in milk by preventing emulsions with dialysis before their extraction with a chloroform shake. Suzaki et al. (169B)used flame ionization detection in a patulin/penicillic acid method applied to grains. Fujimoto et al. (46B)removed interferences to the EC-GLC measurement of penicillic acid and patulin TMS derivatives by preliminary TLC of grain extracts. Eyrich (30B) sprayed his TLC plates with 3-methylbenzothiazolone-2-hydrazone-HC1 before fluorescence measurement of patulin in his examination of apple juice. Rosen et al. (144B) used single ion mass monitoring as their GLC detector when analyzing apple juice for patulin as a T M S derivative. Reiss (136B) used saturated a-dianisidine/HAc or 1%methanolic N-methylbenzothiazolin-2-onevisualization reagents in a TLC patulin method. Meyer (109B) measured patulin fluorescence on a TLC plate after treatment with u-phenylenediarnine/propanol/HzS04. This author (108B)also fluorimetrically detected patulin on plates with chlorotolidine and chloroanisidine reagents. Ware et al. (188B)separated patulin in apple juice by HPLC and confirmed it by GC of the acetate derivative. Ware (187B)reported 5-hydroxymethyl-2-furaldehyde as the main interference in an HPLC method for patulin in apple butter. Rapid screening for aflatoxins and zearalenone (Fz toxin) in corn was found possible with a standard AOAC methanolwater extraction system by Thomas et al. (172B),cleaning up pigments with cupric carbonate after hexane partition. Sarudi 196R
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et al. (152B) extracted Fa from corn with ethyl acetate after an initial fat extraction and made separations by TLC for fluorimetric or spectrophotometric measurements of spot eluent. Fritz et al. (44B)gave their TLC procedure for determining ochratoxin A in foods and showed better precision for instrumental spot measurement on plates. Levi et al. (101B) modified an AOAC TLC method to separate ochratoxin A from green coffee interferences in applying it to those samples. A collaborative study by Levi (IOOB)detailed recoveries and was satisfactory. Silica gel mini-columns were found useful by Hald et al. (63B)for screening for ochratoxin A in barley. Hult (72B)quantitatively measured this toxin by reduction of the fluorescence a t 380 nm after a carboxypeptidase cleavage. Reiss (137B)estimated sterigmatocystin by viewing the fluorescent TLC spot through a variable grey filter to gauge its intensity. Mass spectrometry as a means of measuring sterigmatocystin was reviewed by Koller et al. (91B). T h e application of enzymatic epoxide reaction of trichothecene mycotoxins with excess glutathione and difference measurement was proposed by Foster et al. (40B).Interferences with a GLC method for T-2 toxin from Fusarium were identified by Mirocha e t al. (112B) as monoglycerides and were removed by prior TLC separation or else resolved by GLC as derivatives other than T M S ones. Naoi e t al. (115B) determined T-2 toxin and diacetoxyscirpenol in wheat powder by two-dimensional TLC after extraction, partition, and column cleanup. Saxitoxin from shellfish was analyzed by fluorescence after alkaline H202 oxidation in the procedure of Bates et al. (4B).Rubratoxin B was ethyl acetate extracted and determined by TLC a t relatively high levels in corn without a cleanup by Hayes et al. (67B).Recovery of staphylococcal enterotoxin from foods was effected by Genigeorgis et al. (54B) who made use of affinity chromatography on sep harose. Efforts toward refining techniques for the measurement of nitrosamines have continued a t a lively pace since the dilemma of food preservation vs. artifact is still present. Crosby et al. (18B)extensively reviewed the properties and determination of them. Foreman e t al. (39B) also reviewed their formation and analysis. Sen et al. (158B) dealt with the separation and analysis of volatile nitrosamines in their review. Walters e t al. (186B) described a chemical determination of nonvolatile nitrosamines in which the dried food matrix is reacted with thionyl chloride, yielding nitrosyl chloride which is gas-purged off and trapped and analyzed as nitrite. A cleanup on a n alumina column aided the specificity of the TLC method used by Walker et al. (184B).Heisler et al. (69B) analyzed spinach that had been stored poorly but found no nitrosamines by GC-MS. Skaare et al. (164B)subjected vacuum distillates from fish to GLC analysis with N detection and alsoseparate MS confirmation. Stephany et al. (167B)avoided false positive results with polar and nonpolar glass capillary columns in a GC-MS method for meat. Fine et al. (37B)described the GC separation of some nitroso compounds including sensitive detection by their “thermal energy” analyzer. Fine et al. (36B)also applied their GLC detection device to the analysis of food vacuum distillates, showing extremely low detection limits after concentration. Some high molecular weight nitrosamines were extracted from flour and determined by GLC in the work of Kelly et al. (88B).Kawabata (86B)showed details of a single-crystal-KBr nitrogen selective detector that we used for nitrosamine GLC. Experiments to separate conformers of substituted asymmetric nitrosamines were performed by Iwaoka e t al. (78B) with LC and TLC. Oettinger et al. (120B) described a device for detecting nitrosamines in HPLC effluents by the “thermal analyzer” principle of NO2 emission but found it less sensitive than the GC detector version. Further HPLC nitrosamine applications using this detection mode were published by Fine et al. (35B). A cleanup scheme by Iwaoka et al. (77B) involved repetitive solvent partition before liquid or gas chromatography of nitrosamines. Gough et al. (58B)made use of a two-column series GC-MS system employing valves to vent solvent before the SCOT column and also to bypass it for longer-retained nitrosamines. N-Nitrosoamino acids were methylated with diazomethane before alkali-flame ionization GC in the procedure for foods reported by Ishibashi et al. (76B).Eisenbrand e t al. (26B) formed the trimethylsilyl ethers of nitrosoamino acids before GLC separation with multiple ion MS detection. Crathorne et al. (17B) used “isomeric” compounds of the same
molecular weight as known nitrosamines to fine-tune their MS detector. Goodhead e t al. (57B) found that GC-MS only confirmed half of possible nitrosamines indicated by a Coulson conductivity system. Chang et al. (14B)explored the analysis of nitrosodimethylamine with differential pulse polarography. The chromatographic analysis of residual hormone contaminants in foods was reviewed by Ryan (150B)who covered many types. Ryan et al. (149B)determined melengestrol acetate at ppb levels in beef with a gas chromatographic method. Stilboestrol was measured fluorimetrically after extraction from beef liver and partition by Ponder (128B).Day e t al. (19B),in their chromatographic method, confirmed the stilboestrol dichloroacetyl derivative with coupled GC-MS. Jain e t al. (80B) formed T M S ethers to analyze for diethylstilboestrol by GC in feed supplements. Hoellerer et al. (71B) used GC of T M S derivatives to detect abnormal levels of estrogens in calf and chicken liver. Sephadex gel chromatography aided Hauser et al. (66B)in fractionating extracts before TLC or GLC analysis of meat and liver extracts. De Brabender et al. (20B)detected tracts of tapazole and thiouracil antithyroid residues with their method using TLC after an ionexchange separation. Thiouracils were detected down to 1 ppb by HPLC in the technique of Wildanger (190B). Antibiotics in meat tissue were subjected to electrophoretic separation and detected with test organisms by Schmidhofer e t al. (154B).Sulfonamide bacteriostats were determined in milk using agar diffusion and zone inhibition in Gedek’s (51B) method. Hamann et al. (64B)employed the inhibition of lactic acid produced in yogurt cultures to show the presence of antibiotics in milk. Hamann et al. (65B)liquid-liquid extracted chloramphenicol from milk before identifying it by TLC and GC of the T M S derivative. Bacillus subtilis bioassays were indicators of antibiotic residues in meat for Rieve et al. (139B) who recommended that the penicillinase test of Tolle and Roth’s procedure all be done. Tetracycline traces in foods were estimated with a visual TLC scheme by Ryan et al. (148B).A TLC method for oxytetracycline residues in poultry was published by Rutczynska-Skonieczna (147B).This same author (146B) determined nitrofurazone in milk with TLC. Michielli et al. (11OB) could measure nicarbazin in chicken meat by differential pulse polarography after a simple extraction. Frahm et al. (41B) hydrolyzed nifursol extracted from turkey before florisil cleanup and EG-GLC measurement. Furylfuramide in various foods was reacted with heptafluorobutyric acid before electron capture GC in the paper of Nose et al. (119B). Chloramine T in dairy products was hydrolyzed and oxidized before ultimate measurement as benzoic acid in a GC procedure by van Gils et al. (180B). Corley et al. (15B) measured 1-(4 chlorophenyl)-3-(2,6-difluorobenzo 1) urea in milk with HPLC after EtAc extraction and hexanehH&’N lipid removal. Sulfathiazole in honey was separated by TLC and visualized with dimethylaminobenzaldehyde in the method of Grandi (59B). The amount of fuel oil contamination in shellfish was estimated by a GLC profile comparison of an oil to an extract in Morgan’s (113B) method. Paradis e t al. (125B) tried to differentiate diesel oil contamination of lobster from natural hydrocarbons with their GC method. Drawert et al. (23B) investigated hydrocarbons found in smoked ham with GC-MS schemes and concluded that they are from smoke, not fat. Potthast (132B) extracted polycyclic aromatic hydrocarbons found in smoked meat on a column after mixing with celite. This procedure was further elaborated by Potthast et al. (133B).O’Hara et al. (121B) rechromatographed benzo[alpyrene by HPLC after a n initial cleanup and TLC separation to determine it in smoke condensates. Hirokado et al. (70B) described a method for this compound involving partition, alumina column chromatography, and spectrofluorimetry. McGinnis et al. (105B)examined yeast grown on hydrocarbons for polynuclear aromatic hydrocarbons using TLC separation. Archibald et al. (2B) analyzed yeast by paper chromatography for these compounds. Siegfried (162%) compared GC and TLC/fluorimetry methods for benzo[a] pyrene in plant tissue. Kedzierski (87B)used UV absorbance measurements a t 383 nm after column chromatography in his method applied to cereals. A procedure by Grimmer et al. (60B)made use of Sephadex cleanup before GLC to separate polycyclics in foods. Trotter et al. ( 175B) investigated erratic recoveries of PCB when chlorinated with antimony penta-
chloride and found it due to the impurity S b C14Br. Shirai et al. (IOOB)detected polychlorinated terphenyls in food wrapping material with a TLC procedure. Fehringer (32B) used EC-GC for PBBs in feeds. Polybrominated biphenyl residues extracted from feed and dairy products were confirmed by GC peak disappearance after UV irradiation in the work of Erney (28B). Fukuhara e t al. (47B) had to employ saponification and alumina column cleanup of seafood extracts in their GLC method and showed further sensitivity improvement with MS detection of 2,3,7,8-tetrachlorodibenzo-p-dioxin. Gee et al. (52B) analyzed for chloroanisoles and chlorophenols in chickens by EC-GC after ethylation of extracts. DDT interference with PCB analysis was removed when Trotter ( I 74B) saponified and oxidized clean extracts. Tanaka et al. (171B)steam distilled biphenyl from citrus fruits and removed codistilled citrus oil on a n alumina column before colorimetric analysis. Wozniak e t al. (196B) steam distilled into cyclohexane and measured biphenyl in citrus samples in GLC. Dibenzylbenzene heat transfer oils were detected in fats using TLC/fluorescence in the method of Seitz (163B).Imai et al. (75B)separated Dowtherm A by first steam distilling an oil before a flame ionization GC measurement. Modified terphenyl heat transfer compounds were isolated from oils as unsaponifiables and measured by IR in Marcus’ ( 103B) procedure. Isopropanol residues in de-waxed fruits were measured by Calhoun et al. (11B)with a GC headspace technique. Acetone and isopropanol in oilseed meal were swept directly off solid samples in a hot GC inlet in the method of Dupuy et al. (24B). Methylene chloride, ethylene dichloride, and trichloethylene residues in spices were vacuum distilled off before EC-GC in a procedure by Page et al. (123B).Mascini e t al. (104B)tried a chloride selective electrode as sensor for chlorinated solvent residues from coffee after combusting the vapors. A headspace over a propanol-hop extract solution gave Neumann et al. ( I 17B) a good comparison to a distillation method for MeC12. Gether et al. (55B)measured residual tetrachloroethylene in defatted meat meal with EC-GC of a hexane extract. Sidhu et al. (161B) established residues of 1’2-dibromethane in grains by titration as Br- after distillation and NaOH reaction. Ethyl bromoacetate and trichloronitromethane in wine were solvent extracted by Revuelta et al. (138B)and measured by EC-GLC. Kroeller (92B) read the color given by extracted s-butylamine at 368 nm after reaction with 4-fluoro-m-xylene in a method for oranges. Ethyl carbamate in wine was extracted, reacted with trifluoroacetic anhydride, and measured by a conductivity GC detector in the scheme of Walker et al. (185B).Inorganic bromide residues in grain were converted to bromoethanol by ethylene oxide before a GLC measurement in a method (111B)based on a procedure of Heuser and Scudamore. Bound formaldehyde was distilled in a two-stage procedure given by Van Dooren (179B).Karasz et al. (83B) measured formaldehyde in maple syrup by adding acetylacetone color reagent directly. An indicating picrate-paper enabled Karkocha (84B) to estimate HCN in almonds. Polyvinylpyrollidone traces were adsorbed on a column, dyed with Vital red, and eluted for colorimetry in Frauenfelder’s (43B) work. Scopoletin from wooden barrels was found in aged liquors by TLC in a paper by Otsuka et al. (122B).Pfeilsticker et al. (127B)reported artifact phenomena when they applied the method of Heuser and Scudamore to determine ethylene chlorhydrin residues. Pfeilsticker et al. (126B) used direct extract injection for a GC measurement of ethylene-chlorohydrin, -oxide, and -glycol in grain. Epoxides in hop extracts were reacted with HBr for analysis and also examined by TLC in an investigation by Knorr (89B).Methylmercury residues in swordfish were irradiated with neutrons and separated on silica gel columns by de Jong et al. (21B).Schafer et al. (153B) estimated methylmercuric residues in fish by EC-GLC after extraction as the cysteine complex. Boric acid was detected by Franco et al. (42B)in caviar by an emission method studied collaboractively for the AOAC. Methods of analyzing for migration of materials from plastics into food were reviewed by Kupfer (93B).Koch et al. (90B) described the use of a model system to simulate fat migration into lastics. Figge e t al. (34B) further described the use of the ( l C) HB 307 fat simulant to measure plasticizer migration. Phthalate ester plasticizers were determined in fish and shellfish by EC-GLC using second column confirmation in the publication of Giam et al. (56B).Figge (33B) reported
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an improved technique for the radioactive measurements needed in working with the (14C)HB-307 fat simulant system. Meranger (107B) screened for di-n-octyltin stabilizer migration into alcoholic beverages with a graphite furnace AAS method. Williams examined the aforementioned sample type and also oils and vinegars by direct injection or headspace GLC to detect vinylchloride monomer migration. Ernst et al. (29B)advocated using a Hall conductivity detector to analyze xylene extracts for VCM residues in food by GLC. Breder et al. ( 9 B ) gave their GC method for VCM traces in various sample types. Gabany e t al. (49B) also studied migration of VCM in a series of model systems using a sealed jar apparatus. Rosen et al. (145B) monitored m/e 62 and 64 in a GC-MS headspace method for VCM in food. Williams (191B) also reported a sensitive GC-MS headspace method. This author (192B) also brominated VCM residues and determined the l-chloro-1,2-dibromethane by EC-GLC. A method for 4-methylimidazole in caramel was improved by Carnevale (12B)who determined it as an acetyl derivative against a GC internal standard. Fuchs et al. (45B) also chromatographed the acetyl derivative and confirmed i t on alternate GC columns, TLC, and MS. An ultraviolet absorption method for 0-toluene sulfonamide impurity in saccharin was described by Jacin (79B) who also used GLC of the T M S derivative. Nelson (116B)investigated an HPLC separation of OTS in saccharin using ion exchange. Hydrazoic acid was measured in food by conversion to ethyl azide by diethyl sulfate and then gas chromatographed with a thermionic detector in a paper by Anania et al. (1B).Guanine in cereals was acid extracted, cleaned up, and separated by TLC in Legat’s (97B) method. Ion-exchange liquid chromatography provided the means for Cox et al. (16B) to rapidly measure uric acid in animal feeds. The selective adsorptive behavior of chrysotile asbestos toward bromocresol purple enabled Rose (143B) to detect 0.5% in talc. An additional cleanup step for isolating “light filth” from fruit paste was studied by Kvenberg et al. (95B).Kvenberg (94B)also reported a procedure applicable t o breading. T h e talc content of rice was estimated by Grunwaldt et al. (61B) by washing and then determining the Mg proportion of the mineral residue. Brickey et al. (IOB) recommended changing from HzOz to NaOCl bleaching in a light filth method for cocoa, chocolate, and press cake. The objective measurement of degradation or decomposition of foods has always been difficult since subjective correlations are necessary. A GC headspace technique was proposed by Kaminski et al. (82B)to detect grain degradation by mold attack based on volatile metabolites. Juffs (81B) tried to correlate starch gel electrophoresis with milk proteolysis but found high bacterial counts prerequisite for this. Hurrell e t al. (73B)investigated three dye-binding methods to indicate heat damage to proteins. Wood et al. (I95B)analyzed for ipomeamarone in damaged sweet potatoes with gas chromatographic measurement of the TLC spots appearing positive. The discoloration of dried cabbage was correlated to a dehydro-ascorbic acid-glycine ethyl ester condensation product in the work of Ranganna (135B). Murthy et al. (114B) used a lesser pink color from coconut treated with HC1 to indicate relative rancidity. Liuzzo et al. (102%) tested a total reducing reaction with KMn04 as a means to estimate oyster quality. A reaction product of B H T in heated oil was identified by Leventhal et al. (99B) as 3,3’,5,5’-tetra-bis(tert-butyl)stilbenequinone using multiple TLC. A taint in boar meat was isolated from the unsaponifiables and identified as 5 a-androst-16-en-3-one by Kaufmann et al. (85B). Furda e t al. (48B) identified the main decomposition product of the sweetener L-aspartyl-L-phenylalanineas 6-benzyl-3-carboxymethyl-piperazine-2,5-dione. CARBOHYDRATES Simplification and improved specificity continue to be important in the analytical techniques for carbohydrates. An automated glucose-oxidase-peroxidase procedure for glucose has been evaluated by Romano (69C) and a n improved procedure described using o -dianisidine for color development. Enzyme reaction kinetics have been used by Klitzing (42C) to determine glucose in 15 s by its reaction with ATP and then NAPH in the presence of hexokinase and glucose-6-phosphate dehydrogenase. A similar enzyme system, followed by fluorometric assay has been applied to ultra-micro quantities of glucose by Tomisek et al. (79C).Accuracy of sugar determi198R
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nations by the anthrone method have found by CerningBeroard (15C) to depend upon the sugar used as standard. Optimum conditions for the determination of glucose by periodate titration have been determined by Dusic et al. (21‘2). Enzyme and reduction methods for D-glucose and D-fructose in sugar beet and factory juices have been compared by Kubadinow (46C),who reported higher results by the reduction method. Soxhlet extraction with 80%alcohol or hot water has been used by Della Monica e t al. (19C)to remove sugars from potatoes and fruits; the extracts are analyzed by a two-step procedure for glucose, fructose, and sucrose. Dusic (2OC) has published procedures for the determination of arabinose, xylose, and ribose by periodate oxidation. A colorimetric procedure usin the reaction of lactose with methylamine has been suggestecfby Nickerson et al. (58C)as a means of estimating lactose in the presence of its hydrolytic products. An enzymic method for the determination of (l-14C) lactose and (l-14C) glucose has been described by Davies et al. (I8C)using enzymes to convert the sugars into (14C)carbon dioxide. An automatic analyzer which measures redox systems by differential potentiometry has been applied by Bosset et al. (I I C ) to the determination of lactose with cerium(1V) solution, but cerium(1V) proved to be too strong an oxidant for the determination of lactose in milk. A thin-layer chromatographic method has been described by Lee et al. (48C)for the determination of sugars and the semi-quantitative determination of lactose in a variety of foods. Crystalline lactose in whey powders has been estimated by Anderson et al. (2C) by taking the difference between total moisture by Karl Fischer and free moisture by vacuum drying a t 65 OC. Sugars in sweetened condensed milk products have been determined by Birch et al. (9C)using both colorimetric and polarimetric measurement. A specific micro-assay of D-arabinose and L-fucose has been proposed by Yamanaka (84C)using D-arabinose dehydrogenase. An automated method for total reducing sugars in wort and beer after hydrolysis has been described by Moll e t al. (532) using the copper neocuproine complex for determination of the hydrolyzed sugars. Conditions for silylation of sugars have been discussed by Zuercher e t al. (87C, 88C) and optimum conditions established. The preparation of sugaroxime silyl derivatives for the gas chromatographic analysis of sugars has been discussed by Zuercher et al. (89C, 9OC). Vapour-programmed thin-layer chromatography has been described by de Zeeuw et al. (86C) who used a new spotting device and densitometric measurement. A procedure for the preparation of trimethylsilyl ethers of kestose isomers in aqueous solution has been proposed by Nurok (SOC),and the same author has discussed the separation of these isomers by gas chromatography (59C).Conditions for preparing test solutions of the sugars in foods have been described by Iwata et al. (37C) for analysis by gas chromatography after trimethylsilation. The use of butaneboronic esters in the gas-liquid chromatography of some monosaccharides has been discussed by Wood et al. (83C).Differential determination of hexoses and pentoses has been achieved by Usov et al. ( S I C ) using o-toluidine reagent and reading a t two wavelengths. High pressure liquid chromatography has been applied by Rapp et al. (67C)to the determination of simple sugars, glycerol, and ethanol in wine. Fermentable material has been determined by Petersen (64C) using dry yeast and measurement of the volume of carbon dioxide produced. A rapid determination of reducing matter in sugar beet has been suggested by Scholze (74C) which uses colorimetry after reaction with 3,5-dinitrosalicylic acid. Liquid chromatography of saccharides, including simple sugars and starch hydrolysis products, has been described by Linden et al. (49C).Thermometric titrimetry has been proposed by Bark et al. (7C) for the determination of carbohydrates which can be analyzed by the Malaprade method. Sucrose has been determined in cane juice and molasses by Bruijn et al. (14C) and in sugar beets by Malec et al. (50C) using isotope dilution methods. An automated method for measuring added sucrose in cereal products has been described by Finley e t al. (24‘2) which uses an immobilized invertase column as an integral part of the automatic analysis set up. Thin-layer chromatography and the thiobarbituric acid reaction have been used by Tanaka et al. (77C)to determine sucrose, raffinose, and stachyose in legume seeds. Small amounts of hexoses and sucrose have been determined by
Rozovskii et al. (70C)using osmium(VII1) as oxidant and diperiodatocuprate t o measure the reduced osmium. A review of the state-of-the-art of thin-layer chromatography of carbohydrates has been published by Ghebregzabher et al. (27C). A thin-layer chromatographic method for the identification of mono-, di-, and trisaccharides has been applied by Hansen (29C)to 28 sugars resulting from carbohydrate hydrolysis. Partition chromatography on anion-exchange resins has been used by Havlicek et al. ( 3 I C )for the separation and characterization of sugars in wort and beer. Mono- and disaccharides have been analyzed by Lawrence (47C) by high performance liquid chromatography on ionexchange resins. By altering the eluent mixture of wateracetonitrile, Palmer (61C) has obtained a versatile system for liquid chromatography for various sugars. Chromatography a t -10 “C has been used by Ramnas e t al. (66C)for the separation of sugars into anomers. A colorimetric method for neutral and acidic carbohydrates has been suggested by Patil et al. (62C) which uses ethanolic thymol and ferric chloride in concentrated hydrochloric acid for color development. Silylated derivatives of disaccharides have been analyzed by Adam et al. ( I C )by gas chromatography on open-tubular glass columns. Ion-exchange chromatography of the borate complexes of saccharides has been described by Walborg et al. (82C)using an automated system. Oligosaccharides in starch hydrolysates have been identified by Hansen (28C)by thin-layer chromatography on Silica gel 60. Havlicek et al. (30C)have used partition chromatography on ion-exchange resins for the separation of oligosaccharides. An automated column chromatographic separation of alinked glucose oligosaccharides has been developed by Torii et al. (80C). Gas chromatography has been proposed by Morrison (56C)for the determination of the degree of polymerization of oligo- and polysaccharides after conversion of the reducing end to alditol and hydrolysis of the polymer. Columns for high pressure liquid chromatography of carbohydrates have been described by Belue et al. ( 8 C ) for use on polysaccharides and low molecular weight carbohydrates. The use of sodium borohydride has been suggested by McCready et al. (54C)for the elimination of reducing groups before and after colorimetric analysis with phenolsulfuric acid for the analysis of mixtures of mono- and disaccharides with oligosaccharides. Maltosaccharides have been examined by Kainuma e t al. (39C) using gel chromatography. The analysis of xylooligosaccharides up to the tetraose has been proposed by Kamiyama et al. (40C)by gas chromatography of the alditols followed by preparation of the trifluoroacetyl derivatives. Rapid analysis of carbohydrates in food has been suggested by Conrad et al. (17C) by means of high pressure liquid chromatography. Liquid chromatography has also been used by Brobst et al. (13C)for the analysis of carbohydrate mixtures up to ten glucose units. Optimal conditions for the acid hydrolysis of wheat pentosans have been discussed by Jelaca (38C) and the soluble sugars obtained identified by ion-exchange chromatography. An improved version of the method for the determination of starch by iodine spectrophotometry has been developed by Nedelcheva et al. (57C). The accuracy of the hydrogen iodide method for the degree of substitution of hydroxyethylated starch has been shown by Boxall et al. (12C) to depend on the efficiency of the traps. Bolling et al. (IOC)have shown that the determined amylose content of milled rice and wheat is affected by the solvent used to extract lipids from the grain. A double wavelength method for the determination of amylose as its iodine complex has been proposed by Sanyal et al. ( 7 I C ) which is linear up to 0.4 mg amylose in 10 mL. Amylopectin has also been determined by Sanyal (72C) using a similar technique. A critical comparison of determinations of amylose by colorimetry and potentiometry has been reported by Banks et al. (6C) and good correlation obtained. Hydroxypropyl groups in cellulose ethers have been determined by Schwarz ( 7 3 2 ) by reaction with ninhydrin after acid hydrolysis. Food stabilizers have been determined in food products by Chang et al. (16C) using zonal electrophoresis in borate or malonate buffers. A review of methods for the detection of thickness stabilizers and gums in foods has been published by Endean (22C). A simple semi-quantitative method for polysaccharide additives in protein rich foods has been described by Klostermeyer e t al. (44C)which uses precipitation of the gum with an appropriate reagent after enzyme hydrolysis of
the protein. A special preparation for this analysis in fresh cheeses has also been described by Klostermeyer et al. (43C). Aliginates and pectins in foods have been determined by Martelli et al. ( 5 I C ) using thin-layer chromatography. A modification of the ASTM method for determining the degree of substitution of carboxymethylcellulose has been proposed by Zadow (85C) which improves end-point detection. The use of turbidity measurements has been suggested by Matulewicz et al. (52C) for the determination of the precipitation curves of carrageenans. Galacturonic acid in wine and fruit juices has been determined by Arndt et al. (4C)using thin-layer chromatography, and by Sarris et al. (73C) using an automatic determination of the hydroxymethylfurfural produced after reaction with mineral acids and applied to the study of pectins. An enzymic method for the determination of dextran in sugar has been developed by Richards e t al. (68C)using dextranase and dialysis. A method for @-glucanin barley has been described by Fleming et al. (26C)requiring a differential assay of glucose by glucose oxidase and a-glucan by treatment with exo-1,4-a-glucosidase. Infrared spectroscopy has been used by Filippov et al. (23C) for the determination of the degree of esterification of pectin. The problems in the analysis of potatoes for pectin have been discussed by Keijbets et al. ( 4 I C ) and interferences with various methods described. Tomato pectic substance has been examined by Stein e t al. (76C) using gel filtration and disk gel electrophoresis. Uronic acids have been determined by Perschak (63C)by extraction, anion-exchange cleanup, and reaction with Tollens reagent. Saponins in foodstuffs have been determined by Andrzejewska (3C) by extraction and thin-layer chromatography. A method for total potato glycoalkaloids has been described by Fitzpatrick et al. (25C) using extraction, hydrolysis, and nonaqueous titration of the aglycones; and the potato glycoalkaloids have been separated by Herb et al. (33C)by the use of gas chromatography after permethylation. Sorbitol has been determined by Artaud e t al. (5C) by gas chromatography of its trimethylsilyl ether, and by Rabinowitz e t al. (65‘2) as cyclic butaneboronate. An automated method for available carbohydrate in food has been described by Hudson et al. (35C) using p-hydroxybenzoic acid hydrazide as the color reagent for carbohydrates. Several methods for determination of available carbohydrate in carbohydrate-reduced foods have been investigated by Korsrud et al. (45C) and hydrolysis with 0.1 N HCl plus Rhozyme S and ferricyanide titration for reducing sugar was found most satisfactory. Methods for “fiber” in vegetable material have been compared by McConnell et al. (53C) and the gravimetric methods of Southgate, Van Soest, and Edwards gave similar results. New filtration equipment for the determination of crude fiber has been described by Holst et al. (34C)which eliminates the need for asbestos. An enzymic method for the determination of dietary fiber has been proposed by Hellendoorn e t al. (32C) which uses pepsin and pancreatin digestion to remove digestible material. A Report of the Proceedings of the International Commission for Uniform Methods of Sugar Analysis has been published (36C). Applications of gas chromatography to carbohydrates by Dutton and applications of enzymic methods to the structural analysis of polysaccharides by Marshall are articles included in Volume 30 of the “Advances in Carbohydrate Chemistry and Biochemistry Series” edited by Tipson (78C).
COLOR Both natural and artificial colors in foods have been examined by both new and old analytical techniques. A review of Shrikhande ( 4 3 0 ) discussed anthocyanins in foods, including analytical methods for their determination. Polyamide chromatography has been described by Strack et al. ( 4 6 0 )as a method for anthocyanins in foods which improves separation and detection of the colors. Anthocyanin pigments in sour cherries have been identified by Shrikhande et al. ( 4 4 0 )using paper chromatography, and in figs by Puech et al. ( 3 9 0 )using a similar technique. A study of grape anthocyanins in a carbonated beverage has been described by Palamidis et al. ( 3 4 0 ) showing the stability during storage. Anthocyanins in grape skin extract have been examined by Manley et al. ( 2 8 0 )using high pressure liquid chromatography, and in Concord grapes ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
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by Hrazdina ( 2 2 0 ) using column chromatography on polyamide. A procedure for the determination of betanin in foods has been described by Lehmann et al. ( 2 7 0 ) using polyamide microcolumns. The analytical methods for carotenes in palm oil have been reviewed by Mueller-Mulot (330) and the method of the Deutsche Gesellschaft fuer Fettwissenshaft is included. Chromatography on cellulose has been described by Farre Rovira ( 17 0 ) for carotenoids in flour and semolina, and the effect of bleaching agents identified. Coloring compounds in tomatoes have been studied by Zhuchenko et al. ( 5 7 0 )who determined @-caroteneand lycopene, by Kimura et al. ( 2 5 0 ) who recommend butylated hydroxytoluene addition to prevent oxidation of carotenoids during thin-layer chromatography, and by Watada et al. ( 5 3 0 )who measured chlorophyll and carotenoids using a light absprbance technique. Chlorophylls of olive oils have been characterized by Dujardin et al. ( 1 4 0 )using fluorometry and thin-layer chromatography. Citrus flavonoids have been separated on Sephadex LH-20 by Tomas et al. ( 5 2 0 ) ,and asparagus flavonols and flavones have been identified by Woeldecke et al. ( 5 5 0 ) . The specificity of the vanillin test for flavanols has been questioned by Sarkar et al. ( 4 2 0 )who describe the possibility of false positive interpretations and suggest improvements. A fluorescence method for rutin in fruits has been described by Panov et al. ( 3 5 0 )using two-dimensional paper chromatography and fluorescence detection. Fluorescence methods have also been proposed by Chelkowski et al. ( 9 0 ) for the determination of flavines in raw material. Tannins in tea have been measured by Kapel et aI. (230)using cerium(1V) sulfate, and in musts and wines by Montedoro et al. ( 3 2 0 )using selective precipitation with methylcellulose. Separation by means of Sephadex columns and photometric evaluation of the pigments has been described by Takeo ( 4 7 0 )as a means of judging the quality of black tea infusions. Maillard browning reaction products have been determined by Wolfrom et al. ( 5 6 0 ) by gas-liquid chromatography after trimethylsilation. Separation of synthetic dyestuffs in liquors, wines, and beverages have been described by Tewari e t al. using paper chromatography ( 4 9 0 ) , thin-layer chromatography ( 5 0 0 ) , and paper electrophoresis ( 5 1 0 ) .Twelve water-soluble food colors have been separated and determined by Terashita et al. (480)using agar column chromatography. Ascending paper chromatography has been used by Rizvi ( 4 0 0 )for the determination of artificial dyes in tomato ketchups. Dyes and intermediates have been analyzed by Passarelli (360)using high pressure liquid chromatography which cuts analysis times. Massart et al. ( 3 1 0 ) have described the application of numerical-taxonomy techniques to the choice of optimal sets of solvents in thin-layer chromatography for 26 food dyes. The separation of synthetic water-soluble dyes has been achieved by Kenmochi et al. ( 2 4 0 )using column chromatography on aminoethyl cellulose-Celite. A means of eliminating background absorption at two wavelengths has been suggested by Honkawa ( 2 1 0 ) by the use of a function generator which balances the signal contribution a t the two wavelengths and has been applied to the analysis of dye mixtures. A thin-layer chromatographic method for water soluble food dyes has been described by De Clercq et al. ( 1 1 0 ) using elution from silica gel G with copper sulfate solutions in alcohol. Amberlite LA-2 methods of extraction of colors from foods have been updated by Graichen ( 1 9 0 )and submitted for collaborative analysis; some further revisions were found necessary and another collaborative study is planned. The effects of various solvents in the separation of four dyes permitted in the EEC have been tabulated by Pearson ( 3 7 0 )for use in paper and thin-layer chromatography. Oil soluble colors have been separated and determined in foods by Banerjee et al. ( 6 0 )by alumina column chromatography. Organic dyes have been separated by Andrzejewska ( 2 0 ) from natural pigments using purification on polyamide columns and thin-layer chromatography. A colorimetric method for annatto in whey has been described by Hammond et al. ( 2 0 0 )using colorimetry after ammoniaethanol extraction. A rapid method for erythrosine in canned red fruits has been suggested by Adams et al. ( 1 0 )using colorimetry after decolorization of the natural anthocyanins with sodium sulfite. Leuco bases have been measured by Dantzman e t al. ( 1 0 0 )in aqueous solutions of dyes by bubbling oxygen through the solution in the presence of cupric chloride and 200R
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dimethylformamide followed by colorimetry. Uncombined intermediates have been determined by Singh ( 4 5 0 )in FD&C Blue No. 2 by high pressure liquid chromatography. FD&C Red No. 2 and FD&C Red No. 40 have been observed by Ross ( 4 1 0 ) to be thermally degraded by aqueous D-fructose and D-glucose a t elevated temperatures. The interference of erythrosine (FD&C Red No. 3) with the determination of FD&C Red Nos. 2, 4, and 40 has been noted by Draper ( 1 3 0 ) and precautions are detailed to reduce the interference. A study has been made by Powell et al. ( 3 8 0 ) on the polarographic behavior of Fast red E and a possible method for similar dyes in foodstuffs suggested. Thin-layer chromatography has been used by Bell ( 8 0 ) to determine subsidiary dyes in D&C Red No. 19 and D&C Red No. 37. Ion exchange on Cellex D has been described by Fratz ( 1 8 0 ) for the determination of 44’(diazoamino)bis(5-methoxy-2-methylbenzenesulfonic acid) in FD&C Red No. 40 and Bailey et al. ( 5 0 ) have used high pressure chromatography for the same determination. A method for the analysis of FD&C Yellow 5 and its intermediates which uses reversed-phase liquid chromatography has been described by Wittmer ( 5 4 0 ) .Procedures for the determination of 4,4’-diazoaminodi(benzenesulfonicacid) in FD&C Yellow No. 6 have been described by Marmion ( 3 0 0 )using gradient elution chromatography and by Bailey e t al. ( 4 0 ) using elution chromatography and high pressure liquid chromatography. Higher and lower sulfonated dyes in FD&C Yellow No. 6 have been analyzed by Bell ( 7 0 )using thin-layer chromatography and a spectrodensitometer. Bailey et al. ( 3 0 ) have published a spectral compilation of dyes, intermediates, and other reaction products related to FD&C Yellow No. 6. A method for the determination of unsulfonated primary aromatic derivatives in water soluble food dyes and food additives has been proposed by Dixon et al. ( 1 2 0 )using thin-layer chromatography, column chromatography, and spectrophotometry. Studies on the purity of sulfanilic acid, an intermediate in food dye manufacture, have been published by Marmion ( 2 9 0 ) .The use of color measurement as a Quality Control tool for foods has been discussed by Kramer ( 2 6 0 ) .The comparison of color scales for dark colored beverages and the development of new scales for these products has been described by Eagerman et al. (150, 1 6 0 ) . ENZYMES Analytical techniques employed in the analysis of enzymes in foods range from the use of more specific substrates to automated and semi-automated procedures. Enzymatic activities in malt flours have been evaluated by Bruemmer ( 3 E ) using five synthetic substrates. Quantitative analysis of the enzyme complement of commercial rennets has been described by O’Leary et al. (21E)using column chromatography and measurement of the milk-clotting activity of the fractions, and DeKoning (9E)has described a system to identify rennets of unknown composition using isoelectric focusing. Ascorbate activity in wheat has been determined by Kahnt et al. (16E) in wheat varieties by incubating extracts with reduced glutathione and ascorbic acid. Phadebas tablets have been used by Barnes et al. ( I E ) to determine a-amylase in wheat, and by Sigenthaler (28E)to determine this enzyme in honey. The same substrate has been used by Regula et al. (%E) for the determination of a-amylase in foods. Jeffers et al. (13E)have determined that gibberellic acid increases the amylase activity of wheat using three different official methods to measure the amylase activity. The Amylochrome kit method has been found by Edwards (1OE) to provide a rapid method for the determination of diastase in honey. A suggestion for the improvement of the measurement of the diastatic activity of flour has been made by Johnson et al. (15E)which substitutes colorimetric measurement of the maltose for the titration method. A semi-automated method for the determination of catalase in wheat has been proposed by Kruger (20E).Wheat esterases have been separated and characterized by Cubadda et al. (6E) using gel electrofocusing. Park et al. (22E)have described a modified hydroxamic acid method for the estimation of lipase, and Castberg e t al. ( 4 E ) propose the use of tributyrate as a substrate for the determination of this enzyme in milk. A pH-static method for pectinesterase determination in sweet ’ cherries has been described by Schmid (27E),and a method using direct gas chromatographic measurement of methanol
has been used by Krop et al. (19E) to follow pectinesterase activity in citrus juices. Peroxidase activity in fruits and vegetables has been measured by Kiseleva (18E) using o-phenylenediamine as substrate. Polarographic measurement of phosphatase activity has been described by Davidek et al. ( 7 E )using the reaction with 2-naphthol esters, and applied to the analysis of milk and milk products (8E).Alkaline phosphatase in milk has been analyzed by Schiemann et al. (26E)using an organic buffer. Proteolytic activity in wheat has been measured by Preston (23E)using fluorescamine in an automated system for measuring the cleavage products. Hide-Powder-Azure has been used by John et al. ( 1 4 3 ) as a substrate for determining proteolytic activity in barley malt. Rheology tests for the evaluation of proteolytic activities have been described by Colas ( 5 E ) and Berger et al. ( 2 E ) .A simple assay method for superoxide dismutase has been proposed by Elstner et al. (12E) using the inhibition of the formation of NOz- by the enzyme. The results and problems encountered in measuring trypsin inhibitor activity of flour have been discussed by Rackis et al. (24E).A semi-automated method for the determination of trypsin inhibitors in textured soya proteins has been described by Egberg et al. ( I I E ) ,and the use of isoelectric focusing for the measurement of protease inhibitors in potatoes has been suggested by Kaisar et al. (17E).
FATS, OILS AND FATTY ACIDS A review is given on the determination of fats, oils, and waxes (19F)which deals with qualitative tests, determination of major components, determination of acidimetric, oximetric, and enometric values, as well as the determination of physical properties (with 333 references), and a review is also given of chromatographic techniques (83F)(both GC and TLC) used for the determination of absolute and relative configurations of branched and long chain fatty acids. An evaluation has been made (79F)of eight extraction methods and their effects upon t,he total fat and gas chromatographic fatty-acid compositional analyses of food products, and Farnell(20F) describes an infrared method for the simultaneous determination of fat and moisture in meat products by use of a multiple attenuated total reflectance cell after extraction with trichloroethylenemethanol (27:23), taking measurements at three wavelen ths and using the values obtained to calculate moisture an fat contents by means of calibration graphs. A ring-oven method is provided by Weisz (96F)for the determination of oils, fats, and waxes wherein the sample solution in benzene is applied to the center of a filter paper and is benzene-washed into the ring zone, with the light transmission of the ring then compared against a standard solution of paraffin wax for quantitation, and Morrison et al. (53F) describe methods used for the selective extraction of nonstarch and starch lipids from wheat flour and the analysis and characterization of these fractions by TLC and GC procedures. Use is made of HPLC to measure the glycerides, fatty acids, and sterols of lipids from soya and soya-bean foods (42F) in conjunction with a moving wire flame ionization detector (limits of detection ranging from 0.1 to 1.4 Kg), and Dutton (17F)makes use of infrared ATR spectrophotometry to measure trans-isomerization directly on liquid fats and oils and recommends the method for continuously monitoring trans-isomer development during hydrogenation. The GLC analyses of 200 samples of commercial fats and oils have been compared to the standard ranges specified by the Food and Agricultural Organization/ World Health Organization Codex Alimentarius Committee on Fats and Oils (84F) and only six samples fell notably outside the ranges, and Folstar e t al. (23F) have studied the analysis of oil from green coffee beans, finding that the extraction yield depends on particle size and extraction time and that only oil obtained from completely extracted beans was representative of the original coffee oil (as ascertained by fatty acid composition and amount of unsaponifiable matter). Conway and Adams (14F) find that the A.O.A.C. acid hydrolysis method 14.019 gives high results for foods containing more than 15% of sucrose or fructose and recommend incubation of such samples with a bakers' yeast extract for 4 h at 40 "C prior to the acid hydrolysis step, and Randall (71F) describes equipment and procedures for a rapid method for measuring total fat which provides for the immersion of dried samples in boiling solvent prior to final extraction out of the solvent, reporting that good agreement is obtained vs. con-
f
ventional Goldfisch and Soxhlet techniques. Pettinati et al. (67F)have made an in-depth comparison of the Foss-let fat analyzer technique with the A.O.A.C. method for meat and meat products (the study included some 67 samples of various meat and meat products containing from 1.1-95.4% fat) and find the methods to be statistically equivalent, and Doeden (16F) has evaluated the Mettler automatic dropping point apparatus and has compared dropping point data for a series of oil samples with Wiley melting point data, finding a linear correlation and recommending the automated method as being more reproducible and less time consuming as well as having the advantage of automatic end-point detection in monitoring hydrogenation studies and for quality control use. A rapid method applicable to the routine determination of oil in lecithins and similar phospholipid samples was developed (78F) wherein advantage is taken of the ability of a deactivated (wet) silica gel column to adsorb up to 1g of phospholipids while permitting the quantitative elution of the oil part of the sample with ether, and Karleskind et al. (37F)describe a rapid NMR method for determining the oil content of grains after first drying the sample in a microwave oven under carefully controlled conditions. A fully automated, pulsed NMR procedure is given for measurement of the solid fat content of fats and oils (88F), and the relations between pulsed NMR, wide-line NMR, and dilatometry have been studied (89F) and recommendations made for converting NMR values into dilations and vice versa. Wurziger (98F) reports on the composition of coffee oils in raw and roasted coffee beans from the arabica and robusta varieties and suggests color reactions which permit the detection of robusta coffee in mixtures with arabica coffee, Iverson (32F) describes a GC method for measuring milk fat in cacao butter extracted from milk chocolate, and a procedure is provided for determining the lard content of commercial mixtures of goose dripping with lard (92F)by a TLC separation of the fats into their constituent triglycerides, GC of the saturated glyceride zones, and then comparison of the C52 to fatty acid ratios (about 1:3 for goose dripping and 6:l for lard) against a Calibration graph. The measurement of lard in goose dripping has also been accomplished (9F) by GC analysis of the ratio of stearic acid to oleic acid with the authors reporting that this technique permits the measurement of down to about 10% lard. Unsaturated carbonyl compounds originating from autoxidized fats were identified (36F) by forming their 2,4DNPH derivatives, hydrogenating the aliphatic double bonds by use of palladium on CaC03 as catalyst, and then separating on a TLC Kiselguhr G plate impregnated with Carbowax 750 to determine the chain length of the unsaturated carbonyl compounds and the number of double bonds. Freeman (25F) provides a TLC-densitometry technique for monitoring the progress of oxidation in frying oils by measuring the increase in oxidized glycerides, and Grosch (27F)reviews the changes that take place during the autoxidation of unsaturated fatty acids at relatively low temperature (25 "C), as well as the production of compounds responsible for aroma and the analytical detection of spoilage of fats. Selke et al. (77F)make use of GC-MS analysis for volatile oxidation products formed by heating tristearin in air, Schouten (76F) recommends a preparative TLC method for the quality control of frying oils where the zones for oxidized acids are eluted and weighed, and Sims and Fioriti (82F)describe GC and TLC procedures for analyzing and identifying the N-substituted amides formed when fatty esters are heated a t temperatures above 150 "C with a-amino acids. Work is reported (91F)which is directed at determining the polymers and oxidation products of heated vegetable oils as nonelution materials from a gas chromatographic column, and a method employing this principle (90F) has been subjected to collaborative study. Leu and Andersson (49F)describe a GC procedure for determining the TMS derivatives of methyl hydroxystearate isomers which result from the decomposition of the peroxides that are formed by the oxidation of linoleic acid by lipoxygenase, and Pearson (64F) provides a modified procedure for the determination of the thiobarbitaric acid value which can be applied to a common chloroform extract of fats and oils, comparing results obtained with those obtained for free fatty acids and peroxide values. A method is given (85F)for determining the positions of olefinic linkages of fatty acids, based on conversion of mono- and polyunsaturated fatty acid methyl esters into their correANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
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sponding epoxides by reaction with 3-chloroperoxybenzoic acid and then treating with HI04 solution in ether and separating the resulting aldehydes by TLC, and automated apparatus is described (28F, 1OOF) for determining the induction time of edible oils by a modification of the Swift test. Purr (70F)provides a quick visual colorimetric test for determining fatty peroxides in olives using the dye developer 3 (Merck), and Jirousova (34F)tells of a modified method for estimating the anisidine value of oxidized fats. Investigations on the oxidative rancidity of hazelnut kernels are reported by Barthel et al. (7F) who provide column and thin-layer chromatographic methods for determining the carbonyls isolated from rancid nuts, and a procedure is given (47F)for the isolation and preparation of the free fat of milk powder for the determination of oxidative changes. An apparatus is described (95F) for measuring the amount of oxygen absorbed during vegetable oil oxidation with equations provided which correlate the peroxide indexes with changes in density, and Hassel (29F) makes use of thermal analysis techniques to evaluate the relative oxidative stabilities of vegetable oils, correlating results obtained with the predicted stabilities by the active oxygen method. A procedure (24F)is proposed for monitoring the polymeric fatty acids in rapeseed oil by the isolation and TLC separation of the methyl esters of fatty acids that do not form adducts with urea, and GC analyses have been performed (44F) which compare the changes in composition of fats transferred to rubber and plastics in migration tests using sunflower oil. Weihrauch et al. (94F)describe methods used for the isolation and characterization of oxofatty acids by transmethylation, preparation of 2,4-DNPH derivatives, separation into saturated and unsaturated compounds by argentation chromatography, and final analysis by various chromatographic techniques including GC-MS. A TLC method is reported for determining saponins in selected food products ( 3 F ) ,and a quantitative technique is given (18F) for the column chromatographic separation of lactones from butter and margarine (employing a column with three layers of packing) prior to analysis of the separated lactones by GC. Schaap et al. (73F) make use of a spectrophotometric measurement of the carotene in butterfat to obtain a reliable determination of the solid/liquid ratio which they report to be in good agreement with NMR data, and a quick single stage method is given (66F)for the production of fatty acid methyl esters for chromatographic analysis which is recommended as useful for monitoring the course of hydrogenation or transesterification of edible oils. Peers (65F)provides a nonaqueous microtitration method for determining acidity in oils and fats, titrating samples in toluene with 0.02 N tetrabutylammonium hydroxide to a bromothymol blue end point while argon or nitrogen is bubbled through the solution, Ohlson et al. (59F)describe a coulometric titration method for determining iodine values, and NMR is used for estimation of average molecular weight and the iodine value of marine oils containing wax esters (39F)by means of correlating equations. The physicochemical constants of fats and oils are determined (46F)by use of GC fatty acid compositional data in conjunction with a constructed alignment chart (thus enabling the estimation of the saponification number, the refractive index, neutralization value, specific gravity, heat of combustion, iodine-saponification number (see also 45F), and the hardness number. Van Dijck et al. (87F)have analyzed the unsaponifiable and glyceride composition of oils from Corylus seed oil by TLC and GC methods, and GC methods have also been used to analyze the unsaponifiable matter from cashew nut lipids (5127) and the unsaponifiable matter from crude and processed coconut oil (54F) after fluorisil column separation. Ziegenhorn (99F) has developed a n improved enzymatic method for determining serum triglycerides wherein the triglycerides are hydrolyzed with a mixture of lipase and esterase and the released glycerol is measured by kinetic fixed-time analysis, with use of glycerol kinase, pyruvate kinase, and lactate dehydrogenase, and Utrilla et al. (86F)use a combination of TLC and GC to analyze the trisaturated triglycerides of fats, using TLC to effect the separation of the triglycerides from other fat components prior to GC analysis with methyl heptadecanoate as a standard. Thin-layer metallochromatography of lipids (30F)is used for the analysis of triglycerides (incorporating various transition metal salts into microcrys202R
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talline cellulose as adsorbent) and a method is presented ( 1 I F ) for the quantitative TLC analysis of triglyceride groups differing in unsaturation, based on densitometry of charred bands separated on argentation plates with results given for a standard mixture as well as for a number of edible oils. Kundu et al. (48F) describe the analysis of the mono- and digalactolipids of beans, peas, and soybeans by first separating the galactolipids by TLC or paper chromatography and then determining the fatty acid composition by GC, and Armengol et al. (4F) provide MS, IR, and NMR data for determining glyceryl mono-, di-, and tristearates as well as methods for their chromatographic separation from commercial food emulsions. A TLC method is described (62F)for the detection of acetodiacylglycerols in milk lipids, using Kieselgel G plates and hexane-ethyl acetate (22:3) as the solvent, and Myher and Kuksis (58F) recommend the use of a cyanoalkylphenylsiloxane stationary phase (Silar 5CP) for obtaining improved resolution of homologous monoacyl- and monoalkylglycerols (derived from edible oils) by GC analysis and also apply this technique to the end of obtaining resolution of natural diacylglycerols as well (57F).The Silar-SCP stationary phase has also been used to coat open tubular columns for the GC analysis of docosenoic (22:l) fatty acids of marine and rapeseed oils ( I F )and for the determination of cis-trans isomerism in some polyenoic CISfatty acids along with comparative data in this latter case for butanediol succinate, and Apiezon L columns for identification purposes (2F).A GC method for determining docosenoic acids in fats and oils has been provided (138’) which makes use of a DEGS column and methyl tetracosanoate as an internal standard, is capable of determining down to 0.4% of the docosenoic acids in rapeseed and marine oils, and has been subjected to a collaborative study (12F). Deeth provides a convenient extraction-titration technique (158’) for determining the lipolysis in milk and cream, using a 40: 10:1 mixture of isopropanol-petroleum ether-4 N H2S04and then titrating the acid layer with KOH in methanol, and GC-MS methods are applied ( 2 I F ) to determining isomeric a-branched chain fatty acid methyl esters. The composition of the fatty acids in coffee oil and coffee wax has been analyzed and characterized by gas chromatography (22F)after fluorosil column fractionation; changes in the fatty acid composition of lipid fractions from potatoes during storage were analyzed (26F) by TLC separation followed by GC analysis of the methyl esters of the total lipid, lecithin, and cephalin fractions, and methods are provided by Kimura e t al. (41F) for the microdetermination of fatty acids by GC (10-100 wg). A TLC method is given ( 5 F ) for the separation of methyl esters of polyunsaturated fatty acids by argentation TLC, using dichlorofluorescein spray and UV radiation to locate reference bands and then removing the appropriate zones and identifying individual esters by GC analysis. An isotopic dilution method is given by Kiuru et al. (43F)for the determination of geometrical isomers of octadeca-9,12-dienoic acid in food fats in conjunction with argentation TLC, including a technique for preparing the radioactive isomers by use of 14C tagged diazomethane, and Keen et al. (40F) use ion-exchange resins to isolate the acetic, propionic, and butyric acids of cheese for GC analysis. Capella et al. (10F) provide an argentation TLC method for determining saturated fatty acids from edible fats and oils, and use is made of the silver oxide-organic halide reaction for the esterification of steam volatile fatty acids prior to their analysis by GC (35F). Sheppard and Iverson @OF)review the available esterification methods for fatty acids to be analyzed by GC and recommend methods for the esterification of fatty acids of high and of low molecular weights, and analytical separations em loying HPLC are described by Scholfield (75F),using a Clshorasil column and aqueous acetonitrile, by which polymerized and oxidized esters (not detectable by GC! analysis) can be measured. Murata has employed (5527)a chemical ionization-mass spectrometry method for the analysis of free fatty acids in edible oils, Jaeger et al. (33F)make use of a n automated GC procedure for determining fatty acid methyl esters (including cis and trans isomers) on a glass capillary column coated with FFAP, and the determination of the free fatty acids in wort and beer (50F)and of long chain fatty acids in beer (72F)has also been accomplished by GC methods. Schmid (74F) has determined the phosphatides of cocoa products by extracting ground cocoa products with ethanol, isolating the phosphatide complex, ashing with magnesium
acetate solution to “fix” the phosphorous and then photometrically determining the phosphorous. TLC methods are given for the determination of the phospholipid content of white flour ( 8 F )and of rapeseed and sunflower seed oils (31F), and Shustanova (81F) describes a colorimetric procedure used in conjunction with a standard curve for estimating the ester groups in phospholipids. TLC and GC methods are provided for the determination of the sterol fraction of olive oil (6F),and a Fluorisil column chromatographic technique is described (38F) for the fractional determination of soya-bean sterols which are divided into four fractions (fatty acid esters of sterols, free sterols, and acylated and nonacylated glucosides). Patterson et al. (63F) describe a scheme for the separation of 17 steroids in the scallop by column chromatography on a hydroxyalkoxypropyl derivative of Sephadex LH-20 and on Anasil B, in combination with TLC and GC techniques; chemical ionization MS is applied (56F)to analysis of sterol esters, and Melchert (52F) uses lipophilic gel chromatography for the isolation of sterols and squalene from the unsaponifiable fraction of fats prior to GC analysis. A rapid, modified technique is described (93F) for the extraction of yolk cholesterol (providing improved recoveries), and Wortberg (97F) reports that cholesteroloxidase from Nocardia erythropolis is not specific for cholesterol but also reacts with all the natural 3-~-hydroxysterols, thus contributing a new method of characterizing the “total sterols” in the unsaponifiables of fats. The Liebermann-Burchard reaction has been applied to the unsaponifiables of milk lipids to determine the cholesterol in milk products (61F), and Okabe et al. (608’)describe a micromethod for colorimetrically determining cholesterol, cholesterol esters, and phospholipids after first performing a TLC separation. A GC analysis for total cholesterol was developed by Punwar (68F) for use in multicomponent foods and was collaboratively studied under the aegis of the A.O.A.C. (69F).
FLAVORS AND VOLATILE COMPOUNDS Maga (50G) provides an extensive review of lactones in foods which summarizes isolation and identification techniques as well as occurrences, sensory properties, formation pathways, and synthesis techniques, and a summary is also given (81G ) of infrared identification of compounds separated by gas and thin-layer chromatography with specific applications to flavor analysis. A computerized arrangement is described by Merritt et al. (57G)which is used for acquiring and processing data from several GC-MS analytical systems with special emphasis given to data encoding and procedures for the identification of volatile components. Nanjo and Guilbault (65G)describe the amperometric determination of alcohols, aldehydes, and carboxylic acids using an immobilized alcohol oxidase enzyme electrode and providing activity data for a number of compounds, and an ion-exchange method (72G) is provided for the detection of aliphatic and aromatic aldehydes based on the formation of cyanohydrins and the hydrolysis of these (catalyzed by cation-exchange resin) to carboxylic acids and ammonium ion which is retained by the resin and detected by use of Nessler reagent. A simple, direct, GC monitoring method is described (2412) for the quantitative determination of residual hexane in extracted vegetable oils by packing a sample of oil directly onto glass wool into the inlet liner of a gas chromatograph, inserting this into the heated instrument inlet, and then determining the hexane by temperature programming on a Poropak P column (sensitive to 1 ppm hexane). Deki et al. (18G) make use of GC-MS to identify the 2,4-dinitrophenylhydrazonesof volatile carbonyl compounds using a column packed with 3% OV-101 and then temperature programming, and the authors note that these compounds do not decompose during gas chromatography. The identification of unsaturated 2,4-DNPH compounds derived from carbonyls originating from autoxidized fats has been accomplished (14G)by partial hydrogenation (using P d on CaC03 as catalyst) and then analyzing the reaction mixture on kieselguhr TLC plates impregnated with Carbowax to determine the chain length as well as the number of double bonds, and Casteele et al. (IOG) provide gas chromatographic techniques for T M S derivatives of naturally occurring nonvolatile phenolic compounds and related substances of the type found in natural flavors and plant extracts, reporting that these compounds are stable through analysis. A gas chroma-
tographic method is suggested for the isolation of thiols from food products (43G) by forming the (sic) stable alkylmercaptobenzoate derivatives and then separating these on an SE-30 column. Matheson (55G) describes a modified methylene blue colorimetric method for the determination of hydrogen sulfide in the 0.04 to 0.4 ymol range, detailing a unit for the entrainment and trapping of the same, and use is made of an air-gap, SO2 selective electrode to measure the hydrogen sulfite content in wines (342).Brenner and Khan (5G) provide a simultaneous fluorimetric micromethod for determining HZS and volatile thiols in beer by flushing them with nitrogen into a trapping solution and then titrating them fluorimetrically with a standard solution of tetraacetoxymercurifluorescein. A TLC method is given for determining Methyl S-methionine sulfonium salt (49G)in cacao which is a precursor of dimethyl sulfide. Zehner et al. (9%’) describe a technique for maximizing the flame photometric detector response for determining sulfur compounds by adding a constant sulfur background to the carrier gas, pointing out that the signal is proportional to the square of sulfur in the flame and, by taking advantage of this fact, one can achieve an approximate increase of one order of magnitude in sensitivity. A paper chromatographic procedure for determining capsaicin is described as a micromethod applicable to both low and high pungency samples (33G) and a TLC method was applied by Andre et al. (4G)to measuring the capsaicin content of ground Hungarian paprika. Capsaicin has also been determined in capsicum spices and their oleoresins after extracting with acetone and separating interferences on an alumina column and then performing a gas chromato raphic analysis using piperine as an internal standard ( 1 9 8 ) . The quantitative microanalysis of capsaicin, dihydrocapsaicin, and nordihydrocapsaicin in the fruits of Capsicum annuum by mass fragmentography (using cholestane as an internal standard) is reported by Lee et al. (46G) and De Cleyn and Verzele (13G) provide a high pressure liquid chromatographic method for the separation and quantitative analysis of piperine and its isomers as a measure of the pungent principle of pepper and pepper extracts. A TLC method is given (3G)for the determinatoon of gingerol and shogaol in ginger oleoresin under unsaturated conditions which is suitable for routine analysis, and quantitative determination of the pungent principle in ginger is also achieved by a TLC method described by Nambudiri et al. (64G)who provide spray techniques for developing gingerol and zingerone spots after separation on silica gel plates. Masada et al. (53G) make use of GC-MS methods to determine gingerol and gingediacetate in ginger oil and a GC method is given (IOOG) for the evaluation of cinnamon by steam distilling the essential oils in an apparatus (99G) specially designed to prevent losses of volatiles prior to GC analysis. The rapid detection and determination of maltol and ethylmaltol in foods and beverages is described by Zappavigna et al. (97G)who make use of TLC of chloroform extracts on Kieselgel GF264 plates using isoamyl alcoholconcentrated aqueous ammonia (2:l) as the developing solvent and detect the spots by UV radiation and by spraying with aqueous ferric chloride. Schlack and Dicecco (74G)report on the determination of vanillin and ethylvanillin in ice cream and beverages by GLC, and Soliman et al. describe their work (84G)in analyzing aroma concentrates from roasted sesame seeds by GC-MS. A gas chromatographic method for determining benzaldehyde in marzipan is given (25G) where the benzaldehyde is steam distilled, camphor is added as an internal standard, and the separation is achieved on a UCON LB-550X column, and Hefendehl et al. (36G) describe a method for analyzing peppermint oils by GLC on XE-60 (1% on chromosorb AW-DMCS) which permits the detection of as little as 5% of oil from Brazilian Mentha aruensis in oil from American Mentha piperita. A simple solid injection technique is provided for the analysis of essential oils by GLC with results given for root, bark, and leaf samples of cinnamon (SOC),and Tatum et al. describe a TLC method for estimating the limonin content of citrus juices which is suggested as a quality control test for citrus products (87G).The alcohols in the volatile aroma of citrus juice and peels have been determined (71G)by GC of their benzoyl derivatives (formed by benzoyl chloride and pyridine treatment) and the volatile carbonyl compounds from citrus products were determined by GC of their 2,4ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
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DNPH derivatives (70G).Moshonas et al. (61G) provide two simple methods (bromate titration and gas chromatography of selected components) for evaluating aqueous citrus essences, and Gostecnic and Zlatkis have made a computer analysis of gas chromatographic profiles vs. organoleptic evaluations for quality assessments of cold-pressed orange oils (32G). HPLC has been applied to the determination of limonin in grapefruit juice (26G) after first extracting into chloroform and using chloroform and acetonitrile (19:l) as the eluant on a porous silica (10 pm) column, and HPLC has also been used for the resolution and quantitation of naringin and naringenin rutinoside in filtered grapefruit juice (27G)using a micro C-18 column and eluting with H20-MeCN (80:20). The GC-MS differentiation of aroma substances from various species of strawberries is given (86G),and Parliment and Kolor (68G) describe the analysis of the major volatile components of blueberry by GC followed by MS and IR analysis, providing relative concentrations and the organoleptic importance of the identified peaks. The y-lactones of apricot (59G) and peach (58G) have been analyzed by GLC and the GC-MS analysis of volatile components of rose apple (47G)and cloudberries (37G)is also described. A simple fluorimetric procedure is given by Casimir e t al. (9G) for the determination of methyl anthranilate in Concord grape juice by distilling into a p H 7 buffer and directly measuring the fluorescence, and separation techniques and spectrofluorimetric methods are also given by Merat and Vogel (56G) for determining methyl anthranilate and N-methyl anthranilate in various drinks and aromas. Two methods, one a TLC procedure and the other an incubation technique, have been reported (88G)for determining the lachrymatory factor in onions with both methods based on the color forming reaction of lachrymators with glycineHCOH reagent followed by measure of the color a t 520 mp. Schreyen et al. (79G)have analyzed the volatile flavor compounds of leek by capillary GC-MS, thus characterizing a total of 67 compounds, and a GC method is reported for determining the metaldehyde content of cabbage after extraction with ether (91G).Kemp et al. (41G)report on the analysis of volatile compounds vacuum steam-distilled from cucumber, separating the components by gas chromatography and analyzing them by IR and MS. A GC procedure is reported (2G) for determining geosmin (identified by MS) the earthy smelling component in the neutral fraction of beet aroma and 9-decalol) has also been geosmin (trans-1,lO-dimethyl-transdetermined in dry beans by capillary GC-MS (8G).Freeman et al. (30G) have determined the volatile flavor components of 27 Allium species by GC, TLC, and UV spectrophotometric methods and make use of this data to estimate the S-alk(en)yl-L-cysteine sulfoxides present as flavor precursors, and a rapid spectrometric method for analyzin thiopropanal Soxide in onion is also given (29G).GC-Mg methods are described for analysis of an onion essence (22G)and for analysis of volatile components of cabbage, broccoli, and cauliflower (7G) and dry red beans (6G). A simple accurate titrimetric method is provided by Fleming et al. (28G) for determining COz in cucumber brines by distilling from acidified brine in a sealed jar into an open vial of standardized NaOH standing in the brine, and then titrating the excess base with standard acid. Regression models are provided by Persson and Von Sydow (69G) which correlate gas chromatograph data with sensory data for the evaluation of canned beef, thus providing methods which can be used in product and process work to supplement or refine panel service for routine analyses. The phenolic composition of commercial liquid-smoke preparations and derived bacon has been analyzed by GC-MS methods (44G), and a procedure is described (35G) for analyzing a chicken flavor concentrate wherein fractions separated by GC on a silicon oil on a Chromosorb W column are applied to a small Celite 2,4-DNPH reaction column and the derivatives thus formed are eluted with petroleum ether and analyzed by TLC. Dumont et al. (23G)describe GC-MS methods used to analyze the volatile neutral aroma compounds formed during the cooking of Gruyere cheese and GC-MS techniques are also reported (82G)for determining volatile trace components in Gouda cheese after isolation by low temperature vacuum distillation with H2O-isopentane and separation into polar and nonpolar fractions. Gaba et al. (31G) have developed GC 204R
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and TLC methods for comparing the total carbonyls of fresh and stored desi ghee, and Sloot and Hofman (83G) describe analytical methods for alkylpyrazines in Emmental cheese by GC-MS after vacuum degassing the cheese fat t o isolate the volatiles and separating the isolates into polar and nonpolar fractions. Methods are described for the determination of lactones in blue cheese (40G)and in cheddar cheese (96G) based on their separation on a packed liquid chromatographic column followed by subsequent GC analysis. The analysis of volatile components of roasted cocoa by GC-MS is reported (93G) wherein a novel separation step is used for isolating the aroma by extraction with supercritical COz under pressure followed by atmospheric steam distillation, adsorption on Porapak Q, extraction with ether, and then separation into basic and neutral fractions. Riggin et al. (73G) give an HPLC procedure for determining salsolinol (1methyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline) in cocoa products and Vitzthum e t al. (92G) report on the determination of cycloalkapyrazines in coffee aroma by GC-MS techniques (listing 17 of these as reported for the first time in roasted coffee). The theanine content of tea leaves is determined (48G) by use of a TLC separation followed by colorimetry with ninhydrin (theanine levels were 0.44-0.95% in range from 11 kinds of tea), methyl salicylate has been determined in black tea ( I C ) by gas chromatography after hexane extraction and steam distillation, and the volatile aroma concentrates from Vietnamese tea and lotus tea have been analyzed (66G) by gas chromatography, mass spectrometry, and IR spectrometry. GC-MS techniques are reported (15G-17G) for the identification of the phenolic, neutral, acidic, and basic volatile components of peat-dried malt wherein the fractions are isolated by steam distillation, ether extracted to concentrate them, and are then separated into individual fractions by two-phase extractions at different pH values. The monomeric phenolic compounds by ciders are estimated (95G) by fractionally eluting them from a silica gel column with tertiary butyl alcohol-chloroform mixtures, and monitoring the UV spectra of the eluted fractions, and Wang and Siebert (94G) have determined the level of trans-nonen-2-a1 in beer by HPLC of its 2,4-DNPH derivative. GC methods are given for the determination of benzyl alcohol in stone-fruit brandies (90G),for the determination of anethole in liqueurs (67G)and for the determination of benzaldehyde in wines and amyl acetate in liqueurs ( 5 1 C ) . Stahl et al. (85G) have applied HPLC to the determination of alcohols in various materials including wine using ethyl acetate-propanol-water (121:49:30) as the eluant on a micro crystalline cellulose column, and a n automated procedure is given (60G)for determining alcohol in beer which incorporates a “flash” distillation system where the alcohol is swept into an AutoAnalyzer, treated with HN03-KzCr207 reagent, and the resulting color is measured (with a rate of 30 samples per hour). A GC procedure is provided for measuring methanol in wine (45G)on a Porapak QS column which has a coefficient of variation of 4.4%, and Tress1 and Renner (89G) make use of GC-MS techniques to determine the identity and concentrations of lactones in beer. Jobbagy and Hollo describe a GC head-space method for evaluating the aroma of wines (38G) and have also provided an index number for evaluating wine aroma (39G)by determining the correlation between peak area and organoleptic aroma evaluations. Aroma compounds were extracted from wine by liquid-liquid extraction with pentane-dichloromethane (2:1), concentrated using a Vigreux column, and the nonpolar (75G),thioether (78G),and acidic components (21G) were analyzed using GC-MS techniques. Charalambous et al. ( 1 1 G ) describe HPLC methods for determining the free purines, pyrimidines and mononucleotides in beer and wine samples (using Aminex A6 cation-exchange resin), Martin et al. (52G)provide GC-MS methods for determining the ethyl esters and isoamyl acetate in whiskies and rum (after extraction from salt saturated solutions with pentane), and a n enzymic method is given (54G)for the determination of acetoin in wines by spectrophotometric means. The volatile sulfur compounds of beer aroma were analyzed by Schreier et al. (76G) by GC on a Carbowax 20 M on Chromosorb W AWDMCS (80-100 mesh) column using isopentyl pentyl sulfide as an internal standard with a flame photometric detector, and the same authors describe a similar method (77G) for the volatile sulfur components of beer after first clarifying with
Carrez solution I and I1 prior to extraction and concentration of the volatiles. A GC method is provided by Chen et al. (12G) for the analysis of fusel alcohols in beer and fermenting wort on a 0.3% SP-1000 plus 0.3% H 3 P 0 4on Carbopack A (60-80 mesh) column. GC procedures are also given for the determination of hop bitter compounds which are measured by use of both flame ionization and “reaction radio” (for I4C or 3H labelled compounds) detection systems after chromatography of the T M S derivatives of methanolic hop extracts (20G). Kleber and Hums (42G) make use of low pressure liquid chromatography to monitor the bitter substances from hops, hop extracts, worts, and beers on silica gel columns (recommending this procedure for detecting sudden deviations from normal during beer production), and quantitative procedures are also provided by Mussche for evaluation of beer bitterness (62G) and for measuring the bitter substances in hops (63G).
IDENTITY This section is concerned with data on the analysis of foods as a means of determining the authenticity of samples, and with the problems of analyzing foods mixed with foods. A review on compositional changes occurring in coffee beans during roasting was published by Clifford (19H).A study of changes in amino acids and reducing sugars during coffee roasting was described by Pokorny et al. (57H),and Amorim et al. ( 3 H ) have examined the proteins of green Brazilian coffee by agar-gel electrophoresis. Galactomannan was found to increase with roasting by Ara et al. ( 5 H ) . These authors ( 6 H ) also investigated the behavior of polysaccharide complexes in Robusta-coffee during roasting. Vilar et al. (77H) have analyzed coffee and coffee substitutes for chlorogenic acid and suggest this compound as a means of measuring the coffee content in instant coffees containing substitutes. Peptides in cheeses were determined by Damicz (24H)by molecular filtration on Bio-Gel P4, high-voltage electrophoresis, and paper chromatography. Various types of cheese can then be characterized by the differences in peptide composition. Genuine sheep milk cheeses were distinguished from cow or goat milk cheeses by Corrao et al. (22H)by examination of the fat by ultraviolet spectrophotometry and analysis of the fatty acid esters. Dresselhaus e t al. (32H) have reviewed methods for egg content in alimentary pastes and relationships between egg content and total sterols or cholesterol are indicated. The same authors ( 3 I H )indicate that cholesterol content of eggs for egg content calculation should be changed from 2.90% to 2.55%, and that gas chromatography is the most accurate method for cholesterol determination. Egg content in mayonnaise is estimated by Carballido et al. ( 1 5 H )by the determined percentages of phosphorus, ether extract, and total nitrogen in the product. A sixth report on the comprehensive evaluation of fatty acids in foods has been compiled by Weihrauch et al. (7”) covering cereal products. The infrared spectrum and fatty acid composition of butter have been shown by Valencia Diaz et al. (75H)to provide in combination a method for the detection of adulteration of a butter. Computer programs were written to compare authentic samples of types of commerical fats and oil and applied by Spencer et al. (72H) to the identification of these oils in the crude or refined and bleached states. Fatty acid composition of a variety of margarines has been determined by Nazir et al. (5“. Esters of sesamol and fatty acids are recommended by Guyot et al. (39H)for use as tracers for the labelling of surplus butter. Shea fat has been determined in cocoa butter by Fincke (34H)by the Fitelson reaction after thin-layer chromatography of the unsaponifiables. Corrao e t al. ( 2 1 H )have tabulated and discussed analytical data for Sicilian virgin olive oils. Characterization of lard and beef tallow and their mixtures has been achieved by Bracco et al. (14H)using enzyme hydrolysis and differential calorimetry. Proximate analysis data and amino acid composition of enzymatic fish protein hydrolyzate have been obtained by Yanez e t al. (79H). Polyacrylamide gel electrophoresis has been used by Simal Lozano et al. (69H)to characterize pollack, cod, pout, and hake, and by Alvarez Vega et al. ( 2 H )to identify fish species, but no qualitative differences were found between fresh, frozen, or breaded fish. Disc electrophoresis was applied by Alvarez Vega et al. ( I H ) to aqueous extracts of fish and electrophoretic differences were found not only between
species, but also between varieties of the same species. The total volatile nitrogenlamino nitrogen ratio was found by Cobb et al. (20H)to have a significant negative correlation with the potential shelf-life of brown shrimp, and a significant correlation with total plate counts of acceptable quality brown shrimp and white shrimp. One percent fish oil in vegetable oil was detected by Schwein (64H)using a modified AOAC test for the determination of fish oils and marine oils. A system for multiple automated analyses for orange juice developed by Vandercook et al. (76H) has been used to determine total sugars, reducing sugars, total acidity, total amino acids, and phenolics in 150 samples of orange juice. Adulteration in citrus juices is discussed by Scholey (63H),and the determination of the free amino acid composition is considered to be a satisfactory means of checking authenticity. Analytic data have been compiled by Royo-Iranzo et al. (60H) on the differences in the proportions of the characteristic components of the serum and pulp of the juice from Spanish oranges; solids and liquids were assayed for carotenoids, total nitrogen, ash, and ash components, and the data may be used in detecting adulterated juices. Empirical formulas based on the contents of total free amino acids and total nitrogen were used by Habegger et al. (40H) to calculate the natural fruit juice contents of various orange products. Two methods for evaluating citrus essence were compared by Moshonas et al. (53H)and parellel results obtained by either bromate titration or gas-liquid chromatography. The amino acid composition of bergamot juice has been determined by DiGiacomo et al. (28H).Sugars in a great variety of tropical fruits were determined by Chan et al. (16H-18H). Sugars and nonvolatile acids in Chinese gooseberry fruit were determined by Heatherbell (43H).A study of 22 grape varieties reported by Selvaraj et al. (65H)includes data on sugars, organic acids, amino acids, and invertase activity. Proteins and enzymes of different grape varieties were isolated by Drawert et al. (30H) and then fractionated by disc electrophoresis and isoelectric focusing in polyacrylamide gels. Different grape varieties could be detected. Twenty-three parameters of strawberries have been determined and tabulated by Goodall et al. (38H). Commercial honeys were characterized by Zuercher e t al. (80H)by individual sugar content, enzyme content, water, and acid. Amino acid analyses of honeys and nonhoney sugar products are presented by Davies (26H)and differences found easily detectable; honeys generally have a high proline content. The proteins of honey have been separated by Bergner et al. ( I I H ) by gel chromatography and dialysis, and differences found between floral honey and honey from bees fed on sugar. Different kinds of meat were distinguished by Spell ( 7 I H ) by electrophoresis on polyacrylamide gel containing urea. A rapid method for distinguishing between fresh and thawedfrozen pig’s liver was reported by Hamm et al. (41H)by means of the aspartate aminotransferase band in the electro horetic pattern of the frozen liver. The measurement of the RC content of the creatinine isolated from meat extracts was shown by Sulser (73H)to provide a method for differentiating between natural and synthetic creatinine and, therefore, detecting creatinine added to meat extracts. The methods for the determination of total meat, lean meat, type and quality of meat and additives were reviewed by Pearson (56H).Immunological double-diffusion and rocket electrophoresis techniques were found by Appelqvist et al. ( 4 H ) to yield qualitative and semiquantitative results in the detection of nonmeat protein in sausages. Immunodiffusion techniques have also been used by Hauser et al. (42H)for the determination of nonmeat proteins in heat-treated meats. Milk proteins in meat products are determined by Sinell e t al. (70H) by a n electroimmunodiffusion technique. The method of Montag for the determination of sodium caseinate in cooked meat products has been critically studied by Frittoli e t al. (36H)and found unsuitable. Parameters for soya products in meat blends have been determined by Formo et al. (35H)and the contents of magnesium, manganese, and fiber were found useful in assessing the amount of textured soya flour in beef. Satisfactory results were obtained by Tateo (74H)when the Parson-Lawrie electrophoretic method was applied to the determination of soybean proteins in meat-base products. Stacking acrylamide-gel electrophoresis was used by Lee et al. (47H)to determine the concentration of soya bean protein in meat soya blends to within f2%. Bailey ( 8 H )has examined ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
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trypsin treated extracts from cooked meat products for soya protein by fractionation of positively charged peptides on an automatic cation exchange amino acid analyzer. Sugars in sausages are determined by Mauro (52H)by paper chromatography. Powdered milk added to raw milk was determined by Resmini et al. (59H)by determining the distribution of 45Ca in the supernatant of an ultracentrifuged sample compared with a noncentrifuged sample. A modification of the phosphatase test in which protein is precipitated with copper sulfate-zinc sulfate has been found satisfactory for determining the effectiveness of pasteurization by Serebrennikova et al. (67H).A technique of identifying three or four proteins in mixtures described by Lindqvist et al. (49H)uses computer comparisons of amino acid patterns and was applied to milk and soya proteins. The fruit juice content of milk drinks made with added fruit juice is calculated by Benk et al. (IOH)from characteristic values of mixtures of butter or sour milks with fruit juices. Soft wheat varieties were identified by Autran ( 7 H ) from the electrophoretic patterns of the wheat gliadins. Satterlee et al. (62H) have published data on the chemical characterization of protein concentrates from distiller’s grains. Data on the chemical composition of wheat and triticale flours compiled by Lorenz et al. (51H)includes information on fatty acid, carbonyl, n-hydrocarbon and phenolic acid composition. The official French method ( 4 5 H ) for the determination of the soft wheat content of pasta and semolina uses polyacrylamide gel electrophoresis of the proteins. Electrophoresis has also been used by Resmini (58H) for the detection of soft wheats in macaroni products. The common wheat content in pasta products was determined by Feillet et al. (33H)by slab gel electrophoresis and determining the concentration of the most basic monophenol monooxygenase band. Immunochemical methods have been described by Bracciali et al. (13H) for the determination of soft wheat in semolina and macaroni products. A review of methods for this type of deProteins termination has been published by Silano (68H). from barley, wort, beer, and yeast have been characterized by Drawert et al. (29H)by isoelectric focusing in polyacrylamide gels. Analytical gas chromatographic data on William Bon Chretien pear brandies has been collected by Nosko (55H)and both home prepared and commercial samples were evaluated. Polarimetry is suggested by Dadic (23H) as a useful tool in brewing quality control and in “fingerprinting” beer. Beech et al. ( 9 H ) have reviewed analytical methods for the determination of flavor, quality, and maturity of wines. Thin-layer chromatography was used by Kaimal et al. (46H) to detect mustard-seed, soya-bean, and safflower-seed oils in ground-nut oil. Galvao et al. (37H)have analyzed peanuts and peanut butter for essential mineral elements. A method for distinguishing between naturally occurring and synthetic caffeine is proposed by Lehmann et al. (48H) which uses thin-layer chromatography to detect trace ingredients. Pyrolysis gas chromatography is described by Lloyd et al. (50H) as a method for the differentiation of chewing gum bases, and traditional and modern methods of analyzing chewing gums are discussed by Delaveau et al. (27H). A spot test for Argemone Mexicana seeds in mustard seeds has been proposed by Bose ( l Z H ) ,which tests the seed with concentrated hydrochloric acid and Dragendorff reagent. Thin-layer chromatography was used by Sen et al. (66H)to detect Curcuma zedoaria and C. aromatica in turmeric. A study of the changes in the sugar components of cane during growth and processing has been made by Sayed (61H).Three methods of calculating the protein content of foods have been discussed by Heidelbaugh e t al. (44H). Computer programs of gas chromatographic data have been applied by Davies (25H)to commodity source identification.
INORGANIC Improvements in inorganic constituent analysis are current indicators of new instrumental approaches. A review of Koirtyohann et al. ( 6 1 4 dealt with the use of flame absorption and emission techniques for minerals in foods. Trace elements in milk was the subject of Murthy’s ( 7 7 4 review. Wildanger (112J) covered trace element determination in foods with x-ray spectrometry. A multielement standard material was 206R
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prepared by Anderson e t al. ( I J )by drying a “spiked” gel. McHard et al. ( 7 1 4 reported a nitric acid digestion procedure for trace elements in orange juice. Wet-oxidation efficiencies of perchloric acid mixtures were studied by Martinie e t al. (69J).A mechanised wet-decomposition system requiring 5 min to 3 h was developed by Knapp (60J).Jackson et al. (50J) reported improving a Technicon continuous digestor with better temperature control. Another version of a continuous digestion apparatus was assembled by Egan ( 2 4 4 using metal chelation after digestion. Fricke e t al. (32J) published a multielement emission method based on microwave plasma emission with a heated tantalum strip vaporizor. A routine stepwise neutron activation analysis scheme was detailed by Heine et al. (38J) for milk samples. Plesch ( 8 8 4 used scattered radiation as an internal standard in his x-ray spectrometric measurements of trace elements in foods. An x-ray fluorescence method for Ca, K, C1, S, and P in meat was said to permit analysis of 10 samples for these five elements in one day by Isherwood et al. ( 4 9 4 . Owlya et al. (87J) analyzed margarine for trace elements using neutron activation with high resolution detection and repeated sample counting. A flameless AA method for Fe, Cu, Ni, and Mn in fats and oils was studied by Olejko (84J).Black ( 8 4 compared hi h temperature ashing, direct aspiration in MIBK, and carton rod techniques for trace metal analysis by atomic absorption on soya bean oil. Arsenic analyses after wet and dry ashing procedures were compared by Uthe et al. (108J) with a final arsine/AAS measurement. Elliott et al. (26J) reported an improved trapping tube for the Gutzeit/Ag diethyldithiocarbamate method. Woidich et al. (114J)dry ashed foods with Mg(NO& and then generated arsine with NaBH4 in an atomic absorption method for foods. Woidich et al. (1134 reported replacing pyridine with hexamine in a Gutzeit/Ag diethyldithiocarbamate method. Hydride generation of antimony, arsenic, selenium, and tellurium for atomic fluorescence measurements were reported by Thompson (103J).Hirayama et al. ( 4 1 4 wet ashed fats and coprecipitated As with Fe(OH)3 before reduction and colorimetric determination. A special generator used for arsine production was claimed to be quantitative in a method by Kurokawa et al. (65J).Fiorino et al. (29J) reported sequential generation of hydrides of As, Se, Sb, and Te in their atomic absorption method for foods. Freeman e t al. (30J)employed a graphite furnace method for arsenic, adding Ni2+ to the furnace before drying and atomization. Orvini et al. (86J)combined irradiation, chemical separation, and high resolution counting in their neutron activation analysis for Se, As, Zn, Cd, and Hg. Holak ( 4 3 4 determined As and Se in foods by cathodic stripping voltammetry. The interference of iron in the determination of aluminum by the aluminon method was better eliminated by ascorbic acid than mercaptoacetic according to Jayman et al. ( 5 3 4 . Nakashima et al. ( 7 9 4 reported values of silver in blood and condensed milk with better plasma-torch emission sensitivity in the presence of Bi. Optimum conditions for barium in a UHF plasma emission method were given by Ikebe et al. (48J).Drew (225) published a simplified circumin method for boron in shellfish. Holz ( 4 4 4 described an automated AutoAnalyzer method for calcium and magnesium by colorimetry. Cadmium was determined by atomic absorption after V205 catalyzed wet ashing and ion-exchange separation in the method of Baetz et al. (2J).Noguchi et al. (82J)wet-ashed fats and extracted Na diethyldithiocarbamate complexes of Cd, Cu, Ni, and Mn into MIBK for an AAS measurement. Hinners et al. (40J)compared extraction to total digestion for analysis of cadmium in rice. Dewit et al. ( 2 1 4 investigated ion association with high molecular weight amines after low temperature ashing in their cadmium procedure. The interference of calcium in analyzing for Cd in milk by AAS was reported by Cornel1 (19J).A tantalum ribbon flameless method for Cd in fish digests was published by Blood et al. ( 9 J ) .Neutronand photon-activation analysis procedures were compared for Cd by Jervis et al. (54J).Chelating ion-exchange concentration techniques for trace Cd, Cu, Co, Mn, Ni, and Zn in foods before AAS measurements were described by Baetz et al. (3J).
Jonsson ( 5 5 4 compared differential-pulse stripping voltammetry and AAS for the analysis of Cd and P b in milk. Anodic stripping was used by Mrowetz et al. (76J)for Cu, Pb, and Cd in caseins with the iron determined colorimetrically.
A graphite furnace procedure was used by Maurer (70J) directly on a suspension of cheese to measure copper. Kundu et al. (64J) proposed oxygen-rich atmosphere to decompose oils before nonflame AAS. Jacob et al. (514 extracted Cu and Zn from fats with EDTA before atomic absorption measurement. A thiuram disulfide spectrophotometric method for Cu was modified by Grys (34J) to give better recoveries. Wolf et al. (1154 analyzed sugars for total chromium without loss of the organically bound fraction by low temperature 0 2 plasma ashing before graphite furnace AAS. Berkh et al. ( 6 J )determined Cr polarographically in canned food. Cobalt was determined by flameless graphite AAS after wet digestion and chelate extraction of small samples. Lapitskaya et al. ( 6 6 4 reported a simultaneous polarographic method for Co, Zn, and Mn in fruits. Cobalt in milk was polarographed by Bernatonis et al. (7J) as the dimethylglyoxime complex. The use of a laser atomizer to determine Ag, Bi, Cu, Co, Fe, Mn, Pb, Ni, and Zn in, e.g., plants and liver by atomic absorption was described by Vul'fson et al. (1115).Newton et al. (80J) showed that a W-Re wire loop could be used for flameless AAS for 19 elements. Lead, cadmium, and copper were extracted from food ash as iodides before AAS measurement in the technique of Tsutsumi e t al. (106J).Soluble saccharides and polyols were directly analyzed for P b by anodic stripping from a Hg film on a carbon electrode in the method of Sourek et al. (99J). Slavin et al. (98J) reported 'heavy metal determinations in meats using H N 0 3 digestion and flameless AAS. Lead traces were determined selectively by solid state luminescence in a CaO matrix as observed by Ryan et al. (934. Sugar was analyzed for Pb, Cd, and Zn using flameless AAS after fermentation to reduce matrix interference by Morris et al. (74J). Mack (67J) found standard addition calibration necessary in his method for lead in wine by flameless AAS. Kapur et al. (58J) used a carbon filament to ash and vaporize solutions of soluble coffee and tea for lead analysis. Huffman et al. ( 4 5 4 observed increases of lead in canned evaporated milk after opening and also had to calibrate their direct carbon rod AAS method with internal standards. Holak (42J) employed H N 0 3 predigestion and subsequent NaN03-KN03 fusion to prepare samples for anodic stripping Cu, Cd, Pb, and Zn analysis. Low results for lead in wine during flameless AAS were avoided by Haller et al. (37J) by injecting dilute H3P04 into the graphite tube. Heavy metals in oils and fats were measurable in an arc spectrographic method by Farhan et al. (27J). Collet (185) volatilized Sn as the iodide to prevent interference with lead in his inverse voltammetric method for Pb, Cu, and Cd in foods. Chow et al. (175) added a P b tracer isotope to a tuna fish digest and calculated original P b content after mass spectrometric analysis of lead-207 and lead-208 ratios. Determinations of mercury by nonflame AAS and atomic fluorescence spectrometry were extensively reviewed by Ure (107J). Chilov ( 1 6 4 reviewed trace mercury methods for foods and the environment. Cold-vapor techniques for mercury analysis were reviewed by Helsby (39J).Tanaka et al. ( 1 0 2 4 combusted fish samples in a quartz tube before a cold vapor measurement. Nishi et al. ( 8 1 4 combusted samples in tubes and removed N and S oxides in a carbonate solution while trapping Hg on gold before a heating/cold vapor analysis. Charcoal was used as adsorbant for Hg by Nakamachi et al. (78J) and subsequently liberated as cold vapor a t 500 "C. An argon plasma was used to detect 0.1 ng of Hg in the method of Kaiser et al. (57J). A simplified apparatus and temperature programmed digestion comprised the essential points of Feldman's (28J) procedure for mercury analysis. Nondispersive atomic fluorescence of cold Hg vapor was reported to correlate with AAS and neutron activation analysis for fish analysis according to Caupeil et al. ( 1 3 4 . Raffke et al. (9OJ) gave a field test procedure for Hg in cereals based on color reaction with di-2-naphthylthiocarbazone.Methylmercury extracted from foods with benzene was separated by TLC by Ohyama et al. (835)as the dithizone complex and then measured by AAS. Atomic absorption interferences with manganese were studied by Bradfield (IOJ)but the helpful addition of La3+ could not compensate for H2SO4 from a digestion. An automated catalytic method for Mo in plant material was described by Bradfield et al. (11J) involving its effect on the KI-Hz02 reaction. Potassium in plant ash was determined by back titrating excess tetraphenyl borate reagent amperome-
trically in the method of Siska (97J). Eipeson et al. (25J) compared a differential EDTA titrimetric method and a polarographic one for tin and iron in canned food. Selenium in crops was determined by Shimoishi ( 9 5 4 by electron capture gas chromatography after digestion and formation of a 4nitro-0-phenylenediamine derivative. Stijve et al. (1OOJ)reported another EC GLC technique wherein the 4,5-dichloro-o -phenylenediamine adduct of selenium was formed. The official AOAC fluorimetric method for selenium was modified by Olson et al. (85J)to give more complete digestion and reagent stability. Ihnat et al. (46J) compared flameless carbon cup AAS to fluorimetry for selenium traces in foods. The fluorimetic naphthalene-2,3-diamine method was critically examined by Haddad et al. (36J) and reagent purification recommended. Strontium traces in foods were measured by Ikebe et al. ( 4 7 4 using UHF plasma generated spectra from digested samples. Thallium in food dyes was extracted as the bromide in ether and reacted with methyl violet before measurement a t 580 nm in Kroeller's (62J) procedure. Kroeller (63J) also determined uranium in food dyes in a precipitation-TLC method capable of detecting 0.1 pg. The fluorine content of baby foods was reported on by Chavdarova et al. (14J) who used ashing, fusion, and L a ( N 0 3 ) ~potentiometric titration indicated by a F- electrode. Jacobson et al. (52J) described a collaborative study for Fin vegetation that used a specific ion electrode measurement. Van Den Heede et al. (109J) studied four sample decomposition methods for F- analysis and preferred low temperature oxygen plasma. Kirsten (59J) modified the combustion chamber of a previous apparatus to accommodate larger samples for fluorine analysis. A potentiometric titration of chloride in beer and wort was published by Preen et al. (89J) that used a silver indicator electrode and Hg2S04 reference. Morrissey (755) titrated the salt extracted from butter with AgN03 using silver and calomel electrodes. A collaborative study of potentiometric salt titration in foods was reported by Brammell(12J).Cheng et al. (154 automated chloride and phosphate determinations in sugar and molasses with two colorimetric complexing systems. Iodine, iodide, and organic iodide were determined differentially by EG GLC after conversion to iodoacetone in a method by Grys (355)applied to milk. Van Vliet et al. (11OJ) predigested samples before employing an automated H ~ S O ~ / N ~ A S O ~ / C colori~(SO~)~ metric method for iodine. Joerin (56J)measured total iodine in milk by oxidation, reduction, 1 2 distillation, and tetrabase/chloramine T color formation. Both x-ray fluorescence and iodide electrode methods agreed for iodine in milk, indicating its presence as I- to Crecelius ( 2 0 4 in his work. Iodine-129 was measured a t natural levels by Rook et al. (91J) after combustion, charcoal collection, neutron irradiation, isotope separation, and counting. Total and organic bromide determinations in foods were reviewed by Getzendaner (334. Martin et al. ( 6 8 4 determined Br and Zn in wheat flour by observing x-rays resultant from proton bombardment. Interferences in the Fiske and Subba Row method for inorganic phosphate were eliminated by using sodium dodecyl sulfate to prevent precipitations as described by Dulley (23J). A continuous flow spectrophotometric method for phosphorus reported by Ruzicka et al. (92J) allowed 420 samples to be measured in an hour after manual digestion. Tomberlin et al. (104J)irradiated wheat samples with and without a Cd filter to resolve phosphorus and magnesium from other background in their activation scheme. Phosphorus-32 was counted by liquid scintillation automatically in the method of Fric et al. (31J)by measuring the Cerenkov radiation. Sodium sulfate in water soluble colors was measured in an automated P b ( N 0 3 ) titration ~ method by Bailey et al. ( 4 4 that used a K3Fe(CN)6-K4Fe(CN)6 coated silver electrode vs. a Pt electrode to detect the end point. Shah ( 9 4 4 estimated sulfate in beer by Bas04 turbidity measurement in a Haze Meter. Hydrogen peroxide in noodles was extracted with MeOH and reacted with phenol/4-aminoantipyrine/peroxidasein a colorimetric method by Miyamoto et al. (72J). Tonkaboni (105J) proposed a simplification of the De Clercq/Cannizzaro method for CO2 in beer with a thymolphthalein end-point indicator for the back titration. C02 was determined differentially from organic acids by titration in the method of Szabo et al. (101J) for beer. An automated COz method using dialysis separation and cresol red color reduction was reported for beer by Moll et al. (73J). Six commercial dissolved oxygen analyzers were ANALYTICAL CHEMISTRY, VOL. 49,
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compared with the Jenkinson and Compton Method for beer analysis by Barollier et al. ( 5 4 .
MOISTURE Powley (19K) describes recent developments in instrumentation for measuring moisture in solids and gases, and a general review of moisture methods is given by Mitchell (15K) with specific emphasis on applications for polymeric materials. Results of a collaborative study of seven different methods of measuring water activities of various foodstuffs are reported by Labuza et al. (13K)and Ross (21K)describes equations for estimating the water activity in intermediate moisture foods. Weldring et al. (26K) describe an apparatus for accurately determining the isotherms for water vapor sorption in foods, and Sood and Heldman make use of a vapor pressure manometer (24K) to measure the water activity in nonfat dry milk. Use is made of differential scanning calorimetry by Karmas and Chen ( 9 K ) to provide a rapid quantitative method for the measure of bound water in aqueous systems and Sloan e t al. (23K)provide water sorption isotherms for various humectants used in IM foods. An apparatus is described for measurement of the equilibrium relative humidity of a food sample ( 8 K ) ,and Schneider e t al. make use of modification of the Karl Fischer titration to determine surface moisture on sugar (22K),employing a saturated solution of anhydrous sucrose in methanol as the titration medium. A gravimetric adaptation is provided (IOK)of the filter-paper press method for determining the water binding capacity of cooked fish, and Parizkova (17K) gives a differential IR technique for measuring trace amounts of water in fatty materials by using the stretching OH vibration band at 3700 cm-’ and comparing untreated samples in CC14 against the same solutions dried with Molecular Sieve 3 A. Equations are given by Dulphy et al. ( 4 K )for correcting the apparent oven moisture values of silages from various sources for the significant volatile components which are also lost, and tables are provided by Wagstaffe (25K)from which the total dry extract of wines can be rapidly estimated from the density and ethanol content of the sample, the latter determined by measuring the refractive index. Basker ( 2 K )provides an indirect calculation for estimating the density of sugar solutions a t a particular temperature from its density a t another temperature and the refractive indices of both the solution and the solvent. A permittivity method is described for the rapid determination of water in meat after homogenizing the sample water into dioxane (12K).The cell is described and results are reported to be almost linear up to a 3.5%water solution. The measure of moisture in meat is also quickly accomplished by GLC on a Porapak Q column after first blending with anhydrous methanol and decanting off the clear liquid (20K). Addis et al. ( I K ) describe a rapid refractometric technique for determining moisture in meat after homogenizing vigorously with isopropanol, and Farnell ( 5 K ) describes an IR method for determining moisture in fresh meat and meat products by extraction into a known volume of solvent consisting of trichloroethylene and methanol. A microwave-oven method (18K)for rapidly determining moisture in meat is also described wherein samples are mixed with FeO and NaCl prior to heating for 2.5 min in a domestic-type 1-kW oven. The use of neutron gauging ( 6 K )is applied for the measure of moisture in bulk powdered foods and in canned Army field rations, with a small californium-252 capsule as the source. Zeman et al. (27K) describe a microwave apparatus and method for the determination of small amounts of water in vegetable oils using mixtures of 1part of sample oil to 4 parts of dioxane containing 2% water and also using a similar mixture of anhydrous sunflower oil as a reference. An apparatus and procedure is given by Kay et al. ( I I K )for the measurement of the water content of milk powders by time-domain spectroscopy wherein the pulse height obtained is dependent on the dielectric properties of the sample (which are in turn usually governed by the water content) and pulsed NMR water methods are reported (7K)for skim milk powders (using a free induction decay mode) and for cottage cheese (using a spin echo technique). Mansfield (14K)determines the water content of foods containing liquid fat or oil using NMR by exchanging hydrogen for deuterium in the HzO, leaving the H signals associated with the fat unchanged. Wide line NMR is used by Mousseri et al. (16K) for determining the bound 208R
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water capacities of corn starch and its derivatives, and Basler et al. ( 3 K )describe methods for using NMR for elucidating the state of water (free or bound) in starch gels.
ORGANIC ACIDS Formic acid was esterified in juices and beverages with ethanol, then distilled into hydroxylamine.HC1 and later measured a t 520 nm after conversion to iron hydroxamate in the procedure of Tanner (28L).Kroeller et al. (9L)used TLC to separate and estimate levels of indol-3-yl acids in potatoes. Ion-exchange liquid chromatography using pressure enabled Richards (20L)to separate mono- and dicarboxylic acids with UV detection at 210 nm. Takata et al. (27L) monitored the LC separation of carboxylic acids with controlled potential coulometry during elution. Rapp (19L)separated the dicarboxylic acids of grape must and wine by high pressure cation-exchange chromatography after concentration to permit refractometric detection. Wallenstein et al. (33L) employed ion exchangeCraig distribution for acids in beets and juices. An automated method for oxalic acid in plant material based on the color reduction of a zirconium/3,4-dihydroxyazobenzene-2’-carboxylic acid complex was reported by Cooke et al. (4L).Michal et al. ( 1 4 L )published an enzymatic method for succinic acid in a diversity of foods. Baking powders were analyzed for organic and phosphoric acids by Zuercher e t al. (34L) with a technique based on GC of T M S derivatives. Gray ( 5 L ) determined lactic acid in whey as its butyl ester by GLC. Schwartz e t al. (25L)esterfied milk fat organic acids a t trace levels with diazomethane in a column of adsorbant before elution and GLC. An enzymic pyruvate method applicable to milk was reported as both a manual and automated method by Suhren et al. (2615).Hyakutake et al. ( 7 L )demonstrated separations of tricarboxylic acid-cycle acids by high speed liquid chromatography on LS-140 gel. Schulz et al. (24L)acylated traces of aliphatic carboxylic acids with 0,O- dimethylhydroxy hydroxymethylphosphonate before GLC with thermionic P detection. Sasson et al. (21L)employed a GLC procedure to find some previously unreported acids in orange peel and juice. Mann et al. (IOL)methylated abscisic acid from an initial TLC plate separation by diazomethane treatment of the silica gel in suspension before gas chromatography. The carbazole method for uronic acid was automated by Thibault et al. (29L)and found useful for pectins after de-esterification and hydrolysis. Industrial pectins were examined for esterification and free acids by Mizote et al. ( I 5 L )who compared a “Cat-Floc’’ procedure to an acid-base method. Arndt et al. ( I L )separated galacturonic acid in wine and juices by TLC of its osazone before final spectrophotometric measurement. Techniques using gas chromatography-mass spectrometry for isolation and identification of organic acids in wort and beer were given by Tress1 et al. (30L).Moll et al. (16L)spectrophotometrically determined iso-a-acids in beer with an automated solvent extraction system. Molyneux e t al. (18L) reported agreement of his NMR determination of a and p hop acids with other methods. Kagi et al. ( 8 L )improved a GLC determination of isohumulone by extraction of the T M S derivatives into isooctane before chromatography. Molyneux et al. ( I 7 L ) demonstrated patterns for different hop varieties using HPLC. The level and significance of catechin in beer was investigated by McGuinness et al. (13L) by GLC of T M S derivatives. Twelve oxoflavonoid derivatives, as well as (+)catechin and cinnamic acid were separated by HPLC when Wulf et al. ( 3 I L ) analyzed grapes and wine. The flavonoids and chlorogenic acids of hops were fractionated by Vancraenenbroeck et al. (32L) using counter-current distribution. Schmidtlein et al. (22%) analyzed quantitatively for free phenolic acids using column and thin-layer chromatography after hydrolysis of fruit and vegetable extracts. Maga et al. (11L)used capillary column GC to investigate oilseed phenolic acid fractions. Tannins as total polyhydric phenols were measured by Schneider (23L) and referred to tea quality. Hanefeld et al. (6L)directly measured caffeic acid esters and catechins on TLC plates and showed application to fruits and vegetables. Clifford et al. (3L)proposed a difference technique for feruloylquinic acids in coffee beans based on molybdophosphate reagent and NaI04 reagent spectrophotometric measurements. The chlorogenic acid fraction of green coffee beans was also separated by Clifford ( 2 L )by TLC on poly-
(vinylpyrrolidone)-CaS04.Grain milling fractions were examined for phenolic acids by Maga et al. (12L)who employed a gas chromatographic method.
NITROGEN The great number of papers on the determination of nitrogen and nitrogen-containing compounds has made it necessary to choose those relating to new techniques or improvements in old techniques and necessarily forced the omission of many worthwhile papers. Two new, faster digestion procedures for the Kjeldahl procedures are described by Von Lengerken et al. (99M) using hydrogen peroxide, selenium, and sulfuric acid as digesting agents. A saving of time over the conventional Kjeldahl is claimed by Batey et al. (5M) by the use of sulfuric-perchloric digestion. A new Kjeldahl catalyst, zirconium dioxide, is recommended by Glowa (34M) to eliminate the use of mercuric oxide. Cupric sulfate has been tested by Wall et al. (103M) in the Kjel-Foss automated instrument and may be substituted for mercuric oxide as a digestion catalyst, and Joerin (45M)reports that if cupric sulfate is used as a catalyst for the determination of protein in milk, then both the potassium sulfate and the digestion time must be increased. A review of Kjeldahl and Dumas methods and automatic analyzers based on these methods by Fleck (29M) also includes brief discussions of methods for nitrogen in specific samples. Among procedures suggested for analysis of Kjeldahl digests are a semi-automated ninhydrin assay described by Quinn et al. (77M),a rapid coulometric method applied by Bostroem et al. (1OM)after the use of a block digestion system, and the use of an ammonia probe in an automated flow system described by Buckee (12M).Four different total protein nitrogen methods were evaluated by Wall et al. (101M) including the Kjel-Foss, the Missouri-Technicon with block digestor, the A.O.A.C. Kjeldahl, and the Kjeldahl with a low level of cupric sulfate catalyst. The four methods gave good accuracy and precision and the relative rapidity and costs were compared for multiple analyses. The Missouri-Technicon block digestor method is further described by Wall et al. (102M).An automated method using the Technicon AutoAnalyzer is shown by Schafer et al. (86M) to provide good precision on determination of nitrogen in milk products. Biuret methods for the determination of protein are applied to milk by Bosset et al. ( 9 M ) using continuous flow analysis, to wheat protein by Mitsuda et al. (62M) who use special solvent treatment to eliminate the interference by starch, to cereal proteins also by Mitsuda et al. (63M) with the use of hydrogen peroxide to eliminate interference from color substances, and by No11 et al. (67M) to meal and flour using a modified biuret reagent which incorporates isopropyl alcohol in the reagent. Interferences in the Lowry protein determination due to manganous, cobaltous, and mercuric chlorides are avoided by Higuchi et al. (40M)by using a standard curve containing the corresponding amount of the metal salt, or by increasing the copper concentration in the reagent. A method for protein in meat samples described by Hendrik (39M) uses sodium hypobromite titration on a neutralized digest. A rapid nonKjeldahl method for determination of the protein content of bread, suggested by Holmes (41M),utilizes steam distillation of ammonia from a dispersion of the sample in barium chloride and sodium hydroxide solutions. The “Infrared Milk Analyzer” is described by Hall (38M)which determines fat, protein, and lactose. Measurement of the protein is by extinction reading a t 6.46 microns. Results agreed well with the microKjeldahl procedure. Dye-binding procedures for the determination of protein in milk are discussed by Park et al. (70M) who compared Kjeldahl, Technicon dye-binding, and Udy methods. The Kjeldahl and Udy methods showed good agreement with each other. Sherbon (88M)has submitted the Pro-Milk automated dye-binding method for protein in milk to collaborative analysis, and the method was found precise and accurate. A patent has been issued to Statter (92M) for an instrument for the determination of protein in meat using a dye-binding technique. A rapid method for the estimation of protein in maize suggested by Pearson et al. (72M) used the reaction of the protein with sulfosalicylic acid after extraction with dilute sodium hydroxide. A fast method for nitrogen determination
in single seeds described by Sundqvist et al. (94M) is based on the (d,p) and ( d p ) reactions of 14N.Gupta et al. (37M)have used 14-MeV neutron activation in the evaluation of protein content in crop plants, particularly rice and other grains. Proton activation with a beam of 16-MeV protons is used by Dohan et al. (25M) for the analysis of protein in grain. An automated protein determination system described by Alexander et al. ( 2 M ) disperses the protein in silver nitrate and measures the change in silver concentration with a silver sulfide crystal Ag+ selective electrode assembly. Carboxymethylcellulose has been found by Zadow et al. (107M) to form insoluble complexes with several proteins; the extent of the precipitation depends upon pH and ionic strength. Six methods for the determination of protein in potato tubers have been studied by Vigue et al. (96M)and shortcomings of applicable methods discussed. Several methods for protein determination in wheat have been compared by Pomeranz et al. (75M)and precision and accuracy found maximum for the Kjeldahl method. A source of error in ammonia determinations has been traced by 0 hAlmhain et al. (69M)to the filter paper used in the methods; however Pearson (71M)reports that this error may be minimized by the use of smaller diameter paper and using a blank determination. Ammonia in beer is determined by Wisk et al. (106M) with a specific ion electrode for ammonia. The problems in the determination of ammonia in brown cake are discussed by Sturm e t al. (93M),and a vacuum distillation method is found suitable. Quantitative extraction of amine or amide nitrogen with aqueous hydrochloric acid is described by Kuck (51M)for the analysis of these compounds in vegetable oils. Procedures for sequence analysis of polypeptides and proteins by combined gas chromatography-mass spectrometry have been discussed and compared by Nau ( 6 6 M ) .A method for the quantitative determination of the K-casein in milk is reported by Hossain (43M)using renin splitting. A critical evaluation of the Harland-Ashworth test for undenatured whey proteins in milk by Puhan (76M)reports that the test is of doubtful value in the classification of milk powders. Amido Black 10B is used by Kolakowski (49M)to determine peptides of fish after trichloracetic acid separation; the same author (50M) also applies a turbidimetric procedure for polypeptides by increasing the trichloracetic content after the first extraction. A technique for the rapid determination of zein in maize reported by Jones et al. (46M) involves deposition of a hot ethanol extract of powdered corn on filter paper disks and determining nitrogen on the disks. Peptides have been analyzed for disulfide by Anderson et al. ( 3 M ) after alkaline cleavage and reaction with 5,5’-dithiobis(2-nitrobenzoic acid). Sulfhydryl and disulfide groups have been determined by Beveridge et al. ( 7 M )in some food proteins using Ellman’s reagent. Amino nitrogen in factory sugar juices is determined by Reinefeld et al. (78M)using the reaction with 2,4,6-trinitrobenzene-l-sulfonic acid. A simple gasometric method for the determination of free amino acid has been developed by Matoba et al. (59M).An enzyme electrode prepared with L-amino-acid oxidase is suggested by Nanjo et al. (65M)for the determination of L-amino acids, and by Guilbault et al. (36M).A study of the effect of the volume of hydrochloric acid used for protein hydrolysis is reported by Robe1 (81M)and a ratio of 2800:l (acid to carbohydrate) is suggested. The state of the art of gas chromatography of amino acids is reviewed by Husek et al. (44M).Amino acids have been analyzed by gas chromatography by March (57M)after formation of the N-heptafluorobutyryl derivatives of the propyl esters, by Makita et al. (56M)by formation of the methyl esters of the N-isobutoxycarbonyl derivatives, and by Kirkman (48M) who compared gas chromatography of the N-heptafluorobutyryl propyl esters with automated cation-exchange chromatography. A nitrogen sensitive thermionic detector is used by Butler et al. (13M) for the determination of the trifluoroacetylated amino acid methyl esters. Davies (23M) has modified the Technicon AutoAnalyzer technique for analysis for amino acids so that two analyses may be completed every four hours. Ion-exchange paper chromatography is used by El Din Awad et al. (26M)to separate some racemic DL-amino acids on alginate. Dansyl derivatives of amines in mixtures are analyzed by Addeo et al. ( 1 M ) by mass spectrometry using metastable defocusing. ANALYTICAL CHEMISTRY, VOL. 49,
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A rapid semiautomated liquid chromatographic method was developed by Vandercook et al. (95M) for the determination of y-aminobutyric acid and arginine in orange juice. A simple fluorometric method for glycine in dietetic beverages is described by Coppola et al. (19M) by the reaction with fluorescamine down to the level of 0.02% glycine. A method for hydroxyproline in meat and meat products using chloramine-T is proposed by Dinarieva et al. (24M).Gas chromatography is suggested by Moss et al. (64M)for the analysis of hydroxyproline and hydroxylysine. Lysine in protein is determined by Sandler et al. (84M)based on the dye binding capacity of the protein before and after treatment masking the terminal amino group of lysine with ethyl chloroformate. The ninhydrin color reaction is suggested by Beckwith et al. ( 6 M )for direct estimation of lysine in corn meals. Chemical methods for available lysine have been compared by Couch et al. (20M)on various proteins and by Creamer et al. (21M) on heated milk powders. A simplified method for lysine by gas chromatography is reported by Zscheile et al. (108M),and an automated method for L-lysine in grain by Wall et al. (IOOM). Lysine has also been determined by high-voltage electrophoresis by Srivastava et al. ( 9 1 M )in cereals. Ninhydrin and prolamin turbidity tests have been compared by Rhodes (79M)for their utility in rapid screening of high-lysine barleys. Another test for lysine in barley is suggested by Fritz et al. ( 3 1 M ) using the color reaction with 2-chloro-3,5-dinitropyridine. A rapid ninhydrin color test for grain screening is applied by Mertz et al. (61M) to split kernels. Gas chromatographic determination of methionine and lysine in feeding stuffs has been described by Gerstl et al. (32M, 33M). Nitrosoproline in uncooked bacon has been isolated and identified by Kushnir et al. (52M)using thin-layer chromatography, gas chromatography, and mass spectrometry. Theanine in tea is determined by Lehmann et al. (54M) by extraction and thin-layer chromatography, and by Vitzthum et al. (97M) by gas chromatography. A new acid-hydrolysis method for determining tryptophan in peptides and proteins is reported by Penke et al. (73M) using mercaptoethanesulfonic acid. Spectrofluorimetric assay of tryptophan is described by Buttery et al. ( 1 )after norharman formation, and by Sasaki et al. (85M)by measuring the fluorescence emission of tryptophan itself. A rapid method described by Concon (18M)for tryptophan in grains uses the reaction with acetic acid-ferric chloride and sulfuric acid. Another method for tryptophan proposed by Matheson ( 5 8 M ) uses colorimetry after the reaction with dimethylaminobenzaldehyde. A method for overcoming the interference of ethanol with the tryptophan procedure of Spies and Chambers is suggested by Concon (17M).Results of a collaborative study on the determination of tryptophan reported by Westgarth et al. (104M) indicate that the Miller method is preferred over the Spies and Chambers method. Soluble salts of cerium IV in the presence of hydroxylamine have been found by Chrastil (16M) to be useful in determining tyrosine in a protein hydrolysate. Aroma concentrates from wine have been analyzed by Schreier et al. (87M) for N-substituted amides by gas chromatography. Volatile amines and amine oxides in food products have been determined by Ruiter (82M) by steam distillation and gas chromatography. Trimethylamine and dimethylamine in fish are determined by Ritskes (80M) on a Carbowax 400/polyethylenimine column with an alkaline precolumn. Amines in fresh and processed pork are determined by Lakritz et al. (53M)by conversion into their dansyl derivatives, thin-layer chromatographic separation, and spectrofluorimetric determination. An automated method for volatile bases in fish and shrimp is described by Ruiter et al. (83M)using an AutoAnalyzer. Biologically active amines, tyramine, tryptamine, and histamine are determined in foods by Voigt et al. (98M) by their reaction with 7-chloro-4-nitrobenzofurazan. Histamine is determined by Lerke e t al. (55M) by derivatization with 0-phthalaldehyde and measuring the fluorescence produced. Quaternary amines in natural extracts are analyzed by Merbach et al. (60M)by nuclear magnetic resonance spectrometry. Tyramine analysis in South African cheeses is achieved by Kaplan et al. (47M) by gas-liquid chromatography. Golovnya et al. (35M) have reported separation of alkylamines on columns modified with trisodium phosphate. A procedure is described by Singer et a1 (89M)for the analysis of naturally occurring nitrosatable secondary amines by the identification of tosylamide derivatives by gas chromatography-mass 210R
ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
spectrometry. Phenethylamine in foods has been determined by Chaytor e t al. (15M)by gas chromatography. Gel chromatography has been used by Frischkorn et al. (30M) to determine caffeine in soft drinks, and by Pokorny et al. (74M)for caffeine in coffee, tea, and mate. Theobromine was determined in bark, beans and leaves of cacao, coffee, and cola by Somorin (90M)using extraction, chromatography on silica gel, and spectrophotometric measurement. High pressure liquid chromatography is applied by Wildanger (105M) to the analysis of caffeine, theophylline, and theobromine in various foods. Hydrolysis in 72% perchloric acid and separation by ion-exchange chromatography is suggested by Erskine et al. (28M) for the analysis of purine and pyrimidine bases in n-alkane grown yeasts. A method for quantitative thin-layer chromatography of adinosine 5’-triphosphate and its degradation products in meat has been described by Norman e t al. (68M).Creatinine is determined by Blass et al. ( 8 M ) by inverse polarography with alkaline picrate and 3,5-dinitrosalicylic acid. A method for the quantitative determination of 5-hydroxytryptamide in coffee has been developed by Culmsee ( 2 2 M ) .Nucleic acids in pea seeds are analyzed by El-Hamalawi et al. (27M)by the use of ethidium complexes. The dansyl derivatives of biogenic amines in foods are used by Bancher et al. ( 4 M ) for the determination by thin-layer chromatography of these compounds. Urea and ammonium salts in meat products are determined by Honikel et al. (42M) by the use of test strips. Revised methods of sampling and testing gelatin have been published by the British Standards Institution ( 1 1 M ) .
VITAMINS Means of improving the procedures for the determination of vitamins use modified classical techniques, automated techniques, and modern instrumentation. An improved procedure for determining vitamin A with trichloroacetic acid has been described by Grys (18N);and Vahlquist (59N)has used the same reagent to determine total vitamin A and esterified vitamin A in milk. A direct solvent-extraction technique has been used by Bayfield ( 6 N )to determine total vitamin A by trichloroacetic acid, and the vitamin A esters by paper chromatography. A simplification of the official vitamin A method for feeds has been developed by Parrish (37N)to be applied to foods and was submitted for a collaborative study (38N) and as a result the method was adopted as official first action. Industrial control of vitamin A in butter has been simplified by the use of saponification in dimethyl by Belliot et al. (8N) sulfoxide for routine determinations. A gel chromatographic separation of retinol, retinyl esters, and other fat-soluble vitamins has been achieved by Holasova et al. ( 2 I N ) on s e phadex LH-20 followed by separation on five columns in series. A modified fluorometric procedure for vitamin A in milk has been found by Senyk et al. (54N)to provide rapid analysis of large numbers of samples. Atuma et al. ( 4 N )have reported on the voltammetric behavior of vitamin A and D a t carbonpaste and vitreous-carbon electrodes and applied the method to the analysis of margarine. A specific method for the determination of provitamin A carotenoids in orange juice has been described by Reeder et al. (47N)using high speed liquid chromatography after saponification. Vitamin D has been determined by Zanobibi e t al. (66N)in avocados by its reaction with antimony trichloride and by thin-layer chromatography. A collaborative study on the determination of vitamin D in cottonseed oil has been reported by Quackenbush et al. (44N) which included both chemical and biological methods. Agreement between methods was in general poor and further method development work is planned. A chemical method for vitamin D in foods has been proposed by Petrova e t al. (41N) which used hydrolysis, chromatography, and spectrophotometry. The hydroxylated derivatives of vitamin Ds have been separated by Matthews et al. (31N)using high speed liquid chromatography. Vitamin Dz in fortified fullcream dried milk has been determined by Bell et al. ( 7 N )using gas chromatography of the trimethylsilyl ether. Thin-layer chromatography on silica gel has been used by Waters et al. ( 6 0 N ) for determining a-tocopherol in citrus essential oils. High-speed liquid chromatography has been used by Abe et al. ( I N )to separate tocopherols in vegetable oils, and by Gavins et al. (11N) using high-resolution liquid
chromatography on Corasil 11. Oil seeds have been analyzed for tocopherols by Dompert et al. (13N) using gas chromatography after separation by thin-layer chromatography, and a similar technique has been described by Abe et al. ( 2 N )for the analysis of foods. Another thin-layer, gas chromatographic technique for tocopherols has been proposed by Boatella Riera ( 9 N ) for the analysis of vegetable oils. An electrochemical determination of vitamin E in margarine and other oils has been suggested by Atuma ( 3 N ) using voltammetry with a carbon-paste or vitreous-carbon electrode. By the use of fractional crystallization a t -65 "C, the triglycerides and unsaponifiables have been separated by Zandi et al. (65N)and the tocopherols are then identified by thin-layer chromatography and determined by the Emmerie-Engels reaction. A scheme of chemical analysis has been devised by Wiggins (61N)for the determination of vitamins A, D, and E. The separation of fat-soluble vitamins by thin-layer chromatography has been studied by Perisic-Janjic et al. (40N) who suggest separation on thin layers other than silica gel or alumina. A better method for the recovery of thiamine from Decalso in the thiochrome method has been proposed by Pippen et al. ( 4 3 N ) .An improved procedure for the determination of thiamine has been suggested by Edwin et al. (14N) using the reaction with cyanogen bromide. An automated method for the analysis of thiamine in milk has been described by Kirk (26N) which uses automation of the thiochrome method. Automated and manual procedures for thiamine and riboflavin in foods have been compared by Pelletier et al. (39N) and results by both procedures were equivalent. Kirk (27N) has also published an automated method for the determination of riboflavin in milk. Another automated method for the determination of riboflavin in foods has been described by Egberg et al. (15N).A collaborative study of the automated method for the determination of niacin and niacinamide in cereal products has been completed by Gross ( 17 N ) and compared with the manual and microbiological methods. There was no significant difference between methods. Ion-exchange chromatography has been used by Yasumoto et al. (64N) in a semi-automated system for analysis of the vitamin Be complex, and by Williams et al. (62N) for the separation of pyridoxal, pyridoxol, and pyridoxamine. Spectrofluorimetric measurements has been used by Soederhjelm (55N)to measure pyridoxine in enriched foodstuffs. A method for the fluorimetric measurement of pyridoxal in dried milk has been suggested by Fiedlerova et al. (16N) which uses separation on Dowex 50W-X8 as a clean-up step. Cobalamins in liver extracts have been determined by Tortolani et al. (57N) by chromatography on SP-Sephadex. Orotic acid has been determined in milk by Yao et al. (63N)by polarography after coagulation of the proteins. A new method for the determination of panagamic acid has been proposed by Kraszner-Berndorfer et al. (28N) which is based on the reaction of pangamic acid with iodomethane. A radiochemical assay for biotin has been developed by Hood (22N)based on the competitive binding between a known amount of [14C] biotin and nonradioactive biotin for the binding sites on avidin. Choline has been determined by Szasz et al. (56N) in plant substances by precipitation as the reineckate and spectrophotometric measurement. Thin-layer chromatography has been used for the determination of folic acid by Tripet et al. (58N).Free and bound inositol in human and cow's milk has been determined by Ogasa et al. (35N) using gas chromatography. The photodegradation of vitamin K has been followed by Nakata et al. (34N) using gas chromatography. Methods for the determination of ascorbic acid have been especially numerous in the past two years. A modified method for ascorbic acid in preserved juices has been described by Sarwar et al. (51N) using N-bromosuccinimide as titrant. Randall et al. (45N) have described the extraction of total ascorbic acid from vegetables using ethanol as a slurrying medium. A direct spectrophotometric method for the simultaneous determination of L-ascorbic and L-dehydroascorbic acid has been developed by Baczyk et al. ( 5 N ) using measurement at three wavelengths. The fluorometric assay for vitamin C has been adapted by Kirk et al. (25N)to continuous flow analysis. A stopped-flow technique has been used by Karayannis (23N)for a kinetic determination of ascorbic acid reaction. by the 2,6-dichlorophenolindophenol-indopheno1 A spectrophotometric determination of vitamin C in citrus
fruits has been proposed by Hassan 'et al. (20N)using spectrophotometry with peri-naphthindan-2,3,4-trionefor the color reaction. The dinitrophenylhydrazine method for ascorbic acid and dehydroascorbic acid has been simplified by Schmidt et al. (53N) and adopted to an automated microliter system. Gas chromatographic methods for L-ascorbic acid have been developed by Schlack (52N),and for the separation and determination of L-ascorbic acid and its oxidation products by Pfeilsticker et al. ( 4 2 N ) .A new colorimetric reagent for vitamin C, 4-nitro-1,2-phenylenediamine, has been described by Bourgeois et al. (ION)which is used after Sephadex separation and oxidation to dehydroascorbic acid. Another titration reagent for ascorbic acid, thallium(II1) perchlorate has been used by Gupta et al. (19N)to determine the vitamin in fruits. Ascorbic acid has been determined iodimetrically by controlled-potential coulometry by Karlsson ( 2 4 N ) ,by reverse sweep cathode ray polarography by Owen et al. (36N),and by automated constant-current coulometry by Moros et al. (32"). Another electrochemical method has been used by Lindquist (29N)who determines ascorbic acid by voltammetry with a carbon-paste electrode. The enzymic method for the assay of ascorbic and dehydroascorbic acids in fruits has been discussed by Marchesini et al. (30N)using ascorbic oxidase. The reaction of selenious acid with ascorbic acid has been found by Ralls (46N)to provide the basis for a turbidimetric determination of the vitamin in foods. A new chronometric assay of vitamin C has been described by Roe et al. (48N) using the reaction with p-phenylenediamine and measuring the time lag from initiation of the reaction to the first appearance of the colored product. Added crystalline ascorbic acid has been detected in foods by Mueller-Mulot (33N) by a microchemical color test with selenous acid. A rapid spot test for ascorbic acid in tomatoes has been used by Rymal et al. (50N) using paper strips soaked in sodium 2,6dichloroindophenol and sprayed with starch. A discussion of automated analysis of water-soluble vitamins in food has been published by Roy et al. (49N).Chemical and microbiological methods for vitamins in foods have been reviewed by De Ritter (12N).
MISCELLANEOUS A review of food analysis publications from 1971 to 1974 was published by MacLeod (13P). Watt et al. (27P) described USDA research done for tables of food composition. A symposium relevant to food labeling and analysis appeared in the Journal of the Association of Official Analytical Chemists ( 2 4 P ) .Computers applied to flavor chemistry comprised the theme of a symposium reported in the Journal of Agriculture and Food Chemistry (25P). The use of instrumentation in food analysis was discussed in an article (1OP).Carballido et al. (4P) showed applications of infrared spectrometry in food analysis. A near-infrared method for oil, protein, and moisture in cereals was discussed by Williams (30P).Wildanger (29P) reviewed HPLC equipment and practices suitable for food analysis. The British Standards Institution published their Methods for Chemical Analysis of Cheese (15P).Buckbee et al. (3P) reviewed automated and semi-automated methods useful in the brewing industry. Applications of immobilized enzymes for food were reviewed by Bihari et al. (2P).Brazilian green coffee quality was correlated to multiple analyses with linear re ressions by Amorim et al. ( I P ) .Olson et al. (17P)also reviewef immobilized enzyme uses. Iwasa (11P) described green tea chemical analysis with official methods. Ganzlin (8P)showed a simplified extraction of hop extracts for various fractions. This author (9P)also gave comparative extraction data. Acidic and basic components were extracted and homogenized in procedures given by Chaytor et al. (5P)for foods. .A density separation allowed Finley (7P)to segregate carbohydrate and protein rich fractions of flour. Elkins (6P)studied interlaboratory variation with respect to nutrient analysis. Weetall (28P) reported on the analytical applications of immobilized enzymes. Schaefer et al. (21P) investigated 13C NMR as a tool for oil, starch, and protein analysis of seeds. A quality control program for the dairy industry using GC was proposed by Sterken et al. (23P). Malkus (14P) reviewed electrochemical methods in food analysis. Salzer (19P)compared methods t o determine critical spice components. CafANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
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feine, theophylline, and theobromine were separated simultaneously by TLC by Thielemann (26P).Schaal et al. (20P) measured oxygen diffusion through sausage casings with an . 02 electrode.
LITERATURE CITED Addltlves ( I A ) Baluja, G., Franco, J. M., Murado, M. A,, Arch. Envlron. Contam. Toxicol., 1, 375 (1973); Chem. Abstr., 81, 150393s (1974). (2A) Coppola, E. D., Christie, S. N., Hanna, J. G., J. Assoc. Off. Anal. Chem., 58, 58 (1975). (3A) Coppola, E. D., Wickroski, A. F., Hanna, J. G., lbid., p 469. (4A) Cuzzoni, M. T., e z z a n i , G., Farmaco, Ed. Prat., 29, 739 (1974); Chem. Absfr., 82, 84540e (1975). (5A) Drozd, J., Novak, J., Wicar, S., J. FoodSci., 40, 1109 (1975). (6A) Eipeson, W. E., Mahadeviah, M., Gowrarnma, R. V., Sastry, L. V. L., J. Food Sci. Technol., 11, 209 (1974); Chem. Abstr., 83, 56815a (1975). (7A) Fiddler, R. N., Gentilcore, K. M., J. Assoc. Off. Anal. Chem., 58, 1069 (1975). (8A) Fogden, E., Fryer M., Urry, S.,J. Assoc. Public Anal., 12 (4th Qtr), 93 (1974). (9A) Franco, V., Holak, W., J. Assoc. Off. Anal. Chem., 58, 293 (1975). (10A) Gutfinger, T., Ashkenazy, R.. Letan, A,, Analyst (London), 101, 49 (1976). (1 1A) Hauser, E., Weber, U., Fleischwirtschaff, 55, 547 (1975); Anal. Abstr., 30, 6F13 (1976). (12A) Hazemoto, N., Kamo, N., Kobatake,, Y., J. Assoc. Off. Anal. Chem., 57, 1205 (1974). (13A) Hils, A., Deut Lebensm.-Rundsch., 70,265 (1974); Chem. Abstr., 82, 419043 (1975). (14A) Hurtubise, R. J., Anal. Chem., 47, 2457 (1975). (15A) Hussein, M. M., Jacin, H., Rodriguez, F. B., J. Agric. Food Chem., 24, 36 (1976). (16A) lioka, K., Eiyo To Shokuryo, 27,413 (1974); Chem. Abstr., 83, 7276s (1975). (17A) International Organization of the Flavour Industry, lnt. Flavours Food Addit., 6, 339 (1975); Anal. Abstr., 30, 5F37 (1976). (18A) Ishiwata, A., Suzuki, Y., ShokuhinEiseigaku Zasshi, 16, 420 (1975); Chem. Absfr., 84, 149325b (1976). (19A) Jerumanis, J., Rieder, G., Devreux, A,, Brauwissenschafi, 28, 19 (1975); Anal. Abstr., 29, 4F36 (1975). (20A) Kaito, T., Itagaki, K., Sagara. K., Ito, Y., Jpn. Anal., 23, 1494 (1974); Anal. Abstr., 29, 2E36 (1975). (21A) Kalinowski, D., Rocz. fanstw. Zakl. Hig., 28, 165 (1975); Chem. Abstr., 83, 1458422 (1975). (22A) Kaneshima, H., Ogawa, H., Yamagishi, T., Kinoshita, Y., Mori, M., Hokkaidoritsu Eisei Kenkyusho Ho, 24,64 (1974); Chem. Abstr., 8 3 , 5 6 8 0 6 ~ (1975). (23A) Karlsson, R., Torstensson, L-G, Talanta, 21, 945 (1974); Anal. Abstr., 28, 4F31 (1975). (24A) {bid., 22, 27 (1975); Anal. Abstr., 29, 3 8 1 12 (1975). (25A) Klostermeyer, H., Popp. U., Reimerdes, E. H., 2. Le6ensm.-Unters-Forsch, 158, 73 (1975); Chem. Abstr., 83, 77101e (1975). (26A) Kodama, Y., Shintani, K., Morimoto, K., Hiroshima-ken Elsei Kenkyusho Ho, 21, 29 (1974); Chem. Abstr., 82, 8 4 5 6 2 ~(1975). (27A) Kroller, E., Fette, Seifen, Anstrichm, 76, 496 (1974); Anal. Abstr., 29, IF50 (1975). (28A) La Rotonda, M. I., Ferrara, L., Boll. Soc. ltal. Biol. Sper., 51, 690 (1975); Anal. Absfr., 30, 5F40 (1976). (29A) Larsson, B., Fuchs, G., Swed. J. Agric. Res., 4, 109 (1974); Anal. Absfr., 27, 2900 (1974). (30A) Mandrou, B., Roux, E., Brun, S., Ann Falslf. Expert. Chim., 88,29 (1975); Anal. Abstr., 30,5F56, (1976). (31A) Marine Font, A., Valls Lopez, G., Circ. Farm., 33, 25 (1975); Chem. Absb., 83, 416063 (1975). (32A) Mordret, F., Le Barbanchon, N., Rev. Fr. Corps Gras, 22, 387 (1975); Anal. Abstr., 31, 4F22 (1976). (33A) Nagai, I., Oka, H., Tasaka. M., Oka, A., Elsel Kagaku, 21,261 (1975); Chem. Absfr., 84,42107e ( 1976).
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ACKNOWLEDGMENT The efforts expended by Ms. M. Leggio, I. Lombardi, and R. Roak in typing and proofreading are appreciated.
(34A) Nakarnura, M., Watabe, K., Kirigaya, T., Yazawa, Y., Watabe, A., Suzukl, Y., Kawamura, T., Shokuhin Eiselgaku Zasshi, 18, 264 (1975); Chem. Abstr., 84, 88058t (1976). (35A) Nakarnura, Y., bid., 16, 368 (1975); Chem. Abstr., 84, 149368t (1976). (36A) Nagasawa, K., Ogamo, A., Shinozuka, T., J. Chromatogr., 111, 51 (1975). (37A) Nagasawa, K., Shinozuka, T., Ogamo, A,, Elsel Kagaku, 20,337 (1974); Anal. Abstr,, 30, 2F39 (1976). (38A) Nishijima, M., Kanrnuri, M., Takahashi, S.. Kamimura, H., Nakazato, M., Kimura, Y., Shokuhin Eiseigaku Zasshi, 18, 110 (1975); Chem. Abstr., 83, 145855f (1975). (39A) Nishijirna, M., Kanmuri, M., Takahashi, S., Karnimura, H., Nakazato, M., Watari. Y., Kirnura, Y., bid., 17, 78 (1976); Chem. Absfr., 85, 19174m (1976). (40A) Nose, N., Tanaka, A,, Kobayashi, S., Suzuki, T., Hosino, Y., Watanabe, A,, Eisei Kagaku, 20, 194 (1974); Chern. Abstr., 82, 2710y (1975). (41A) Pfeiffer, S.L., Smith, J., J. Assoc. O f f .Anal. Chem., 58, 915 (1975). (42A) Regula, E., J. Chromatogr., 115, 639 (1975). (43A) Revuelta, D., Revuelta, G., Armisen, F., An. Quim., 71, 179 (1975); Anal. Absfr., 29, 4F28 (1975). (44A) Roy, R. B., Sahn, M., Conetta, A,, J. Food Scl., 41, 372 (1976). (45A) Sakai, A., Harada, M., Tanimura, A,, Shokuhin Eiseigaku Zasshi, 16, 123 (1975); Anal. Abstr., 31, 4F23 (1976). (46A) Sakai, T., Miyahara, T., Muto, T.. Kurata, G., EiseiKagaku, 20, 15 (1974); Chem. Abstr., 81, 103336r (1974). (47A) /bid., p 20; Chem. Abstr., 81, 103335q (1974). (48A) Schrnid, M. J., Otteneder, H., Getreide, Mehl Brot., 30, 62 (1976); Chem. Abstr., 84, 1630089 (1976). (49A) Shigematsu, T., Ota, A., Matsui, M., Bull. lnsf. Chem. Res. Kyoto Univ., 51, 268 (1973); Anal. Abstr., 27, 3824 (1974). (50A) Singh, J., Lapointe, M. R., J. Assoc. Off. Anal. Chem., 57, 804 (1974). (51A) Smyly, D. S., Woodward, B. B., Conrad, E. C., J. Assoc. Off. Anal. Chem., 59, 14 (1976). (52A) Sontag, G., Kainz, G., Mikrochim. Acta, 1, 107 (1976); Chem. Abstr., 84, 88071s (1976). (53A) Stafford, A. E., J. Agric. FoodChem., 24, 894 (1976). (54A) Tanaka, Y., Ikebe, K., Tanaka, R., Kunita, N., Shokuhin Eiseigaku Zasshi, 16, 295 (1975); Chem. Abstr., 84, 88059~ (1976). (55A) Unterhalt, B., Z.Le6ensm.-Unters.-Forsch., 159, 161 (1975); Chem. Abstr., 84, 42087y (1976). (56A) Usher, C. D., Telling, G. M., J. Scl. Food Agric., 26, 1793 (1975). (57A) van Bronswijk, W., Aust. Wine Brew Spirit Rev., 40 (1974); Anal. Abstr., 30, IF20 (1976). (58A) van Gend, H. W., 2. Le6ensm.-Unters.Forsch., 158, 137 (1975); Chem. Abstr., 83, 112466b (1975). (59A) Weisz, H., Hanif, M., Anal. Chim. Acta, 81, 179 (1976). (60A) Williams, D. T., J. Assoc. Off. Anal. Chem., 57, 1383 (1974). (61A) Yoshikawa, S.,Yabuuchi, H., Mihara, K., Yoshida, Y., Saito. K., Kojima, Y., ShokuhinEiseigaku Zasshi, 15, 381 (1974); Chem. Abstr., 82, 64563q (1975). (62A) Zonneveld, H., J. Sci. Food Agric., 28, 879 (1975); Anal. Abstr., 30, 3F19 (1976).
Adulteration, Contamlnatlon, and Decomposltlon
(le) Anania, M. C., Attina, M., Cacace, F., Farmaco, Ed. Prat., 29, 456 (1974); Anal. Absfr., 28, 3F35 11975). (2Bj Archibald, J., Cochrane, A. L., Analyst (London), 100, 355 (1975). (38) Ashoor, S. H., Chu, F. S., J. Assoc. Off. Anal. Chem., 58, 617 (1975). (48) Bates, H. A,, Rapoport, H., J. Agric. Food Chem., 23, 237 (1975).
ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
(5B) Beljaars, P. R., Schumans, J. C. H. M., Koken, P. J., J. Assoc. Off. Anal. Chem., 58, 263 (1975). (6B) Bencze, K., Kiermeier, F., Miller, M., Z. Le6ensm.-Unters. Forsch., 159, 7 (1975); Anal. Abstr., 30, 4F8 (1976). (78) Berman, M. R., Zare, R. N., Anal. Chem., 47, 1 : 1200 (1975). (8B) Bose, P. K., Roy, B. R., J. FoodSci. Technol., 12, 95 Y5 (1975). (1Y75). (9B) Breder, C. V., Dennison, J. L., Brown, M. E., J. Assoc. Off. Anal. Chem., 58, 1214 (1975). (IOB) Brickey, P. M., Jr., Gecan, J. S., J. Assoc. -Off. Off. Anal. Chem.. 58. 1302 (1975). ( I I B ) Calhoun, M: J., Dellamonica, E . S., J. Assoc. Off. Anal. Chem., 57, 1342 (1974). (12B) Carnevale, J., Food Technol. Aust., 27, 165 (1975); Anal. Abstr., 30, 6F22 (1976). (138) Chand, S.,Srinivasulu, C., Mahapatra, S. N., J. Chromatogr., 106, 475 (1975). (148) Chang, S. K., Harrington, G. W., Anal. Chem., 47, 1857 (1975). (158) Corely, C., Miller, R. W., Hill, K . R., J. Assoc. Off. Anal. Chem., 57, 1269 (1974). (16B) Cox, G. B., Loscombe, C. R., Upfield, J. A,, Analyst (London), 101, 381 (1976). (178) Crathorne, B., Edwards, M. W.. Jones, N. R., Walters, C. L., Woolford, G., J. Chromatogr., 115, 213 (1975). (18B) Crosby, N. T., Sawyer, R., Adv. FoodRes., 22, 1 (1976). (19B) Day, E. W., Jr., Vanatta, L. E., Sieck, R. F., J. Assoc. Off. Anal. Chem., 58, 520 (1975). (208) de Brabander, H. F., Verbeke, R., J. Chromatogr., 108, 141 (1975). (218) de Jong, I. G., Omori, T., Wiles, D. R., J. Chem. SOC.,Chem. Commun., 5, 189 (1974). (22B) Drawert, F., Barton, H., Z. Lebensm.-Unfers. Forsch., 154, 223 (1974); Anal. Abstr., 27, 2918 (1974). (238) Drawert, F., Beck, B., Z. Le6ensm.-Unters. Forsch., 158, 20 (1974); Anal. Abstr., 28, 4F15 (1 975). (248) Dupuy, H. P., Rayner, E. T., Fore, S. P., J. Am. Oil Chem. Soc., 52, 354 (1975). (258) Durackova, Z.,Betina, V., Nemec, P., J. Chromatogr., 116, 141 (1976). (268) Eisenbrand, G., Janzowski, C., Preussmann, R., J. Chromatogr., 115, 602 (1975). (278) El-Nawawy, F. A., Wien. Tieraerrti. Monatsschr., 61, 66 (1974); Anal. Absfr., 28, 5 F l l (1975). (288) Erney, D. R., J. Assoc. Off. Anal. Chem., 58, 1202 (1975). (298) Ernst, G. F., van Lierop, J. B. H., J. Chromafogr., 109, 439 (1975). (308) Eyrich, W., Chem., Mikrobiol., Technol. Lebensm., 4, 17 (1975); Chem. Abstr., 83, 4 1 6 3 3 (1975). (318) Farmer, S.,Chem. lnd. (London),24, 1061 (1975). (328) Fehringer, N. V., J. Assoc. Off. Anal. Chem., 58, 1206 (1975). (338) Figge, K., Dtsch. Lebensm. Rundsch., 71, 129 (1975); Anal. Abstr., 29, 6F12 (1975). (348) Figge, K.. Koch, J., Fette, Seifen, Anstrichm., 77, 184 (1975); Anal. Abstr., 30, IF1 (1 976). (358) Fine, D. H., Ross, R., Rounbehler, D. P., Silvergleid, A., Song, L., J. Agric. Food Chem., 24, 1069 (1976). (368) Fine, D. H., Rounbehler, D. P., Oettinger, P. E., Anal. Chim. Acta.. 78,383 (1975); Anal. Abstr., 30, 4F6 (1976). (378) Fine, D. H., Rounbehler, D. P., J. Chromatogr., 109, 271 (1975). (388) Fonseca, H., Del Nery, H., Rev. Bras. Tecnol., 4, 213 (1973); Anal. Abstr., 28, 2Fll (1975). (398) Foreman, J. K., Goodhead, K., J. Sci. Food Agric., 26, 1771 (1975). (408) Foster, P. M. D., Slater, T. F., Patterson, D. S. P., Biochem. SOC.Trans., 3, 875 (1975); Chem. ~ Abstr., 84, 1 3 4 1 7 0 (1976). (418) Frahm, L. J.. George, G. M., McConnell, J. P., J. ASSOC.Off. Anal. Chem., 58, 694 (1975). (428) Franco, V., Holak, W.. J. Assoc. Off. Anal. Chem., 58, 293 (1975).
(438) Frauenfelder, L. J., J. Assoc. Off. Anal. Chem., 57, 796 (1974). (448) Fritz, W., Donath, R., Nahrung, 18, 827 (1974); Chem. Abstr., 82, 1 1 0 3 5 7 ~ (1975). (458) Fuchs, G., Sundeil, S.,J. Agric. f o o d Chem., 23, 120 (1975). (468) Fujimoto, Y., Suzuki, T., Hoshino, Y . , J. Chromatogr., 105, 99 (1975). (478) Fukuhara, K., Takeda, M., Uchiyama, M., Tanabe, H., Eisei Kagaku, 21, 318 (1975); Anal. Abstr., 31, I F 3 1 (1976). (488) Furda, I., Malizia, P. D., Kolor, M. G., Vernieri, P. J., J. Agric. FoodChem., 23, 340 (1975). (498) Gabany, A. E., Jr., Senman, H., Am. Lab., 8, 49 (1976); Chem. Abstr., 85, 92285c (1976). (508) Garner, R. C., J. Chromatogr., 103, 186 (1975). (518) Gedek, W., Arch. Lebensmittelhyg., 27, 91 (1976); Chem. Abstr., 85, 922864 (1976). (528) Gee, M. G., Land, D. G., Robinson, D., J. Sci. Food Agric., 25, 829 (1974). (538) Gegiou, D., Analyst (London), 99, 745 (1974). (548) Genigeorgis, C., Kuo, J. K., Appl. Environ. Microbiol., 31, 274 (1976); Chem. Abstr., 84, 1493601 (1976). (558)Gether, J., Lunde, G., Le6ensm.-Wiss. Technol., 8, 183 (1975); Anal. Abstr., 30, 5G17 (1976). (568) Giam, C. S.,Chan, H. S.,Neff, G. S.,Anal. Chem., 47, 2225 (1975). (578) Goodhead, K., Gough, T. A,, Food Cosmet. Toxicol., 13, 307 (1975); Anal. Abstr., 30, 5F12 ,I 1976) . . -,. (588) Gough, T. A,, Sugden, K., J. Chromatogr., 109, 265 (1975). (598) Grandi, A., Apidologie, 6, 91 (1975); Anal. Abstr.. ~. , 31. 1F30 11976). (608) Grimme;, G., Boehnke, H., J. Assoc. Off. Anal. Chem., 58, 725 (1975). (618) Grunwaldt, H. S., Heigener, H., Landwirlsch. forsch., 28, 298 (1975); Chem. Abstr., 84, 162968q ( 1976). (628) Hagan, S.N.,Tietjen, W. H., J. Assoc. Off. Anal. Chem., 58, 620 (1975). (638) Hald, B.,Krogh, P., J. Assoc. Off. Anal. Chem., 58, 156 (1975). (648) Hamann, J., Heeschen. W., Tolle, A,, Hahn, G., Milchwissenschaft, 30, 139 (1975); Chem. Abstr., 82, 153903q (1975). (658) Hamann, J., Toile, A,, Bluethgen, A , , Heeschen. W., Milchwissenschaft, 30, 68 (1975); Anal. Abstr,, 29, 5F42 (1975). (668) Hauser, H. J.. Guenther, H. O., J. Chromatogr., 95, 232 (1974). (678) Hayes, A. W., McCain, H. W., f o o d c o m e t . Toxicol., 13, 221 (1975). (688) Heathcote, J. G., Hibbert. J. R., J. Chromatogr., 108, 131 (1975). (698) Heisler, E. G., Siciliano, J., Krulick, S., Feinberg, J., Schwartz, J. H., J. Agric. Food Chem., 22, 1029 (1974). (708) Hirokado, M., Endo, F., Usami, H., Fujii, T., Tokyo Toritsu Eisei Kenkyusho Kenkyu Nempo, 26, 220 (1975); Chem. Abstr., 84, 1 4 9 4 0 0 ~(1976). (718) Hoeiierer, G., Jahr, D., Z. Le6ensm.-Unters. forsch., 157, 65 (1975). (728) Hult, K., Gatenbeck, S.,J. Assoc. Off. Anal. Chem., 59, 128 (1976). (738) Hurrell, R . F., Carpenter, K. J., Br. J. Nutr., 33, 101 (1975); Chem. Abstr., 82, 168913s (1975). (748) Imai, C.. Watanabe, H., Haga, N., Ii., T., J. Am. OllChem. Soc., 51,326 (1974). (758) bid., p 495. (768) Ishibashi, T., Matsui, M., Kawabata, T., Bunseki Kagaku, 24, 107 (1975); Anal. Abstr., 29, 4F8 (1 975). (778) Iwaoka, W. T., Weisman, M. S.,Tannenbaum, S.R., /ARC Sci. Publ., 9, 32 (1975); Chem. Abstr., 130083d (1975). (788) Iwaoka, W. T., Hansen, T., Hsieh, S.-T., Archer, M. C., J. Chromatogr., 103, 349 (1975). (798) Jacin, H., Dtsch. Lebensm. Rundsch., 71, 428 (1975); Anal. Abstr., 31, IF26 (1976). (808) Jain, A. V., Schall, E. D., J. Assoc. Off. Anal. Chem., 58, 818 (1975). (818) Juffs, H. S.,J. DairyRes., 42,277 (1975); Chem. Abstr., 83, 568254 (1975). (828) Kaminski, E., Stawicki, S., Wasowicz, E., Przybylski, R., Conserv. Grains Recoltes Humides, C. R. Symp. lnt., 1973, 261; Chem. Abstr., 83, 56833e (1975). (838) Karasz, A. B., DeCocco, F., Maxstadt, J. J., Curthoys, A., J. Assoc. Off. Anal. Chem., 57, 541 (1974).
-
~
(848) Karkocha, I., Rocz. Panstw. Zakl. Hig., 24, 703 (1973); Anal. Abstr., 27, 3595 (1974). (858) Kaufmann, G:, Schubert, K., Nahrung, 19, K5 (1975); Anal. Abstr., 29, 3F11 (1975). (868) Kawabata, T., /ARC Sci. Pub/., 9, 154 (1975); Anal. Abstr., 30, 4F5 (1976). (878) Kedzierski, B.,Pr. lnst. Lab. &daw. Przem. Spozyw., 25, 277 (1975); Chem. Abstr., 84, 162997s (1976). (888) Kelly, F. T., Nunn. J. R., /ARC Sci. Pub/., 9, (1975). 26 (1975); Chem. Abstr., 83, 1 4 5 8 2 5 ~ (898) Knorr, F., Brauwissenschaft, 28, 136 (1975); Anal. Abstr., 29, 6F34 (1975). (908) Koch, J., Kroehn. R., Dtsch. Lebensm. Rundsch., 71, 291 (1975); Anal. Abstr., 30, 3F39 ( 1976). (918) Koiier, W. D., Orth, R., Mitteilungsbl. GDCh-Fachgruppe Lebensmittelchem. Gerichtl. Chem., 29, 153 (1975); Chern. Abstr., 83, 112435r (1975). (928) Kroeller, E., Dtsch. Lebensm. Rundsch., 71, 112 (1975); Anal. Abstr., 29, 4F29 (1975). (938) Kupfer, W., ibid., 72, 81 (1976); Anal. Abstr., 31, 4F1 (1976). (948) Kvenberg, J. E., J. Assoc. OK Anal. Chem., 58, 441 (1975). (958) Kvenberg, J. E., Eisenberg, W. V., King, A. C., ibld., p 443. (968) Lafont, P., Lafont, J.. Cah. Nub. Diet., I O , 57 (1975); Anal. Abstr., 30, 6F6 (1976). (978) Legat, T., Rocz. Panstw. Zakl. Hig., 26, 171 (1975); Anal. Abstr., 30, 3F8 (1976). (988) Leistner, L., fleischwirtschaft, 55, 985 (1975); Anal. Abstr., 30, 5G21 (1976). (998) Leventhal, B.,Daun, H., Gilbert, S. G., J. foodSci., 41, 467 (1976). (1008) Levi, C. P., J. Assoc. Off Anal. Chem., 58, 258 (1975). (1018) Levi, C. P., Trenk, H. L., Mohr. H. K., ibid., 57, 866 (1974). (1028) Liuzzo, J. A., Lagarde, S.C., Grodner, R. M., Novak, A. F., J. food Sci., 40, 125 (1975). (1038) Marcus, J. G., J. Am. Oil Chem. Soc., 5 1, 472 (1974). (1048) Mascini, M., Lucci, A,, Ferramondo, A,, Mitt. Geb. Lebensmibelunters. Hyg., 65, 221 (1974); Anal. Abstr., 27, 2909 (1974). (1058) McGinnis, E. L., Norris, M. S.,J. Agric. FoodChem., 23, 221 (1975). (106B) McKinney, J. D., J. Am. Oil Chem. Soc., 52, 213 (1975). (1078) Meranger, J-C., J. ASSOC.Off. Anal. Chem., 58, 1143 (1975). (1088) Meyer, R. A., Nahrung, 20, 79 (1976); Anal. Abstr., 31, 4F12 (1976). (1098) Meyer, R. A., ibid., 19, K 1 (1975); Anal. Abstr., 29, 3G2 (1975). (1108) Michielli. R. F., Downing, G. V., Jr., J. Agric. food Chem., 22, 449 ( 1974). (1 118) Ministry of Agricuiture, U. K., Fisheries and Food, Ana/yst(London),101,386 (1976); Chem. Abstr., 85, 92272w (1976). (1128) Mirocha, C. J., Pathre, S.V., Behrens, J., J. Assoc. Off. Anal. Chem., 59, 221 (1976). (1138) Morgan, N. L., Bull. Environ. Contam. Toxicol., 14, 309 (1975); Anal. Abstr., 30, 4F10 ( 1976). (1148) Murthy, M. N. K.. Chandrasekhara, N., J. foodSci. Technol., 11, 238 (1974). (1 158) Naoi, Y., Kazama, E., Saito, K.. Ogawa, H., Shimura, K., Kimura, Y . , Tokyo Toritsu €;sei Kenkyusho Kenkyu Nempo, 25,203 (1974); Chem. Abstr., 82, 153879m (1975). (1168) Nelson, J. J., J. Assoc. Off. Anal. Chem., 59, 243 (1976). (1178) Neumann, L., Wagner, J., Monatsschr. Brau., 27, 137 (1974); Anal. Abstr., 28, 3F48 (1975). (1188) Nissenbaum, A., Lifshitz, A,, Stepek, Y., Lebensm. Wiss. Technol., 7, 152 (1974); Anal. Abstr., 29, 3F14 (1975). (1198) Nose, N., Tanaka, A,, Kobayashi, S.,Suzuki, T., Hoshino, Y., Watanabe, A,, EiseiKagaku, 20, 194(1974); Anal. Abstr., 29, 6F29 (1975). (1208) Oettinger, P. E., Huffman, F., Fine, D. H., Lieb, D., Anal. Lett., 8,411 (1975); Anal. Abstr., 30, 2F14 (1976). (1218) O'Hara, J. R., Chin, M. S.,Dainius, B., Kiibuck. J. H., J. food Sci., 39, 38 (1974). (1228) Otsuka, K.. Zenibayashi, Y . , Agric. Biol. Chem., 38, 1079 (1974); Anal. Abstr., 27, 3618 (1974). (1238) Page, 8. D., Kennedy, 8.P. C., J. Assoc. Off. Anal. Chem., 58, 1062 (1975). (1248) Paradis, M., Ackman, R . G.. J. fish. Res. Board Can., 32, 316 (1975); Chem. Abstr., 83,
4159811 (1975). (1258) Patterson, D. S. P., Roberts, 8. A,, Food Cosmet. Toxicol., 13, 541 (1975); Anal. Abstr., 31, 4F14 (1976). (1268) Pfeilsticker, K., Fabricius, G., Timme, G., Z. Le6ensm.-Unters. forsch., 158, 21 (1975); Chem. Abstr., 83, 41639x (1976). (1278) Pfeilsticker, K., Fabricius, G., Schulte, G., ibid., 155, 263 (1974); Anal. Abstr., 28, 4F33 (1975). (1288) Ponder, C., J. Assoc. Off. Anal. Chem., 57, 919 (1974). (1298) Pons, W. A., Jr., ibid., 58, 746 (1975). (1308) Pons, W. A., Jr., bid., 59, 101 (1976). (1318) Postei, W., Goerg, A,, Brauwissenschaft, 29, 193 (1976); Chem. Abstr., 85, 92287e (1976). (1328) Potthast, K., Mitteilungsbl. GDChfachgruppe Lebensmibelchem. Gerichtl. Chem., 29, 90 (1975); Anal. Abstr., 30, 5F27 (1976). (1338) Potthast, K., Eigner, G., J. Chromatogr., 103, 173 (1975). (1348) Przbylski, W., J. Assoc. Off. Anal. Chem., 58, 163 (1975). (1358) Ranganna, S.,J. Agric. Food Chem., 22, 1139 (1974). (1368) Reiss, J., Mikrochim. Acta, I, 473 (1975); Anal. Abstr., 30, I F 6 (1976). (1378) Reiss, J., Fresenius' Z. Anal. Chem., 275, 30(1975); Anal. Abstr., 30, 2F19 (1976). (1388) Revuelta, D., Revueita, G., Armisen, F., An. Ouim., 71, 503 (1975); Anal. Abstr., 30, I F 2 1 (1976). (1398) Rieve, D., Wermerssen, H., Zimmermann, T., Arch. Lebensmittelhyg., 25, 264 (1974); Chem. Abstr., 83, 263701 (1975). (1408) Roberts, 8. A,, Patterson, D. S. P., J. Assoc. Off. Anal. Chem., 58, 1178 (1975). (1418) Rorner, T. R., ibid., 58, 500 (1975). (1428) Romer, T. R., Campbell, A. D., ibid., 59, 110 (1976). (1438) Rose, H. A,, J. Pharm. Sci., 63, 268 (1974); Anal. Abstr., 27, 2211 (1974). (1448) Rosen. J. D., Pareles, S.R., J. Agric. Food Chem., 22, 1024 (1974). (1458) Rosen, J. D., Morano, J. R., Pareles, S. R., Giacin, J. R., Gilbert, S. G., J. Assoc. Off. Anal. Chem., 58, 700 (1975). (1468) Rutczynska-Skonieczna, E. M., Rocz. Panstw. Zakl. Hig., 24,579 (1973); Anal. Abstr., 27, 2231 (1974). (1478) Rutczynska-Skonieczna, E. M., ibid., 27, 161 (1976); Anal. Abstr., 31, 4F28 (1976). (1488) Ryan, J. J., Dupont, J. A,, J. Assoc. Off. Anal. Chem., 57, 828 (1974). (1498) Ryan, J. J., Dupont, J. A,, J. Agric. Food Chem., 23, 917 (1975). (1508) Ryan, J. J., J. Chromatogr., 127 (I), 1 (1976). (1518) Samarajeewa, U., Arseculeratne, S. N., J. food Sci. Technol., 12, 27 (1975). (1528) Sarudi, I., Jr., Kasa, I., Bajnoczy, G., Dtsch. Lebensm. Rundsch., 72, 96 (1976); Anal. Abstr., 31, 4G5 (1976). (1538) Schafer, M. L., Rhea, U., Peeler, J. T., Hamilton, C. H., Campbell, J. E., J. Agric. Food Chem., 23, 1079 (1975). (1548) Schmidhofer, T., Egli, H.-R., Chimia, 28, 424 (19.74); Anal. Abstr., 28, 4F36 (1975). (1558) Schmidlin-Meszaros, J., Mitt. Geb. Lebensmittelunters. Hyg.? 85, 453 (1974); Chem. Abstr., 84, 42081s (1976). (1568) Seitz, L. M., J. Chromatogr., 104, 81 (1975). (1578) Seitz, L. M., Mohr, H. E., J. Assoc. Off. Ana. Chem., 59, 106 (1976). (1588) Sen, N. P., lyengar, J. R., Donaldson, 8. D. Panalaks, T., Miles, W. F. /ARC Sci. Publ., 9, 49 (1975); Chem. Abstr., 83, 77069a (1975). (1598) Shannon, G. M.. Shotwell, 0. L., J. Assoc. Off. Anal. Chem., 58, 743 (1975). (1608) Shirai, F., Minagawa, K., Takeshita, R., EiseiKagaku, 20, 282 (1974); Anal. Abstr., 29, 6F14 (1975). (1618) Sidhu, J. S.,Muthu. M., Bains, G. S., Pestic. Sci., 6, 451 (1975); Anal. Abstr., 30, 5638 ( 1976). (1628) Siegfried, R., J. Chromatogr., 118, 270 (1976). (1638) Sietz, F. G., fette, Seifen, Anstrichm., 77, 12 (1975); Anal. Abstr., 29, 3F28 (1975). (1648) Skaare, J. U., Dahle, H. K., J. Chromatogr., 111, 426 (1975). (1658) Stack, M. E., Pohland, A. E., J. Assoc. Off. Anal. Chem., 58, 110 (1975). (1668) Stanley, J. B.,Lee, L. S., Cucullu, A. F., deGruy, I. V., J. Agric. Food Chem., 23, 447
ANALYTICAL CHEMISTRY, VOL. 49,
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(1975). (1678) Stephany, R. W., Freudenthai, J., Egmond, E.,Gramberg, L. G., Schuller, P. L., J. Agric. Food Chem., 24, 536 (1976). (168B) Stubblefield, R. D., Shannon, G. M., J. Assoc. Off. Anal. Chem., 57, 852 (1975). (169B) Suzuki, T., Fujimoto, Y.. Hoshino, Y., Tanaka, A,, Agric. Biol. Chem., 38, 1259 (1974); Anal. Abstr., 28, 2G1 (1975). (1708) Suzuki, T., Fujimoto, Y., Hoshino, Y., Tanaka, A., J. Chromatogr., 105, 95 (1975). (1718) Tanaka, A., Fujimoto, Y., Agric. 8iol. Chem., 39, 723 (1975); Anal. Abstr., 29, 5F35 (1975). (1728) Thomas, F., Eppley. R. M., Trucksess, M. W., J. Assoc. Off. Anal. Chem., 58, 114 (1975). (173B) Thorpe, C. W., Johnson, R. L., ibid., 57, 861 (1974). (174B) Trotter, W. J., ibid., 58, 461 (1975). (1758) Trotter, W. J., Young, S. J. V., ibid., p 466 ... (1768) Trucksess, M. W., ibid., 57, 1220 ( 1974). (177B) Trucksess, M. W., ibid., 59, 722 (1976). (1788) Tuinstra, L. G. M. T., Bronsgeest, J. M., J. Chromatogr., 111, 448 (1975). (1798) Van Dooren, P. H., J. Sci. food Agric., 27, 51 (1976). (18OB) Van Gils, W. F., Visser, G., Hidskes, G. G., Z. Lebensm. Unters. Forsch., 158, 285 (1975); Anal. Abstr., 30, 3F13 (1976). (1818) Vasundhara, T. S., Jayaraman. S., Parihar, D. B., J. Chromatogr., 115, 535 (1975). (1828) Velasco, J., J. Assoc. Off. Anal. Chem., 58, 757 (1975). (1838) Velasco, J., Morris, S. L., J. Agric. Food Chem., 24, 86 (1976). (1848) Walker, E. A., Castegnaro. M., Pignatelli, B., Analyst(London), 100, 817 (1975); Anal. Abstr., 30, 6F5 (1976). (185B) Walker, G., Winteriin, W., Fouda, H., Seiber, J., J. Agric. Food Chem., 22, 944 (1974). (186B) Walters, C. L., Fueggle, D. G., Lunt, T. G., /ARC Sci. Pub/., 9, 22 (1975); Chem. Abstr., 83, 112458a (1 975). (1878) Ware, G. M., J. Assoc. Off. Anal. Chem., 58, 754 (1975). (188s) Ware, G. M., Thorpe, C. W., Pohland. A. E., ibid., 57, 1111 (1974). (1898) Wild, R., Dobrovolny, H., Brauwissenschaff, 29, 93 (1976); Anal. Abstr., 31, 4F29 ( 1976). (19OB) Wildanger, W., Z. Lebensm. Unters. Forsch., 158, l(1975); Chem. Abstr., 83, 56818d (1975). (1918) Williams, D. T., J. Assoc. Off. Anal. Chem., 59, 30 (1976). (1928) Williams, D. T., ibid., p 32. (1938) Williams, D. T., Miles, W. F., ibid., 58, 272 (1975). (1948) Wilson, D. M., Tabor, W. H., Trucksess, M. W., ibid., 59, 125 (1976). (195B) Wood, G., Huang, A,, J. Agric. Food Chem., 23, 239 (1975). (1968) Wozniak, J., Tokarz, A,, Rocz. fanstw. Zakl. Hig., 27, 177 (1976); Anal. Abstr., 31, 4F25 (1976). Carbohydrates (IC) Adam, S., Jennings, W. G., J. Chromatogr., 115, 218 (1975). (2C) Anderson, 8. A., Berlin, E.. J. Dairy Sci., 57, 786 (1974). (3C) Andrzejewska, E., Rocz. Panst. Zakl. Hig., 26, 87 (1975); Anal. Abstr., 30, 2F24 (1976). (4C) Arndt, W., Thaler, H.. Mitt. Hoeheren Bundeslehr- Versuchsanst. Wein-Obstbau Kiostenneuburg, 24, 325 (1974); Anal. Abstr., 29, 6F39 (1975). (5C) Artaud, J., Estienne, J., Cas, M., Ann. fals. Expert. Chim., 67, 171 (1974):Chem. Abs.fr., 82. 41906m (1975). (6C) Banks, W., Greenwood, C. T., Muir, D. D., Staerke. 26. 73 (19741 -. , (7C) Bark', L. S., Prachuabpaibui, P., Anal. Chim. Acta, 72, 196 (1974). (8C) Belue, G. P., McGinnis. G. D., J. Chromatogr., 97, 25 (1974). (9C) Birch, G. G., Mwangelwa, 0.M., J. Sci. Food Agric., 25, 1355 (1974). (IOC) Bolling, H., El Baya, A. W., Chem., Mikrobiol., Technol. Lebensm., 3, 161 (1975); Chem. Abstr., 82. 1 6 8 9 2 3 ~(1975). (11C) Bosset, J., Blanc; B., Planner, E., Anal. ~
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Chim. Acta, 77, 171 (1975). (12C) Boxall, L. M., Greenwood, C. T., Mulr. D. D., Lab. fract., 23, 67 (1974); Anal. Abstr., 27, 2217 (1974). (13C) Brobst, K. M., Scobell, N. D., Steele, E. M.. Proc. Annu. Meet. Am. SOC. Brew. Chem., 43 (1973); Anal. Abstr., 28, 5F24 (1975). (14C) Bruijn, J., Carreyet. R. A., Proc. 47th Congr. S. Afr. Sug. Tech. Assoc., 44 (1973); Anal. Abstr., 28, IF9 (1975). (15C) Cerning-Beroard, J., Cereal Chem., 52, 857 (1975). (16C) Chang. J. C., Renoll, M. W., Hansen, P. M. T., J. FoodSci., 39, 97 (1974). (17C) Conrad. E. C., Palmer, K., Food Technol., 30, 84 (1976). (18C) Davies, E., Bourke, E.. Costello, J., Ana/yst (London), 100, 758 (1975). (19C) Della Monica, E. S., Calhoun, M. J., McDowell, P. E., J. FoodSci., 39, 1062 (1974). (20C) Dusic, Z., Acta fharm. Jugoslaw., 25, 35 (1975); Anal. Abstr., 29, 2C21 (1975). (21C) Dusic, Z., Berka, A,. ibid., p 43; Anal. Abstr., 29, 2C22 (1975). (22C) Endean, M. E., Sci. Technol. Surv.-Br. food Manuf. lnd. Res. Assoc., 83, (1973); Chem. Abstr., 82, 1 5 3 8 5 0 ~(1975). (23C) Filippov, M. P., Kohn, R., Chem. Zvesti, 29, 88 (1975): Anal. Abstr., 29, 3F9 (1975). (24C) Finley, J. W., Olson, A. C., CerealChem., 52, 500 (1975). (25C) Fitzpatrick, T. J.. Osman, S. F., Am. Potato J., 51, 318 (1974). (26C)Fleming,M., Manners, D. J., Jackson, R. M., Cooke, S. C., J. lnst. Brew., London, 80, 399 (1974); Anal. Abstr., 28, 4F44 (1975). (27C) Ghebregzabher. M., Rufini, S., Monaldi, B., Lato, M., J. Chromatogr., 127, 133 (1976). (28C) Hansen, S. A,, ibid., 105, 388 (1975). (29C) lbid., 107, 224 (1975). (30C) Havlicek, J., Samuelson, O., Anal. Chem., 47, 1854 (1975). (31C) Havlicek, J., Samuelson, O., J. lnst. Brew., London, 81, 466 (1975); Anal. Abstr.. 30, 5F47 (1976). (32C) Hellendoorn, E. W., Noordhoff, M. G., Slagman, J., J. Sci. FoodAgric., 26, 1461 (1975). (33C) Herb, S. F., Fitzpatrick, T. J., Osman, S. F.. J. Agric. food Chem., 23, 520 (1975). (34'2) Holst, D. O., Gehrke, C. W., J. Assoc. Off. Anal. Chem., 58, 474 (1975). (35C) Hudson, G. J., John, P. M. V., Bailey, B. S., Southgate, D. A. T., J. Sci. Food Agric., 27, 681 (1976). (36C) International Commission for Uniform Methods of Sugar Analysis, c/o British Sugar Corp. Ltd., Peterborough, Cambs. (1975). (37C) Iwata, Y., Sasaki, Y., Origuchi, K., Kojima, A., Nippon Shokuhin Kogyo Gakkai-Shi, 20, 60 (1973); Chem. Abstr., 84, 420941, (1976). (38C) Jelaca, S. L., Zb. frir. Nauke, Matica Srp., 45, 119 (1973); Chem. Abstr., 82, 1538689 (1975). (39C) Kainuma, K., Nogami, A., Mercier, C., J. Chromatogr., 121, 361 (1976). (40C) Kamiyama, Y., Sakai, Y., Agric. Bo/. Chem., 38, 2385 (1974). (41C) Keijbets, M. J. H., Pilnik, W., Potato Res., 17, 169 (1974); Chem. Abstr., 81, 118611a (1974). (42C) Klitzing, L. von, G-1-TFachz. Lab., 18, 107 (1974); Anal. Abstr., 27, 2728 (1974). (43C) Klostermeyer. H., Popp, U., Schmitz. I., 2. Lebensm.-Unters.-Forsch., 158, 31 (1975). (44C) Klostermeyer, H., Popp, U., Reimerdes, E.-H., ibid., p 73. (45C) Korsrud, G. O., Trick, K. D., Can. lnst. Food Sci. Technol. J., 9, 92 (1976); Chem. Abstr., 85, 45004a (1976). (46C) Kubadinow, N., Zucker, 27, 72 (1974); Anal. Abstr., 28, 3F19 (1975). (47C) Lawrence, J. G., Chimia, 29, 367 (1975); Anal. Abstr., 30, 3'212 (1976). (48'2) Lee, D. E., Lillibridge, C. B., Brown, C. S., Dreschsler, K., Fromme, B., Am. J. Clin. Nutr., 29, 428 (1976). (49C) Linden, J. C., Lawhead, C. L., J. Chromatogr., 105, 125 (1975). (50C) Malec, K., Szuchnik, A,, Rydel, S., Walerianczyk, E., Z. Zucklnd., 100, 502 (1975); Anal. Abstr.. 31. 4G3 (1976). (51C) Martelli; A., Proserpio. G., Sci. Techno/. Alimenti, 3, 367 (1973); Chem. Abstr., 84, 162973f f' 19761. (52C) Matulewicz, M. C., Cerezo, A. S., J. Sci. Food Agric., 26, 243 (1975)
ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
(53C) McConnell, A. A., Eastwood, M. A,, ibid., 25, 1451 (1974). (54C) McCready, R. M., Ducav. E. D.. Carbohvd. Res., 28, 100 (1973). (55C) Moll, M., Flayeux, R., Lehuede, J.-M., Bios, France, 6, 94 (1975); Anal. Abstr., 29, 5F44 (1975). ' (56C) Morrison, I. M., J. Chromatogr., 108, 361 (1975). (57C) Nedelcheva, M., Stoilkov, G., Popova. S., Staerke, 27, 298 (1975). (58C) Nickerson. T. A,, Vujicic, i. F., Lin, A. Y., J. Dairy Sci., 59, 386 (1976). (59C) Nurok, D., lnt. Sugar J., 76, 305 (1974). (60C) Nurok, D., J. Chromatogr., Sci., 14, 305 I 1976). ' (61C) Palmer, J. K., Anal. Lett., 8, 215 (1975); Anal. Abstr., 29, 5F16 (1975). (62C) Patil, N. B., Bhide, S. V., Kale, N. R., Carbohyd. Res., 29, 513 (1973). (63C) Perschak, F., Zucker, 28,357(1975); Anal. Abstr., 30, 6F8 (1976). (64C) Petersen, J., British Patent 1,371,637; (1971); Anal. Abstr., 28, 4D27 (1975). (65C) Rabinowitz, M. P., Reisberg, P., Bodis, J. I., J. fharm. Sci., 63, 1601 (1974). (66C) Ramnas, O., Samuelson, O., Acta Chem. Scand., Ser. 8. 28, 955 (1974); Anal. Abstr., 28, 5C15 (1975). (67C) Rapp, A., Bachmann, O., Ziegler, A,. Deut. Lebensm-Rundsch., 71. 345 (1975). (68C) Richards, G. N., Stokie, G., lnt. Sugar J., 76, 103 (1974). (69C) Romano, A . T., Clin. Chem., (WinstonSalem, N.C.), 19, 1152 (1973). (70C) Rozovskii, G. I., Talalene, D., Jankauskas, R., Zh. Anal. Khim., 29, 2243 (1974); Anal. Abstr., 29, 5C16 (1975). (71C) Sanyal, M., Rao, V. S.,De, K. B., Fresenius' Z.Anal. Chem., 271, 208 (1974); Anal. Abstr., 28, 4C17 (1975). (72C) Sanyal, M., Staerke, 27, 263 (1975). (732) Sarris. J., Vijayalakshmi, M. A,, Latrasse, A., ind. Aliment. Agric., 92, 1265 (1971); Chem. Abstr.. 84. 1 4 9 3 1 4 ~(19761. (74C) Scholze, D., Lebensmittel-lnd., 21, 255 (1974). Anal Abstr. 29. 3F5 (19751 (75C) Schwarz, G. W.G.,~Fresenius' Z. Anal. Chem., 271, 31 (1974); Anal. Abstr., 28, 6C71 (1975). (76C) Stein, E. R., Brown, H. E., J. Agric. food Chem., 23, 526 (1975). (77C) Tanaka, M., Thananunkul, D., Lee, T.-Ch., Chichester, C. D., J. FoodSci., 40, 1087 (1975). (78C) Tipson, R. S., Advances in Carbohydrate Chemistry and Biochemistry, vol. 30, New York, Academic Press, 1974. (79C) Tomisek, A. J., Natelson, S., Microchem. J., 19, 54 (1974). (8OC) Torii, M., Sakakibara, K., J. Chromatogr., 96, 255 (1974). @IC) Usov, A. I., Yarotskii, S. V., lzw. Akad. Nauk SSSR, Ser. Khim., 877 (1974); Anal. Abstr., 27, 3340 (1974). (82C) Walborg, E. F., Jr., Kondo, L. E., Robinson, J. M., Methods Enzymol., 8,41, 10 (1975); Anal. Abstr., 31, ID31 (1976). (83C) Wood, P. J., Siddiqui, I. R., Weisz, J., Carbohyd. Res., 42, l(1975). (84C) Yamanaka, K., Agric. Bioi. Chem., 39, 2227 (1975); Anal. Abstr., 30, 6F10 (1976). (8%) Zadow, J. G., Sv. fapperstidn., 78, 376 (1975); Anal. Abstr., 31, IC51 (1976). (86C) de Zeeuw, R. A., Dull, G. C., J. Chromatogr., 110, 279 (1975). (87C) Zuercher, K., Hadorn, H., Deut. LebensmRundsch.. 70, 425 (1974). (88C) lbid., 71, 68 (1975). (89C) Zuercher, K., Hadorn. H., Stack, C., ibid., p 393. (9OC) Zuercher, K., Hadorn, H., Stack, C., Miff. Geb. Lebensmittelunters. Hyg., 66, 92 (1975). \
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Color
(ID) Adams, J. B., Butler, R., Analyst(London), 101, 140 (1976). (2D) Andrzejewska, E., Rocz. fanstw. Zakl. Hig., 26, 575 (1975); Chem. Abstr., 84, 88063r (1976). (3D) Bailey, J. E., Calvey, R . J., J. Assoc. Off. Anal. Chem., 58, 1087 (1975). (4D) Bailey, J. E., Cox, E. A,, ibid., p 609. (5D) lbid., 59, 5 (1976). (6D) Banerjee, T. S., Guha, K. C., Saha, A,, Roy, B. R., J. FoodSci. Technol., 11, 230 (1974). (7D) Bell, S., J. Assoc. Off. Anal. Chem., 58, 717
(1975). (8D) lbid., 57,961 (1974). (9D) Chelkowski, J., Czarnecki, Z., Przem. SDOZYW.,28, 117 (1974); Chem. Abstr., 82,845513 (i975). (10D) Dantzman, J., Stein, C., J. Assoc. Off. Anal. Chem., 57,963 (1974). (11D) De Clercq, H., Massart. D. L., J. Chromatogr., 93,243 (1974). (12D) Dixon, E. J., Groffman, D. M., Analyst (London), 100,476 (1975). (13D) Draper, R. E., J. Assoc. Off. Anal. Chem., 58,614 (1975). (14D) Dujardin, E., Fouassin, A,, Degraeve, H., Rev. Ferment. lnd. Aliment., 30,63 (1975); Chem. Abstr., 85, 19147e (1976). (15D) Eagerman, B. A,, Clydesdale, F. M., Francis, F. J., J. FoodSci., 38, 1051 (1974). (16D) lbid., p 1056. (17D) Farre Rovira, R.. Circ. Farm., 33, 493 (1975); Chem. Abstr., 84, 149362m (1976). (18D) Fratz, D. D., J. Assoc. Off. Anal. Chem., 59, 578 (1976). (19D) Graichen, C., ibid., 58, 278 (1975). (20D) Hammond, E. G., Chang. J., Reinbold, G. W., J. Dairy Sci., 58, 1365 (1975). (21D) Honkawa, T., Anal. Lett., 8,901 (1975). (220) Hrazdina, G., Le6ensm.-Wiss. Technol., 8, 111 (1975). (23D) Kapei, M., Karunanithy, R., Analyst (London), 99,661 (1974). (24D) Kenmochi, K., Katayama, O., Yoshikawa, S., Nippon Shokuhin Kogyo Gakkal-Shi, 20, 16 (1973); Chem. Abstr., 83, 1124789 (1975). (25D) Kimura, S., Ishitani, T., Umeda, K., Tsubata, K., Takai, J., Nippon Shokuhin Kogyo Gakkai-Shi, 19, 299 (1972); Chem. Abstr., 83, 145965s (1975). (26D) Kramer, A., Food Technol., 30, 62 (1976). (27D) Lehmann, G., Moran, M.. Neumann. B., Z. Lebensm.-Unters.-Forsch., 155,85 (1974). (28D) Maniey. C. H., Shubiak, P., Can. lnst. Food Sci. Technol. J., 8, 35 (1975). (29D) Marmion, D. M., J. Assoc. Off. Anal. Chem., 58, 50 (1975). (30D) lbid., p 719. (31D) Massart, D. L., De Clercq, H., Anal. Chem., 46, 1988 (1974). (32D) Montedoro, G., Fantozzi, P., Le6ensm.Wiss. Technol., 7, 155 (1974). (33D) Mueller-Mulot, W., Fette, Seifen, Anstrichm., 78, 18 (1976). (34D) Palamidis. N., Markakis, P., J. Food Sci., 40, 1047 (1975). (35D) Panov, I., Donchev. Kh.. Tr. Vissh. lnst. Nar. StoD., Varna, 44, 146 (1972); Anal. Abstr., 28,5F19 PassarelIi, R. J., J. Chromatogr. Sci., 153 (1975). (37D) Pearson, D., J. Assoc. Public Anal., 13, 103 1197!i\ (38D) Powell, F. E., Snowden, C. J., Analyst (London), 100,503 (1975). (39D) Puech, A. A,, Rebeiz, C. A,, Catlin, P. B., Crane, J. C., J. Food Scl., 40,775 (1975). (40D) Rizvi, S. R. H., Sci. lnd. (Karachi), 9,226 (1972); Chem. Abstr., 81, 150576d (1974). (41D) Ross, K. D., J. Agric. FoodChem., 23,475 (1975). (42D) Sarkar, S. K., Howarth, R. E., ibid., 24,317 (1976). (430) Shrikhande, A. J., CRC Crit. Rev. Food Sci. Nutr., 7, 193 (1976). (44D) Shrikhande, A. J., Francis, F. J., J. Food Sci., 38,649 (1974). (45D) Sinah, M., J. Assoc. Off. Anal. Chem., 58, 48 (1975). (46D) Strack, D., Mansell, R. L., J, Chromatogr., 109,325 (1975). (47D) Takeo. T., JARQ, 8, 159 (1974); Chem. Abstr., 82, 153884) (1975). (48D) Terashita, T., Kono, M., Kinki Daigaku Nogakubu Kiyo, 9, 37 (1976); Chem. Abstr., 85, 45007d (1976). (490) Tewari, S.N., Sharma, S. C., Sharma, V. K., Fresenlus'Z. Anal. Chem., 269, 128 (1974). (500) Tewari, S. N., Sharma, S. C., Sharma, V. K., Chromatographia, 7, 308 (1974); Anal. Abstr., 28,2F26 (1975). (51D) Tewari, S. N., Sharma, S.C., Sharma, I. C., ibid., p 84; Anal. Abstr., 27,2235 (1974). (52D) Tomas, F., Pastor, R., Carpena, O., Rev. Agroquim. Tecnol. Aliment., 13,554 (1973); Chem. Abstr., 81, 103311d (1974). (53D) Watada, A. E., Norris, K. H.. Worthington, I . - .
J. T., Massie, D. R., J. FoodSci., 41,329 (1976). (54D) Wittmer, D. P., Nuessle, N. O., Haney, W. 'G., Anal. Chem., 47, 1422 (1975). (55D) Woeldecke, M., Herrmann, K., 2. Lebensm-Unters.-Forsch., 155, 151 (1974). (56D) Wolfrom. M. L., Kashimura, N.. Horton, D., J. Agric. FoodChem., 22,791 (1974). (57D) Zhuchenko, A. A., Andryushchenko, V. K., Fainshtein, 2. R., Vyrodova. A. P., Fiziol. Biokhim. Kul't. Rast., 6, 434 (1974); Chem. Abstr., 81, 1 3 4 7 0 4 ~(1974).
Enzymes (IE) Barnes, W. C., Blakeney. A. B., Staerke, 26, 193 (1974). (2E) Berger, M., Grandvoinet, P., De la Gueriviere, J. F., Bussiere, G., Seck, A. S., Gerard, R., Ann. Technol. Agric., 23,233 (1974); Chem. Abstr., 83, 41599j (1975). (3E) Bruemmer, J. M., Getreide, Mehi Brot, 28, 57 (1974); Chem. Abstr., 81, 1 1 8 6 0 2 ~(1974). (4E) Castberg, H. B., Solberg, P., Egelrud, T., J, Dairy Res., 42,247 (1975). (5E) Colas, A., Ann. Technol. Agrlc., 23, 241 (1974): Chem. Abstr., 83,26371k (1975). (6E) Cubadda, R., Quattrucci, E., J. Sci. Food Agr., 25,417 (1974). (7E) Davidek, J., Egertova, J., Seifert, J., 2.Lebensm-Unters-Forsch., 156,263 (1974). (8E) Davidek, J., Herman, P., Seifert, J., Milchwissenschaft., 31, 76 (1976); Chem. Abstr., 84, 1 4 9 3 2 6 ~(1976). (9E) DeKoning, P. J., Mondo Latte, 28, 647 (1974); Chem. Abstr., 83,26369r (1975). (10E) Edwards, R. A., Faraji-Haremi, R., Wootton, M., J. Apic. Res., 14,47 (1975); Anal. Abstr., 30, 4F14 (1976). (1 1E) Egberg, D. C.. Potter, R. H., Honold. G. R., J. Agric. Food Chem., 23,603 (1975). (12E) Elstner, E. F., Heupel, A,, Anal. Biochem., 70,616 (1976). (13E) Jeffers, H. C.. Rubenthaler, G. L., Cereal Chem., 51, 772 (1974). (14E) John, M., Schmidt, J., Dellweg, H., Mschr. Brau., 28, 14 (1975); Anal. Abstr., 29, 4F35 (1975). (15E) Johnson, N. C., Phillips, D. P., CerealSci. Today, 19,18 (1974). (16E) Kahnt, W.-D., Mundy, V., Grosch, W.. Z. Lebensm.-Unters.-Forsch., 158,77 (1975). (17E) Kaisar, K.-P., Bruhn, L. C., Belltz. H.-D., ibid., 154,339 (1974). (18E) Kiseleva, L. V., Nariniyants, G. R., Tr., Vses. Nauchno-lssled. lnst. Konservn. Ovoshchesush. Prom-sti., 21, 14 (1974); Chem. Abstr., 82,168926~ (1975). (19E) Krop, J. J. P., Pilnik. W., Faddegon, J. M., Le6ensm.-Wiss. Technol., 7, 50 (1974). (20E) Kruger, J. E., Cereal Chem., 53, 796 ( 1976). (21E) O'Leary, P. A,, Fox, P. F., J. DairyRes., 41, 381 (1974). (22E) Park, K. H., Duden, R., Fricker, A,, Z. Le6ensm.-Unters.-Forsch., 157,327 (1975). (23E) Preston, K. R., Cereal Chem., 52, 451 (1975). (24E) Rackis, J. J., McGhee, J. E., Liener, I. E.. Kakade, M. L., Puski, G., Cereal Sci. Today, 19,513 (1974). (25E) Regula, E., Kohn, M., Wassermann, L., Lebensm.-Wiss. Technol., 7, 57 (1974). (26E) Schiemann, D. A , , Brodsky, M. H., J. Milk Food Technol., 39, 191 (1976); Chem. Abstr., 84, 149365q (1976). (27E) Schmid, P., 2.Le6ensm.-Unters.-Forsch., 157,23 (1975). (28E) Siegenthaler, U., Mitt. Geb. Lebensm.Unters.-Hyg., 66,393 (1975).
Fats, Oils, and Fatty Acids (1F) Ackman, R. G., Eaton, C. A,, Sipos, J. C., Tech. Rep. Fish Mar. Sew. Can., 577,(1975); Anal. Abstr., 31, 1F39 (1976). (2F) Ackman, R. G., Hooper, S. N., J. Chromatogr. Sci., 12, 131 (1974). (3F) Andrzejewska. E., Rocz. Panstw. Zakl. Hlg., 26, 87 (1975); Chem. Abstr., 83,7303y (1975). (4F) Armengol, J., Gasull, E., Marques, J., An. Bromatol., 26,357 (1974) (5F) Bandyapadhyay, G. K., Dutta, J., J. Chromatogr., 114,280 (1975). (6F) Baragli, S., Lotti, G., Rlv. SOC./tal. Sci. A/;ment, 4, 251 (1975); Chem. Abstr., 84, 88214r (1976).
(7F) Barthel, G., Laskawy, G., Grosch, W., Deut. Le6ensm.-Rundsch., 70,201 (1974); Anal. Abstr., 28. 2F20 (19751. ~, (8F) Bende, E., Szabo, A,, Somogyi, V., Sutoipar, 21, 164 (1974); Chem. Abstr., 83,263684 (1975). (9F) Brixius, L., Treiber, H., Fette, Seifen, Anstrichm., 76,83 (1974). (1OF) Capella, P., Lercker, G., Conte, L. S., Riv.Sci., Technol. Alimenti Nutr. Um., 5, 235 (1975); Chem. Abstr., 84,88044k (1976). (11F) Chobanov, D., Tarandjiska, R., Chobanova, R., J. Am. Oil Chem. SOC.,53,48 (1976). (12F) Conacher, H. B. S., J. Assoc. Off. Anal. Chem., 58,488 (1975). (13F) Conacher, H. B. S.,Chadha, R. K., J. Assoc. Off. Anal. Chem., 57, 1161 (1974). (14F) Conway, E. S., Adams, M., J. Assoc. Off. Anal. Chem., 58, 23 (1975). (15F) Deeth, H. C., Fitz-Gerald, C. H., Wood, A. F., Aust. J. Dairy Technol., 30, 109 (1975); Chem. Abstr., 84, 1 1 9 9 9 1 (1976). ~ (16F) Doeden, W. G., J. Am. Oil Chem. SOC., 52, 124 (1975). (17F) Dutton, H. J., ibid., 51, 407 (1974). (18F) Ellis, R.. Wong, N. P., ibid., 52, 252 (1975). (19F) Falbe, J., Weber, J., MethodChlm., 1, 970 (1974); Chem. Abstr., 83,26352e (1975). (20F) Farnell, P. J., Analyst (London), 100,661 (1975). (21F) Foglia, T. A., Heller, P., Dooley, C. J., J. Am. Oil Chem. SOC., 53,45 (1976). (22F) Folstar, P., Pilnik, W., De Heus, J. G.. Van der Plas, H. C., Lebensm. Wiss. Technol., 8, 286 11975). > (23F) Folstar, P., Pilnik, W , De Heus, J. G.. Van der Plas, H. C., Mitt. Geb. Lebensmittelunters. Hyg., 66.502 (1975). (24F) 'Franzke, C., Noske, H.-J., Poth, B., Nahrung, 19, 595 (1975); Anal. Abstr., 30,2G12 (1976). (25F) Freeman, I. P., Chem. lnd. (London), 623 (1974). (26F) Fricker, A., Koller, W. D., Fette, Seifen, Anstrichm., 76,466 (1974). (27F) Grosch. W., Z. Le6ensm.-Unters-Forsch, 157,70 (1975). (28F) Hadorn, H., Zuercher, K., Deut. Lebensm.Rundsch., 70, 57 (1974); Anal. Abstr., 27, 2237 (19741 -. (29F) Hassel, R. L., J. Am. OilChem. Soc., 53, 179 (1976). (30F) Haworth, D. T., Kahn, D. R., Lemm, A. W., Hoffman, N. E., Bioinorg. Chem., 4, 303 (1975); Anal. Abstr., 30,3F40 (1976). (31F) Hollo, J., Kurucz, E., Biacs, P., Erdelyt, A,, Elelmiszervizsgalati Kozl., 20, 257 (1974); Chem. Abstr., 83,41703p (1975). (32F) Iverson, J. L., J. Assoc. Off. Anal. Chem., 57,934 (1974). (33F) Jaeger, H., Kloer, H. U., Ditschuneit, H., J. LipidRes., 17, 185 (1976). (34F) Jirousova, J., Nahrung, 19,319 (1975). (35F) Johnson, C. B., Wong, E., J. Chromatogr., 109,403 (1975). (36F) Jong, K. de, Begemann, W. J., J. Am. Oil Chem. Soc., 51,360 (1974). (37F) Karleskind, A., Valmalle, G., Chemin, S., Rev. Fr. Corps Gras, 23, 147 (1976); Chem. Abstr., 85,31689r (1976). (38F) Katayama, M., Hou, C. T., Chen, N. C., Hirota, T., Kiribuchi, T., Funahashi, S., Agric. B i d . Chem., 38, 1661 (1974). (39F) Ke, P. J., Ackman, R. G., Hooper, D. L., Anal. Chim Acta, 78,470 (1975). (40F) Keen, A. R., Walker, N. J., J. DailyRes., 41, 397 (1974). (41F) Kimura, T., Iwse, H., Jpn. Anal., 22, 872 (1973); Anal. Abstr., 27,3342 (1974). (42F) Kiuchi, K., Ohta, T., Ebine, H.. J. Chromatogr. Sci., 13,461 (1975). (43F) Kiuru. K., Leppanen, R., Antila, M., Fette, Seifen, Anstrlchm., 76,401 (1974). (44F) Koch, J., Figge, K., Deut. Lebensm.Rundsch., 71, 170 (1975); Anal. Abstr., 29,6Fl1, ( 1975). (45F) Koman, V., Oanielova, E., Chem. Zvesti, 28, 218 (1974); Anal. Abstr., 27,3622 (1974). (46F) lbid., 29,256 (1975). (47F) Kopecky, A., Milchwissenschaft, 31,224 (1976); Chem. Abstr., 85,450091 (1976). (48F) Kundu, M. K., Pokorny, J., Janicek, G., Nahrung, 18, 309 (1974); Chem. Abstr., 81, 1 3 4 8 0 2 ~(1974). (49F) Leu, K., Anderson, J., Lebensm. Wlss. Technol., 7,42 (1974). ~~
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(95F) Weisser, H., Lefebvre, J., Oleagineux, 31, (50F) MacPherson, J. K., Buckee, G. K., J. lnst. (39G) lbid., p 295; Anal. Abstr., 31, 4F33 Brew., 80, 540 (1974); Anal. Abstr., 29, IF55 27 (1976); Chem. Abstr., 85, 191569 (1976). (1976). (96F) Weisz, H., Mikrochim. Acta, II, 519 (1975); (1975). (40G) Jolly, R. C., Kosikowski, F. V., J. Agric. (51F) Maia, G. A,, Brown, W. H., Whiting, F. M., Anal. Abstr., 30, 5F62 (1976). FoodChem., 23, 1175 (1975). Stull, J. W., J. FoodSci., 41, 190 (1976). (97F) Wortberg, B., 2. Le6ensm.-Unters-Forsch., (41G) Kemp, T. R., Knavel, D. E., Stoitz, L. P., 157, 333 (1975). (52F) Melchert, H.-U., Deut. Le6ensm.-Rundsch., ibid., 22, 717 (1974). 71, 400 (1975); Anal. Abstr., 30, 5F64 (1976). (98F) Wurziger, J., Fette, Seifen, Anstrichm., 78, (42G) Kleber, W., Hums, N., Brauwelt, 114,414 (53F) Morrison, W. R., Mann, D. L., Soon, W., 172 (1976). (7974); Anal. Abstr., 28, 4F45 (1975). Coventry, A. M., J. Sci. Food Agric., 26, 507 (43G) Korolczuk, J., Daniewski, M,, Mielniczuk, (99F) Ziegenhorn, J., Clin. Chem. (Winston(1975). Z., J. Chromatogr., 100, 165 (1974). Salem, N.C.), 21, 1627 (1975). (54F) Moura Fe, J. A., J. Sci. FoodAgric., 26, 523 (44G) Knowles, M. E., Gilbert, J., McWeeny, D. (IOOF) Zuercher, K., Mitt. Geb. Lebensmittelun(1975). J., J. Sci. FoodAgric., 26, 189 (1975). ters. Hyg., 65, 90 (1974). (55F) Murata, T.,'Takahashi, S., Takeda, T.. Anal. (45G) Lee, C. Y., Acree, T. E., Butts, R. M., Anal. Flavors and Volatile Compounds Chem., 47, 573 (1975). Chem., 47, 747 (1975). (46G) Lee, K-R, Suzuki, T., Kobashi, M., Hase(56F) lbid., p 577. (IG) Abraham, K. O., Shankaranarayana, M. L., (57F) Myher, J. J., Kuksis, A., J. Chromatogr. Sci., Raghavan, B., Natarajan, C. P., Mikrochim. Acta, 1, gawa, K., Iwai, K., J. Chromatogr., 123, 119 13, 138 (1975). 11 (1976); Chem. Abstr., 84, 88070r (1976). (1976). (58F) Myher, J. J.. Kuksis, A,, Lipids, 9, 382 (2G) Acree. T. E., Lee, C. Y., Butts, R. M., Bar(47G) Lee, P. L., Swords, G., Hunter, G. L. K., J. (1974). nard, J., J. Agric. Food Chem., 24, 430 (1976). FoodSci., 40, 421 (1975). (59F) Ohlson, R., Podlaha, O., Toregard, B., Fette, (3G) Ananthakrishna, S. M.. Govindarajan, V. S., (48G) Lehmann, G., Neumann, B., Z. Le6ensm.Seifen, Anstrichm., 77, 263 (1975). Lebensm. Wiss. Technol., 7, 220 (1974). Unters. Forsch., 156, 32 (1974). (60F) Okabe, A,, Katayama, T., Kanemasa, Y., (4G) Andre, L., Mile, L., Acta Aliment Acad. Sci. (49G) Lopez, A. S., Queshel, V. C., J. Sci. Food Acta Med. Olayama, 28,403 (1974); Biol. Abstr., 60, Hung., 4, 113 (1975); Chem. Abstr., 83, 1300881 Agric., 27, 85 (1976). 6221 (1975). (1975). (50G) Maga, J. A., CRCCrit. Rev. FoodSci. Nutr., (61F) Pantulu, P. C., Rao, M. R., Rao, D. S., An(5G) Brenner, M. W., Khan, A. A,, J. lnst. Brew., 8, l(1976). antakrishnan, C. P., Milchwissenschaft, 30, 735 80, 544 (1974); Anal. Abstr., 29, IF57 (1975). (51G) Martin, G. E., Buscemi, P. C., Butts, B. B., (1975); Chem. Abstr., 84, 88053n (1976). (6G) Buttery, R. G., Seifert, R. M., Ling, L. C., J. J. Assoc. Off. Chem., 58, 582 (1975). (62F) Parodi, P. W., J. Chromatogr., 111, 223 Agric. FoodChem., 23, 516 (1975). (52G) Martin, G. E., Dyer, R. H., Buscemi, P. C., 11975\ . . -,. (7G) Buttery, R. G., Guadagni, D. G., Ling, L. C., ibid., 57, 610 (1974). (63F) Patterson, G. W., Khalil, M. W., Idler, D. R., Seifert, R. M.. Lipton, W., ibid., 24, 829 (1976). (53G) Masada, Y., Inoue, T., Hashimoto, K., FuJ. Chromatogr., 115, 153 (1975). (8G) Buttery, R. G., Guadagni, D. G., Ling, L. C., jioka, M., Uchino, C., lnt. Congr. Essent. Oils, 97 (64F) Pearson, D., J. Assoc. Pub. Anal., 12, 73 ibid., p 419. (1974); Chem. Abstr., 84, 1 0 3 9 9 2 ~(1976). (1974). (9G) Casimir, D. J., Moyer, J. C., Mattick, L. R., (54G) Masuda. H., Muraki, H., J. Sci. FoodAgric., (65F) Peers, K. E., Chem. lnd. (London), 455 J. Assoc. Off. Anal. Chem., 59, 269 (1976). 26, 1027 (1975). (1974). (IOG) Casteele, K. V., DePooter, H., Van Sumere, (55G) Matheson, N. A., Anaiyst (London),99,577 (66F) Perkel, R. L., Malamud, N. L., Dmitrieva, 2. C. F., J. Chromatogr., 121, 49 (1976). (1974). G., Gorshkova, E. I.,Chebotareva, G. V., Krotova, L. (11G) Charalambous, G., Bruckner, K. J., Hard(56G) Merat, E., Vogel, J., Mitt. Geb. LeV., Tr. Vses. Nauch. lssled. lnst. Zhirov, 30, 45 wick, W. A,, Linneback, A,, Tech. Quart. Master bensmittelunters. Hyg., 66, 496 (1975). (1973); Cbem. Abstr., 82, 1 6 8 9 3 0 ~(1975). Brew. Assoc. Am., 11, 150(1974); Anal. Abstr., 28, (57G) Merritt, C., Jr., Robertson, D. H., Cavag(67F) Pettinati, J. D., Swift, C. E., J. Assoc. Off. 6F28 (1975). naro, J. F., Graham, R. A,, Nichols, T. L., J. Agr. Food Anal. Chem., 58, 1182 (1975). (12G) Chen, E. C.-H., David, J. J., J. Sci. Food Chem., 22, 750 (1974). (68F) Punwar, J. K., ibid., p 804. Agric., 25, 1381 (1974). (58G) Molina, P., Soler, A,, Cambronero, J., An. (69F) lbid., 59, 46 (1976). (13G) De Cleyn, R., Verzele, M., ChromatograBromatol., 25, 403 (1973); Chem. Abstr., 81, (70F) Purr, A,, Gordian, 75, 268 (1975); Chem. phia, 8, 342 (1975). 1505652 (1974). Abstr., 84, 42078w (1976). (14G) De Jong, K., Begemann, W. J., J. Am. Oil (59G) lbid., 26, 51 (1974). (71F) Randall, E. L., J. Assoc. Off. Anal. Chem., (60G) Moll, M., Flayeux. R., Lehuede, J-M, Bios, Chem. SOC., 51,360 (1974). 57, 1165 (1974). (15G) Deki, M., Yoshimura, M., Chem. Pharm. France, 6, 90 (1975); Anal. Abstr., 29, 5F48 (72F) Sandra, P., Verzele, M., J. lnst. Brew., 81, Bull., Tokyo, 22, 1748 (1974); Anal. Abstr., 28, 3F49 (1975). 302 (1975); Anal. Abstr., 30, 3F35 (1976). (61G) Moshonas, M. G., Shaw, P. E., ht. Flavours (1975). (73F) Schaap, J. E., Rutten, G. A.M., Ned. Melk (16G) Deki, M., Yoshimura, M., ibid., p 1754. Food Addit., 6, 133 (1975); Chem. Abstr., 83, Zuiveltijdschr., 28, 166 (1974). 130122r (1975). (17G) lbid., p 1760. (74F) Schmid, M. J., Fette, Seifen, Anstrichm., (62G) Mussche, R., J. lnst. Brew., 80, 577 (1974); (18G) lbid., 23, 1374 (1975); Chem. Abstr., 83, 78, 35 (1976). 77098j (1975). Anal. Abstr., 29, 1F58 (1975). (75F) Scholfield, C. R.. J. Am. Oil Chem. SOC., (63G) ibid., 81, 12 (1975); Anal. Abstr., 29,3F20 (19G) DiCecco, J. J., J. Assoc. Off. Anal. Chem., 52, 36 (1975). (1975). 59, l(1976). (76F) Schouten, L., Deut. Lebensm.-Rundsch., (64G) Nambudiri, E. S.. Mathew, A. G., Krish(20G) Drawert, F., Beier, J., Chromatographia, 70, 319 (1974); Anal. Abstr., 28, 5F31 (1975). namurthy, N., Lewis, Y. S., lnt. Flavours FoodAddit., 7, 273 (1974); Anal. Abstr., 28, 2F32 (1975). (77F) Selke, E., Rohwedder, W. K., Dutton, H. J., 6, 135 (1975); Anal. Abstr., 29, 5F27 (1975). (21G) Drawert, F., Schreier, P., Scherer, W., Z. J. Am. Oil Chem. Soc., 52, 232 (1975). Le6ensm.-Unters.-Forsch., 155, 342 (1974). (65G) Nanjo, M., Guilbauit, G. G., Anal. Chim. (78F) Sen Gupta, A. K., Z. Le6ensm.-UntersActa., 75, 169 (1975). (22G) Dubois. P., Brule, G., Rigaud, J.. Dekimpe, Forsch., 158, 71 (1975). J., Technol. Aliment. (Buenos Aires), 6, 12 (1972); (66G) Nguyen T. T., Yamanishi, T., Agric. Biol. (79F) Sheppard, A. J., Hubbard, W. D., Prosser, Chem., 39, 1263 (1975). Chem. Abstr., 82, 41971d (1975). A. R., J. Am. OilChem. SOC., 51, 416 (1974). (67G) Parker, R. G., J. Assoc. Off. Anal. Chem., (23G) Dumont, J. P., Pradel, G., Roger, S., Adda. (8OF) Sheppard, A. J., Iverson, J. L., J. Chroma57, 954 (1974). J., Lait, 56, 18 (1976). togr. Sci., 13, 448 (1975). (68G) Parliment, T. H., Kolor, M. G., J. Food Sci., (24G) Dupuy, H. P., Fore, S. P., Rayner, E. T., J. (81F) Shustanova, L. A,, Khim. Prir. Soedln., 655 Am. Oil Chem. SOC., 52, 118 (1975). 40, 762 (1975). (1974); Chem. Abstr., 82, 1 1 0 3 6 5 ~(1975). (69G) Persson, T., Von Sydow, E., ibid., 39, 537 (25G) Filthuth, D., Gordian, 74, 364 (1974); Anal. (82F) Sims. R. J., Fioriti, J. A,, J. Am. OilChem. ( 1974). Abstr., 29, 5F20 (1975). Soc., 52, 144 (1975). (70G) Pias, J. B., Gasco, L., Rev. Agroquim. (26G) Fisher, J. F., J. Agric. Food Chem., 23, (83F) Smith, C. R., Jr., J. Chromatogr. Sci., 14, Tecnol. Aliment., 15, 113 (1975); Chem. Abstr., 83, 1199(1975). 36'( 1976). 14595411(1975). (27G) Fisher, J. F., Wheaton, T. A,, J. Agric. Food (84F) Spencer, G. F., Herb, S. F., Gormisky, P. Chem., 24, 898 (1976). (71G) lbid., 16, 131 (1976); Chem. Abstr., 85, 31694p (1976). J., J. Am. Oil Chem. SOC., 53, 94 (1976). (28G) Fleming, H. P., Thompson, R. L., Etchells, (85F) Strocchi, A,, Bonaga, G., Riv. /tal. Sostanze (72G) Qureshi, S. Z., Rathi, M. S..Bano, S., Anal. J. L., J. Assoc., Off. Anal. Chem., 57, 130 (1974). Grasse, 52, 84 (1975); Anal. Abstr., 29, 4F43 Chem., 46, 1139 (1974). (29G) Freeman, G. G., Whenham, R. J., J. Sci. (1975). (73G) Riggin, R. M., Kissinger, P. T., J. Agric. Food Agric., 26, 1529 (1975). Food Chem., 24, 900 (1976). (86F) Utriiia, R. M., Juarez, M., Martinez, I., Gra(30G) Freeman, G. G., Whenham, R. J., J. Sci. sas Aceites (Seville), 27, 5 (1976); Chem. Abstr., (74G) Schlack, J. E., Dicecco, J. J., J. Assoc. Off. Food Aoric.. 26. 1869 (1975). 84, 134179h (1976). Anal. Chem., 57, 329 (1974). (31G) Gaba, K. L.. J a h M. K., indian J. Dairy Sci., (87F) Van Dijck, M., Daenens, P., Larueile, L., (75G) Schreier, P., Drawert, F., Z. Lebensm.27, 81 (1974); Chem. Abstr., 81, 1347569 (1974). Rev. Fr. Corps &as, 22, 619 (1975); Chem. Abstr., Unters.-Forsch., 154, 273 (1974). /32G) Gostecnic, G. F., Zlatkis, A,, J. Chroma84, 1 3 4 2 2 6 ~(1976). (76G) Schreier, P., Drawert, F., Junker, A., togr., 106, 73 (1975). Braowissenschaft, 27, 205 (1974); And. Abstr., 28, (88F) Putte, K. P. A. M. van, Enden, J. van den, J. (33G) Govindarajan, V. S., Ananthakrishna. S. M., Am. OilChem. SOC.,51,316 (1974). 4F46 (1975). Flavour hd., 5, 176 (1974); Chem. Abstr., 82, 27042 (89F) Van Putte, K., Vermaas. L., van den Enden, 11975) (77G) lbid., 28, 73 (1975); Anal. Abstr., 29, 5F47 - -,J., Den Hollander, C., ibid., 52, 179 (1975). (1975). (34G) Hansen, E. H., Fiiho, H. B., Ruzicka, J., (9OF) Waltking, A. E., J. Assoc. Off. Anal. Chem., (78G) Schreier, P., Drawert, F., Junker, A., Z. Anal. Chim. Acta, 71, 225 (1974). 58, 898 (1975). Lebensm.-Unters.-Forsch., 154, 279 (1974); Anal. (35G) Harkes, P. D., Begemann, W. J., J. Am. Oil Abstr., 27, 2916 (1974). (91F) Waltking, A. E., Seery, W. E.,Geffert, G. W., Chem. Soc., 51, 356 (1974). J. Am. Oil Chem. SOC., 52, 96 (1975). (79G) Schreyen, L., Dirinck, P., Van Wassenhove, (36G) Hefendehl, F. W., Ziegler, E., Dtsch. LeF., Schamp, N., J. Agric. Food Chem., 24, 336 (92F) Warmbier, M., Fette, Seifen, Anstrichm., 6ensm.-Randsch., 71, 287 (1975); Anal. Abstr., 30, (1976). 76, 86 (1974). 3F18 (1976). (80G) Senanayake. U. M., Edwards, R. A,, Lee, (93F) Washburn, K. W., Nix, D. F., Poultry Sci., (37G) Honkanen, E., Pyysalo, T., 2. Le6ensm.T. H., J. Chromatogr., 116, 468 (1976). 53, 1118 (1974); Anal. Abstr., 29, 5D54 (1975). Unters. Forsch., 180, 393 (1976). (81G) Shankaranarayana, M. L., Abraham, K. O., (94F) Weihrauch, J. L., Brewington, C. R., (38G) Jobbagy, A., Hollo, J., Nahrung, 20, 287 Schwartz, D. P., Lipids, 9, 883 (1974). Raghavan, B., Natarajan. C. P., CRC Crit. Rev. Food (1976); Anal. Abstr., 31, 4F32 (1976). ~
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Sci. Nutr., 6,271 (1975). (82G) Sloot, D., Harkes. P. D., J. Agric. Food Chem., 23,356 (1975). (83G) Sloot, D., Hofman, H. J., ibid., 23, 358 (1975). (84G) Soliman, M. M., Kinoshita, S., Yamanishi, T., Agric. Biol. Chem., 39,973 (1975). (85G) Stahl, E., Laub. E., Woller, R., Fresenius’ Z.Anal. Chem., 275,257 (1975). (86G) Staudt, G., Drawert, F., Tressl, R., Z. fflanzenzuechf.. 75,36 (1975); Chem. Absfr., 84, 1494871(1976). (87G) Tatum, J. H., Berry, R. E., J. FoodSci., 38, 1244 (1974). (88G) Tewari, G. M., Bandyopadhyay, C., J. Agric. Food Chem., 23,645 (1975). (89G) Tressl, R., Renner, R., Mschr. Brau., 28, 195 (1975); Anal. Abstr., 30,3F36 (1976). (90G) Tuttas, R., Beye, F., Z. Lebensm.-Unfers.Forsch., 155,88 (1974). (91G) Vasyagina, R. D., Chmil, V. D., Dobryanskii. V. M., Khim. Sel. Khoz., 14,17 (1976); Chem. Abstr., 84, 120002h (1976). (92G) Vitzthum, 0. G., Werkhoff, P., J. Agric. FoodChem., 23,510(1975). (93G) Vitzthum, 0. G., Werkoff. P., Hubert, P., J. FoodSci., 40,911 (1975). (94G) Wang, P. S..Siebert, K. J., Tech. Quart Master Brew Assoc. Am., 11, 110 (1974); Anal. Abstr., 28, 6F26 (1975). (95G) Whiting, G. C., Coggins, R. A,, J. Sci. Food Agric., 26, 1833 (1975). 06G) Wong, N. P., Ellis, R., LaCroix, D. E., J. Dairy Sci., 58, 1437 (1975). (97G) Zappavigna, R., Brambati, E., Bonino, F., Latte, 2,843 (1974); Anal. Abstr., 30, I F 4 (1976). (98G) Zehner, J. M., Simonaitis, R. A,, J. Chromatogr., 14,348 (1976). (99G) Zuercher, K., Hadorn, H., Miff. Geb. Lebensmittelunters Hyg., 85,466 (1974). (100G) Zuercher, K., Hadorn, H., Strack, C., ibid., 65,440 (1974). ldentlty (IH) Alvarez Vega, E., Simal Lozano, J., Charro Arias, A,, Creus Vidal, J. M., An. Bromatol., 26, 1 (1974); Anal. Abstr., 27,2889 (1974). (2H) Alvarez, E., Simal, J., An. Bromafol, 26,103 (1974); Chem. Abstr., 82, 153870b (1974). (3H) Amorim, H. V., Teixeira, A. A,, Melo, M., Cruz, V. F., Malavolta, E., Turrialba, 25, 18 (1975); Chem. Abstr., 83,7514t (1975). (4H) Appleqvist, L. A., Persson, B., Wallin, B., Naeringsforskning, 19,217, (1975); Chem. Abstr., 85, 19151b (1976). (5H) Ara, V., Thaler, H., Z. Lebensm.-Unters.Forsch, 161, 143 (1976). (6H) Asante, M., Thaier, H., Z. Lebensm.-Unters.-Forsch, 159,93 (1975). (7H) Autran, J. C., Bull. Anc. Eleves Ec. Meun., 270, 316 (1975); Chem. Abstr., 85, 191499 (1976). (8H) Bailey, F. J., J. Sci. Food Agric., 27, 827 (1976). (9H) Beech, F. W., Timberiake, C. F., J. lnst. Brew., 81, 454 (1975); Anal. Abstr., 30, 5F56 (1976). (10H) Benk, E., Hochgesang, G., Milchwissenschaft, 31, 270 (1976); Chem. Abstr., 85, 45088f (1976). (11H) Bergner, K., Diemair, S.,Z. Lebensm.Unters.-Forsch, 157, 1, 7 (1975). (12H) Bose, P. K., J. Food Sci., 11, 28 (1974). (13H) Bracciali, A,, Cantagalii, P.. Piazzi, S. E.. Sordi, S.,Boll. Lab. Chim. frov., 25, 232 (1974); Chem. Abstr., 82, 168821t (1975). (14H) Bracco, U., Winter, H., Rev. Fr. Corps Gras, 23, 87 (1976); Chem. Abstr., 85, 181481 (1976). (15H) Carbaliido, A., Menendez Rivas, M. A,. Lorente, V., An. Bromatol, 24, 259 (1972); Anal. Abstr., 27,2899 (1974). (16H) Chan, H. T., Jr., Kwok, S. C. M., J. Food Sci., 40,419 (1975). (17H) Chan, H. T., Jr., Heu, R. A,, J. Food Sci., 40, 1329 (1975). (18H) Chan, H. T., Jr., Lee, C. W. Q., J. Food Sci., 40,892 (1975). (19H) Clifford, M. N., Process Biochem., IO, 20 (1975); Chem. Absfr., 83, 112443s (1975). (20H) Cobb, 9. F., 111, Vanderzant, C., J. FoodSci., 40, 121 (1975). (21H) Corrao. A., Fazio, G., Cilluffo, V., Gattuso, A. M., lnd. Agrar., 12,182 (1974); Anal. Absfr., 29, 1F64 (1975). (22H) Corrao, A., Gattuso, A. M., Fazio, G.. Cilluffo, V., ind. Agrar., 12,7 (1974); Anal. Absfr., 28,
IF17 (1975). (23H) Dadic, M., Brew. Dig., 54 (1975); Anal. Abstr., 30,4F31 (1976). (24H) Damicz, W., Kostyra, H., Nowicka, R., Zesz. Nauk. Akad. Roln.-Tech. Olsztynie, Technol. Zywn., 3, 3 (1974); Chem. Absfr., 82, 153894n (1975). (25H) Davies, A. M. C., J. Chromatogr., 115,293 (1975). (26H) Davies, A. M. C., J. Apic. Res., 14, 29 (1975); Chem. Absfr., 83, 112516t (1975). (27H) Delaveau, P., Lim, S., Ann. Pharm. Fr., 33, 221 (1975); Anal. Abstr., 30,4F15 (1976). (28H) Di Giacomo, A.. Leuzzi, U., Micah, G., Essenze Deriv. Agrum., 43, 11 (1973): Chem. Absfr., 81, 150577e (1974). (29H) Drawert, F., Radola, B., Mueller, W., Goerg, A., Bednar, J., R o c . Eur. Brew. Conv., 463 (1973); Anal. Abstr., 28, 3F47 (1975). (30H) Drawert, F., Goerg. A,, Z. Lebensm.-Unters.-Forsch., 154,328 (1974). (31H) Dresselhaus, M., Acker, L., Miffeilungsbl. GDCh-Fachgruppe Lebensmiftelchem. Gerichtl. Chem., 28,355(1974); Chem. Abstr., 8 2 , 9 6 5 3 7 ~ (1975). (32H) Dresselhaus, M., Acker, L., Gefreide Mehl Brot., 28, 137 (1974); Anal. Abstr., 29, IF30 (1975). (33H) Feillet, P., Kobrehel, K., CerealChem., 51, 203 (1974). (34H) Fincke. A., Dtsch. Lebensm.-Rundsch., 71, 284 (1975). (35H) Formo, M. W., Honold, G. R., MacLean. D. B., J. Assoc., Off. Anal. Chem., 57,841 (1974). (36H) Frittoli. A., Cantoni, C., lnd. Aliment., finerolo, 12, 140 (1973); Anal. Absfr., 27, 3606 (1974). (37H) Galvao, L. C. A., Lopez, A,, Williams, H. L., J. FoodSci., 41, 1305 (1976). (38H) Goodali, H., Scholey, F.. J. Food Technol., IO, 39 (1975). (39H) Guyot. A., Monseur, X., Sadini, V., Riv. ltal. Sostanze Grasse, 52,622 (1975); Anal. Abstr., 31. 2F10 (1976). (40H) Habegger, M., Sulser, H., Lebensm.-Wiss. Technoi., 7, 182 (1974). (41H) Hamm, R., Masic, D., Sauer, H., Fleischwirtschaff, 55, 242 (1975); Anal. Abstr., 30, 5F28 (1976). (42H) Hauser, E., Bicanova, J., Kuenzler. W., Mitt. Geb. Lebensmittelunters. Hyg., 65, 82 (1974). (43H) Heatherbell, D. A,, J. Sci. FoodAgric., 26, 815 (1975). (44H) Heideibaugh, N. D., Huber, C. S.,Bednarczyk, J. F., Smith, M. C., Rambaut, P. C., Wheeler, H. O., J. Agric. Food Chem., 23, 611 (1975). (45H) J. Off. Repub. Fr., 103 (1975); Anal. Abstr., 31, 1F20(1976). (46H) Kaimal, T. N. B., Mani, V. V. S.,Achaya, K. T., Lakshminarayana, G., J. Chromatogr., 100,243 (1974). (47H) Lee, Y. B., Rickansrud, D. A,, Hagberg, E. C., Briskey, E. J., Greaser, M. L., J. FoodSci., 40, 380 (1975). (48H) Lehmann, G., Neumann, B., Deut. Lebensm.-Rundsch., 71,61 (1975). (49H) Lindqvist, B., Oestgren, J., Lindberg, I., 2. Lebensmittelunters.-Forsch., 159, 15 (1975). (50H) Lloyd, J. B. F., Hadley. K., Roberts, B. R. G., J. Chromatogr., 101,417 (1974). (5 1H) Lorenz, K., Maga. J., J. Milk Food Technol,, 38,84 (1975); Chem. Absfr., 83, 1 1 2 4 3 9 ~(1975). (52H) Mauro, A., lnd. Aliment., finerolo, 12,105 (1973); Anal. Abstr., 27,3603 (1974). (53H) Moshonas, M. G., Shaw, P. E., int. Flavours FoodAddit., 6, 133 (1975); Anal. Abstr., 29,5F31 (1975). (54H) Nazir, D. J., Moorecroft, B. J., Mishkel, M. A., Am. J. Clin. Nutr., 29,331 (1976). (55H) Nosko, S.,Dtsch. Lebensm. Rundsch., 70, 397 (1974). (56H) Pearson, D., Analyst (London), 100, 73 (1975). (57H) Pokorny, J., Nguyen Huy Con, Bulantova, H., Janicek, G., Nahrung, 18,799 (1974). (58H) Resmini, P., Getreide, MehiBrot, 28,234 (1974); Chem. Abstr., 82,41903h (1975). (59H) Resmini, P., Volonterio, G., Sci. Technol. Alimenti, 4, 213 (1974); Chem. Abstr., 85, 107535k (1976). (60H) Royo-lranzo, J., Gimenez Garcia, J.. lnt. Fruchtsaffunion, Wiss.-Tech. Komm., Ber., 13,239 (1973); Chem. Abstr., 81, 1 3 4 8 0 4 (1974). ~ (61H) Sayed, G. E-K., Diss. Abstr. lnt., B., 34, 6049 (1974); 142 pp (Eng.). Avail. Univ. Microfilms,
Ann Arbor, Mich., Order No. 74-10,362, (62H) Satterlee, L. D., Vavak, D. M., Abdul-Kaidr, R., Kendrick, J. G., Cereal Chem., 53, 739 (1976). (63H) Scholey, J., Flavour lnd., 5 , 118 (1974); Anal. Abstr., 27,3598 (1974). (64H) Schwein, W. G., J. Assoc. Off. Anal. Chem., 57, 1005 (1974). (65H) Selvaraj, Y., Suresh. E. R., Divakar, G. S. R., Negi, S. S., J. Food Sci. Technoi., 12, 75 (1975). (66H) Sen, A. R., Sengupta, P., Dastidar, N. G., Analyst(London), 99,153 (1974). (67H) Serebrennikova, V. A,, Rashkina, N. A,, Gig. Sanit., 8,54 (1974); Chem. Abstr., 81,150415a (1974). (68H) Silano, V., Boil. Chim. Unione ita/. Lab. frov., 1, 338 (1975); Chem. Abstr., 84, 162930q (1976). (69H) Simal Lozano, J., Charro Arias, A,, Alvarez Vega, E., An. Bromatol., 24, 235 (1972); Anal. Abstr., 27,2888 (1974). (70H) Sinell, H. J.. Mentz, I., Arch. Lebensmittelhyg., 26, 41 (1975); Chem. Abstr., 63, 567951.1 (1975). (71H) Spell, E., Fleischwirtschaff, 54,533 (1974): Anal. Abstr., 28,2F13 (1975). (72H) Spencer, G. F., Herb, S.F., Gomisky, P. J., J. Am. Oil Chem. Soc., 53,94 (1976). (73H) Sulser, H., Dtsch. Lebensm.-Rundsch.,70, 437 (1974). (74H) Tateo, F., Riv. ltal. Sostanze Grasse, 51, 155 (1974); Chem. Abstr., 81, 1 5 0 3 8 8 ~(1974). (75H) Valencia Diaz, F., Garcia de Jalon Comet, A., Gracia Gomez, M. S.,Grasas Aceit., 26, 277 (1975); Anal. Abstr., 30,5F33 (1976). (76H) Vandercook, C. E., Price, R. L., Harrington, C. A., J. Assoc. Off. Anal. Chem., 58,482 (1975). (77H) Vilar, H. D., Ferreira, L. A. B., Garcia de Orta Ser. €stud. Agron., 1, 41 (1973); Biol. Abstr., 61,31298 (1976). (78H) Weihrauch, J. L., Kinsella, J. E.. Watt, B. K., J. Am. Diet. Assoc., 68,335 (1976). (79H) Yafiez, E., Ballester, D., Monckerberg, F., Heimlich, W., Rutman, M.. J. Food Sci., 41, 1289 (1976). (80H) Zuercher, K., Maurizio, A,, Hadorn, H., Apidologie, 6,59(1975); Chem. Abstr., 83,41679k (1975).
lnorganlc (IJ) Anderson, D. H.. Murphy, J. J., White, W. W., Anal. Chem., 48, 116 (1976). (2J) Baetz, R. A., Kenner, C. T., J. Assoc. Off. Anal. Chem., 57, 14 (1974). (3J) Baetz, R. A., Kenner, C. T., J. Agric. Food Chem., 23,41 (1975). (4J) Bailey, J. E.. Graichen, C., J. Assoc. Off. Anal. Chem., 57,353 (1974). (5J) Baroliier, J.-P., Pottier, L.. Ledrappier, N., Bios (France),6,296 (f975); Anal. Absfr., 30,4F32 (1976). (6J) Berkh, M. S.,Levyanto, S. I.,Belakovskaya, I. V., Konservn. Ovoshchesush. from-st., 3, 41 (1975); Chem. Abstr., 82, 168929b (1975). (7J) Bernatonis, J., Ramonaityte, D., Liet. TSR Aukst. Mokyklu Mokslo Darb., Chem. Chem. Techno/., 15, 407 (1973); Chem. Abstr., 83, 26374p (1975). (8J) Black, L. T., J. Am. OilChem. SOC., 52,88 (1975). (9J) Blood. E. R., Grant, G. C., Anal. Chem., 47, 1438 (1975). (1OJ) Bradfield, E. G., Ana/yst(London), 99,403 (1974). (11J) Bradfield, E. G., Stickland, J. F., Analyst (London), 100, l(1975). (12J) Brammell, W. S., J. Assoc. Off. Anal. Chem., 57, 1209 (1974). (13J) Caupeil, J. E., Hendrikse, P. W., Bongers, J. S., Anal. Chim. Acta, 81,53 (1976). (14J) Chavdarova, R., Schmid, E. R., Becker, R. R., Mikrochim. Acta, I (4), 443 (1975). (15J) Cheng, W. C., Shiue, H. I.,Cheng, T. H., froc. Congr. lnt. SOC. Sug. Cane Technol., 15th, 1379 (1974); Anal. Abstr., 29,3F8 (1975). (16J) Chilov, S.,Talanta, 22, 205 (1975); Anal. Abstr., 29,5874 (1975). (17J) Chow, T. J., Patterson, C. C., Settle, D., Nature (London), 251, 159 (1974). (18J) Coilet, P., Dtsch. Lebensm. Rundsch., 71, 249 (1975). (19J) Cornell. D. G.. Interface, 4, 14 (1975); Chem. Abstr., 83, 1 1 2 4 5 5 ~(1975). (20J) Crecelius. E. A,, Anal. Chem., 47, 2034
ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
217R
(1975). (21J) Dewit, A., Duwijn, R., Smeyers-Verbeke, J., Massart, D. L., Bull. SOC. Chim. Belg., 84, 91 (1975); Chem. Abstr., 82, 168911q (1975). (22J) Drew, R . E., J. Fish. Res. Boardcan., 32, 813 (1975); Anal. Abstr., 30, 6F3 (1976). (23J) Dultey, J. R., Anal. Biochem., 67, 91 (1975). (24J) Egan, H., J. Assoc. fob. Anal., 13, 118 (1975); Anal. Abstr., 31, I F 3 (1976). (25J) Eipeson, W. E., Paulus, K., Lebensm. Wiss. Technol., 7, 47 (1974); Anal. Abstr., 28, 2F2 (1975). (26J) Elliott, S. C., Loper, B. R., Anal. Chem., 46, 2256 (1974). (27J) Farhan, F. M., Pazandeh, H., J. Am. Oil Chem.' SOC., 53, 21 1 (1976). (28J) Feldman, C., Anal. Chem., 46, 1606 (1974). (29J) Fiorino, J. A,, Jones, J. W., Capar, S. G., Anal. Chem., 48, 120 (1976). (30J) Freeman, H., Uthe, J. F., Flemming, B., At. Absorpf. Newsl., 15, 49 (1976). (31J) Fric, F., Paiovcikova, V., lnt. J. Appl. Radiat. /Sot., 26, 305 (1975); Anal. Abstr., 29, 6G3 (1975). (32J) Fricke, F. L., Rose, O., Jr., Caruso, J. A,, Talanta, 23, 317 (1976): Anal. Abstr., 31, 405 (1976). (33J) Getzendaner, M. E., J. Assoc. Off. Anal. Chem., 5 8 , 711 (1975). (34J) Grys, S., Mikrochim. Acta, I (2-3), 147 (1976). (35J) Grys, S., J. Chromatogr.. 100, 43 (1974). (36J) Haddad, P. R., Smythe, L. E., Talanta, 21, 859 (1974); Anal. Abstr., 28, 4D16 (1975). (37J) Haller, H. E., Mack, D., Dtsch. Lebensm. Rundsch., 71, 430 (1975); Anal. Abstr., 31, IF8 (1976). (38J) Heine, K., Wiechen, A,, Milchwissenschaff, 31, 65 (1976). (39J) Helsby, C. A,, Mikrochim. Acta, I (2-3), 307 (1976). (40J) Hinners, T. A,, Bumgarner, J. E., Simmons, W. S., At. Absorpt. Newsl., 13, 146 (1974); Chem. Abstr., 82, 84549q (1975). (41J) Hirayama, H., Shimoda, Z., Noguchi, C., Kobayashi, A,, Shige. T., Takahashi, T., Tsuji, K., Nakasato. S.,Higuchi, M., et al., Yukagaku, 25, 275 (1976); Chem. Abstr., 85, 31691k (1976). (42J) Holak, W.. J. Assoc. Off. Anal. Chem., 58, 777 (1975). (43J) Holak, W.. J. Assoc. Off. Anal. Chem., 59, 650 (1976). (44J) Holz, F., Landwirtsch. Forsch., 26, 56 (1973); Anal. Abstr., 27, 2692 (1974). (45J) Huffman, H. L., Jr., Caruso, J. A,, Talanta, 22, 871 (1975); Anal. Abstr., 30, 5F7 (1976). (46J) Ihnat, M., Westerby, R., Anal. Lett., 7, 257 (1974); Anal. Abstr., 28, I F 5 (1975). (47J) Ikebe. K., Tanaka, Y., Tanaka, R., Kunita, N., Shokuhin Eiseigaku Zasshi, 15, 368 (1974); Chem. Abstr., 82, 84556q (1975). (48J) lbid., 18, 132 (1975); Chem. Abstr., 84, 103907q (1976). (49J) Isherwood, S. A,, King, R. T., J. Sci. Food Agric., 27, 831 (1976). (50J) Jackson, C. J., Morely F., Porter, D. G.. Lab. fract., 24, 23 (1975); Anal. Abstr., 29, 3F1 (1975). (51J) Jacob, R. A , , Klevay, L. M., Anal. Chem., 47, 741 (1975). (52J) Jacobson, J. S.,Heller, L. I., J. Assoc. Off. Anal. Chem., 58, 1129 (1975). (53J) Jayman, T. C. Z., Sivasubramaniam, S., Analyst(London), 99, 296 (1974). (54J) Jervis, R. E., Tiefenbach, B., Chattopadhyay, A,, Can. J. Chem., 52, 3008 (1974); Anal. Abstr., 28, 5D12 (1975). (55J) Jonsson, H., 2. Lebensm.-Unters. Forsch., 160, l(1976). (56J) Joerin, M. M., Analyst (London), 100, 7 (1975). (57J) Kaiser, G., Goetz, D., Schoch, P., Toelg, G., Talanta, 22, 889 (1975); Anal. Abstr., 30, 5880 (1976). (58J) Kupur, J. K., West, T. S.,Anal. Chim. Acta, 73, 180 (1974); Anal. Abstr., 28, 6F5 (1975). (59J) Kirsten, W. J., Anal. Chem., 48, 84 (1976). (60J) Knapp, G., Fresenius' Z. Anal. Chem., 274, 271 (1975); Anal. Abstr., 30, I C 1 (1976). (61J) Koirtyohann, S. R., Pickett. E. E., Flame Emiss. At. Absorpf. Spectrom., 3, 414 (1975); Chem. Abstr., 84, 420393 (1976). (62J) Kroeller, E., Msch. Lebensm. Rundsch., 71,
218R
0
73 (1975). (104J) Tornberlin. T. A,, Eckhoff, N. D., Nucl. ln(63J) lbid., 72, 94 (1976). strum. Methods, 125,549(1975); Anal. Abstr., 30, (64J) Kundu, M. K., Prevot, A,, Anal. Chem., 46, 6G2 (1976). 1591 (1974). (105J) Tonkaboni, M., Brauwissenschaff, 27, 133 (65J) Kurokawa, M., Kaneko, M., Nishiyama, N., (1974); Anal. Abstr., 27, 3614 (1974). Fukui, S., Kanno, S.,EiseiKagaku, 21, 77 (1975); (106J) Tsutsumi, C.. Koizumi, H., Yoshikawa, S., Anal. Abstr., 30, 2F4 (1976). BunsekiKagaku, 25, 150 (1976); Anal. Abstr., 31, (66J) Lapitskaya, S. K., Sviridenko, V. G., Pala4F6 (1976). marchuk, A. S., Z. And. Khim., 30, 629 (1975); Anal. (107J) Ure, A. M., Anal. Chim. Acta, 76, 1 Abstr., 30, 4F2 (1976). (1975). (67J) Mack, D., Dtsch. Lebensm. Rundsch., 71, (108J) Uthe, J. F., Freeman, H. C., Johnston, J. 71 (1975); Anal. Absfr., 29, 4F5 (1975). R., Michalik, P., J. Assoc. Off. Anal. Chem., 57, 1363 (68J) Martin, R. A., Seaman, G. G., Ward, A,, (1974). Cereal Chem., 52, 138 (1975). (109J) Van Den Heede, M. A,, Heyndrickx, A. M., (69J) Martinie, G. D., Schiit, A. A., Anal. Chem., Van Peteghem, C. H.. Van Zele, W. A., J. Assoc. Off. 48, 70 (1976). Anal. Chem., 58, 1135 (1975). (70J) Maurer, L., Z. Lebensm.-Unters. Forsch., (1 1OJ) Van Vliet, H., Basson, W. D., Boehmer, R. 156, 284 (1974). G., Analyst(London), 100, 405 (1975). (71J) McHard, J. A., Winefordner, J. D., Attaway, (111J) Vul'fson, E. K., Gribovskaya, I. F., KarJ. A., J. Agric. FoodChem., 24, 41 (1976). yakin, A. V., Yanushkevich, A. F., Zh. Anal. Khim., (72J) Miyamoto, K., Yokoyama, T., Elsei Kagaku, 30, 1913 (1975); Anal. Abstr., 31, 2D3 (1976). 22, 76 (1976); Anal. Abstr., 31, 4F7 (1976). (1 12J) Wildanger, W., Z . Lebensm. Unters. (73J) Moll, M., Flayeux, R., Lehuede, J-M., Bios Forsch., 155, 321 (1974); Anal. Abstr., 28, 4F1 (France), 6, 85 (1975); Anal. Abstr., 29, 5F45 (1975). (1975). (113J) Woidich, H., Pfannhauser, W., Z. Le(74J) Morris, N. M., Clarke, M. A,, Tripp. V. W., bensm. Unters. Forsch., 159, 323 (1975); Anal. Carpenter, F. G., J. Agric. Food Chem., 24, 45 Abstr., 31, I F 9 (1976). (1976). (1 14J) Woidich, H., Pfannhauser, W., Fresenius' (75J) Morrissey, P. A,, lr. J. Agric. Res., 14, 86 2.Anal. Chem.. 276. 61 (1975); Anal. Abstr.. 30, (1975); Chem. Abstr., 83, 1 3 0 0 9 9 ~(1975). 3F5 (1976). (76J) Mrowetz, G., Thomasow, J.. Milchwissen(115J) Wolf, W., Mertz, W., Masironl, R., J. Agric. schaff, 29, 74 (1974); Anal. Abstr.. 28, 6F2 Food Chem., 22, 1037 (1974). (1975). (77J) Murthy, G. K., Crit. Rev. Environ. Control, 4, l(1974); Chem. Abstr., 81, 1 3 4 6 6 0 ~(1974). Moisture (78J) Nakamachi, H..Okamoto, K., Kusumi, I., Jpn. Anal., 23, 10 (1974); Anal. Abstr., ,28, 4F2 (IK) Addis, P. B., Chudgar, A. S., J. Fow'Sci., 38, (1975). 354 (1973). (79J) Nakashima, R., Sasaki, S.,Shibata, S., (2K) Basker, D., J. Assoc. Offic. Anal. Chem., 58, Anal. Chim. Acta, 77, 65 (1975). 618 (1975). (80J) Newton, M. P., Davis, D. G., Anal. Chem., (3K) Basler, W., Lechert, H., Sfaerke, 25, 289 47, 2003 (1975). (1973); Anal. Abstr., 28, IF11 (1975). (81J) Nishi, S., Horimoto, Y., Nakano, N., Jpn. (4K) Dulphy, J. P., Demarquilly, C., Henry, M.. Anal., 23, 386 (1974); Anal. Abstr., 28, 5D13 Jailler, M., Jamot, J.. L'Hotelier, L., Ann. Zootech., (1975). 24, 743 (1975); Chem. Abstr., 84, 149318b (82J) Noguchi, C., Hirayama, H.,Shige, T., Jinbo, (1976). M., Takahashi, T., Tsuji, K., Nakasato, S., Matsubara, (5K) Farnell, P. J., Analyst (London) 100, 661 S.,Murase, Y., et al., Yukagaku, 24, 100 (1975); (1975). Chem. Absfr., 82, 110379f (1975). (6K) Helf, S., God. Rept. Announce, 74, 57 (83J) Ohyama. T., Kawabata, J., Eiyo To Shoku(1974). ryo, 27, 325 (1974);.Chem. Abstr., 82, 153889q (7K) Hester, R. E., Quine, E. C.. J. Food Technol., (1975). 11, 331 (1976). (84J) Olejko, J. T., J. Am. Oil Chem. Soc., 53, (8K) Hirschberg, F., Szabo, Z., Acta Aliment, 355 480 (1976). (1972); Chem. Abstr., 81, 1 5 0 3 8 3 ~(1974). (85J) Olson, 0. E., Palmer, I . S., Cary, E. E., J. (9K) Karmas, E., Chen, C. C., Anal. Calorimetry, Assoc. Off. Anal. Chem., 58, 117 (1975). 489, (1974); Chem. Abstr., 83, 7291t (1975). (86J) Orvini, E., Gills, T. E., LaFleur, P. D., Anal. (10K) Karmas, E., Turk, K., Z. Lebensm-UnChem., 46, 1294 (1974). ters.-Forsch, 158, 145 (1975). (87J) Owlya, A,, Parsa, B., Fakhrvaezi, F., Radi(11K) Kay, J. M., Islam, M. A,, Blanshard, J. M. V., ochem. Radioanal. Lett., 16, 355 (1974); Anal. J. Food Technol., IO, 123 (1975). Abstr., 27, 2878 (1974). (12K) Kirkbright, G. F., Mayne, P. J., West, T. S., (88J) Plesch, R., GlT Fachz. Lab., 18, 1106 J. Food Techno/., 10, 103;(1975). (1974): Anal. Abstr., 29, 1F1 (1975). (13K) Labuza, T. P., Acott, K., Tatini, S. R., Lee, (89J) Preen, M. A., Woodward, J. D., J. lnst. R. Y., Flink. J., McCail, W., J. FoodSci., 41, 910 Brew., 81, 307 (1975); Anal. Abstr., 30, 3F31 (1976). (1976). (14K) Mansfieid, P. B., Br. Patent, 1,374,427, (9OJ) Raffke, W., Wirthgen, B., Nahrung, 20,41 (issued Nov. 20, 1974). (1976); Anal. Abstr., 31, 2G3 (1976). (15K) Mitchell, J., Anal. Chim. Acta, 81, 231 (91J) Rook, H. L., Suddueth, J. E., Becker, D. A,, (1976). Anal. Chem., 47, 1557 (1975). (16K) Mousseri, J., Steinberg, M. P., Nelson, A. (92J) Ruzicka, J.. Stewart, J. W. B., Anal. Chim. I., Wei, L. S., J. Food Sci., 39, 114 (1974). (17K) Parizkova, H., 2. Le6ensm.-Unters.-Forsch, Acta, 79, 79 (1975); Anal. Absfr., 30, 5G2 (1976). 156, 193 (1974). (932) Ryan, D. E., Holzbecher,J., Rollier, H., Anal. Chim. ,!eta, 73, 49 (1974). (18K) Pettinati, J. D.. J. Assoc. Off. Anal. Chem., 58, 1188 (1975). (94J) Shah, S. K., J. lnst. Brew., 81, 293 (1975); (19K) Powley, C., Control lnstrum, 7, 24 Anal. Abstr., 30, 3F30 (1976). 11975). (95J) Shimoishi, Y., Bull. Chem. SOC.Jpn., 47, ' (20K) Reineccius, G. A,, Addis, P. B., J. FocdSci., 997 (1974); Anal. Abstr., 27, 3634 (1974). 38. 355 11973). (96J) Simmons. W. J., Anal. Chem., 47, 2015 i21K) 'Ross,'K. D., Food Technol. (Chicago),29, (1975). 26 ( 1975). (97J) Siska, E., Dtsch. Lebensm. Rundsch., 71, (22K) Schneider, F., Emmerich, A., Ticmanis, U., 209 (1975); Anal. Abstr., 30, 2F2 (1976). Zucker, 28, 349 (1975); Anal. Abstr., 30, 5F17 (98J) Slavin, S., Peterson, G. E.. Lindahl, P. C., ( 1976). At. Absorpt. Newsl., 14, 57 (1975). (99J) Sourek, R., Flanderkova, B., Stulik, K., (23K) Sloan, A. E., Labuza, T. P., Focdfrcd. Dev., Chem. Listy, 69, 1207 (1975); Anal. Abstr., 30, 6F4 9. 68 (1975). (1976). (24K) Sood, V. C., Heldman, D. R., J. FoodSci., (IOOJ) Stijve. T., Cardinale, E., J. Chromatogr., 39, 1011 (1974). 109, 239 (1975). (25K) WaQStaffe, P. J., Analyst (London), 99, 537 (101J) Szabo, A , , Bende, E., Lebensm. lnd.. 22, (1974). 127 (1975); Anal. Abstr., 30, 5F53 (1976). (26K) Weldring, J. A. G., Wolters, I., Van den (102J) Tanaka, Y., Ikebe, K., Tanaka, R., Kunita, Berg, C., Meded. Landbouwhogesch. Wageningen, N., Shokuhin Eiseigaku Zasshi, 15, 386 (1974): 75 (1975); Chem. Abstr., 84, 1 4 9 3 6 4 ~ (1976). Chem. Absfr., 82, 84553m (1975). (27K) Zeman, I., Zemanova, D., Veda Vyzk. f o (103J) Thompson, K. C., Analyst (London), 100, travin, Prum., 26, 209 (1974); Chem. Abstr., 85, 307 (1975). 45006c (1976).
ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
'
Organic Aclds (1L) Arndt, W., Thaier, H., Mitt. Hoeheren Bundeslehr-Versuchsanst. Wein-Obstbau, Klosterneuburg, 24, 325 (1974); Chem. Abstr., 82, 96544x (1975). (2L) Clifford, M. N., J. Chromatogr., 94, 261 (1974). (3L) Clifford, M. N., Wight, J., J. Sci. FoodAgric., 27, 73 (1976). (4L) Cooke, D. T., Sansum, L. L., J. Sci. Food Agric., 27, 883 (1976). (5L) Gray, I. K., N.Z. J. DairySci., 11, 54(1976); Chem. Abstr., 85, 45005b (1976). (6L) Hanefeld, M., Herrmann, K., J. Chromatogr., 123, 391 (1976). (7L) Hyakutake, H., Toshihiko, H., J. Chromatogr., 108, 385 (1975). (8L) Kagi, D. A,. Hildebrand, R. P., Clarke, B. J., J. Chromatogr., 115, 79 (1975). (9L) Kroeller, E., Krull, L., Dsch. Lebensm. Roudsch., 71, 294 (1975). (IOL) Mann, J. D., Porter, N. G., Lancaster, J. E., J. Chromatogr., 92 177 (1974). (1 1L) Maga, J. A., Lorenz, K., J. Sci. FoodAgric., 25, 797 (1974). (12L) Maga, J. A., Lorenz, K.,'Lebensm.-Wiss. Technol., 7, 273 (1974). (13L) McGuinness, J. D., Laws, D. R. J., Eastmond, R., Gardner, R. J., J. lnst. Brew., 81, 237 (1975); Anal. Abstr., 30, IF18 (1976). (14L) Michal, G., Beutler, H. O., Lang, G., Guentner. U., Fresenius'Z. Anal. Chem., 279, 137 (1976). (15L) Mizote, A,, Odagiri, H., Toei, K., Tanaka, K., Analyst (London), 100, 822 (1975). (16L) Moll, M., Fiayeux, R., Lehuede, J-M., Brauwissenschaft, 28, 134 (1975); Anal. Abstr., 29, 6F37 (1975). (17L) Molyneux, R. J., Wong. Y.4, Proc. Am. SOC. Brew Chem., 71, (1973); Anal. Abstr., 29, 3F19 11 , 97.5) - . _,. (18L) Molyneux, R. J., Wong, Y-I, J. Agr. Food Chem., 23, 1201 (1975). (19L) Rapp, A,, Ziegler, A,, Chromatographia, 9, 148 (1976); Anal. Abstr., 31, 4F31 (1976). (20L) Richards, M., J. Chromatogr., 115, 259 (1 975). (21L) Sasson, A,, Erner, Y., Monselise, S. P., J. Agric., FoodChem., 24, 652 (1976). (22L) Schmidtlein, H.. Herrmann, K., J. Chromatogr., 115, 123 (1975). (23L) Schneider, G., Arch. Pharm., Weinheim, 309, 38 (1976); Anal. Abstr., 31, 2E6 (1976). (24L) Schuiz, P., Vilceanu, R., J. Chromatogr.. I l l , 105 (1975). (25L) Schwartz, D. P., Bright, R. S., Anal. Biochem., 61, 271 (1974). (26L) Suhren, G., Heeschen, W., Toile, A,, Milchwissenschaft, 31, 257 (1976); Chem. Abstr., 85, 45011a(1976). (27L) Takata, Y., Arikawa, Y., Jpn. Anal., 23, 1522 (1974); Anal. Abstr., 29, 2029 (1975). (28L) Tanner, H., Schweiz. Z . Obst-Weinbau, 112, 38 (1976); Chem. Abstr., 84, 162996r (1 976). (29L) Thibault, J. F., Robin, J. P., Ann. Technol. Agric., 24, 99 (1975); Chem. Abstr., 84, 42080r (1976). (30L) Tressl, R., Kossa, T., Renner, R., Koeppler, H., Mschr. Brau., 28, 109 (1975); Anal. Abstr., 29, 6F36 (1975). (31L) Wuif, L. W., Nagei, C. W., J. Chromatogr., 116, 271 (1976). (32L) Vancraenenbroeck, R., Lontie, R., Bull. Assoc. Roy Anciens Etud. Brass. Univ. Louvain, 70, 71 (1974); Anal. Abstr., 29, 3F21 (1975). (33L) Wallenstein, H. D., Egler, H., 2.Zucklnd., 100, 187 (1975); Anal. Abstr., 31, IF17 (1976). (34L) Zuercher, K., Hadorn, H., Mitt. Geb. Lebensmittelunters.Hyg., 66, 379 (1975); Anal. Abstr., 30, 2F33 (1976). Nitrogen (IM) Addeo, F., Malorni, A., Marino, G., Anal. Biochem., 64, 98 (1975). (2M) Alexander, P. W., Rechnitz, G. A,, Anal. Chem., 46, 860 (1974). (3M) Anderson, W. L., Wetlaufer, D. B., Anal. Biochem., 67, 493 (1975). (4M) Bancher, E., Washuettl, J., Riederer, P.. Stachelberger, H., Wen. Tieraerztl. Mschr., 82, 232 (1975); Anal. Abstr., 31, ID55 (1976). (5M) Batey, T., Cresser, M. S., Willett, I. R., Anal. Chim. Acta., 69, 484 (1974).
(6M) Beckwith, A. C., Paulis, J. W., Wall, J. S..J. Agric. FoodChem., 23, 194 (1975). (7M) Beveridge, T., Toma, S. J., Nakai, S., J. Food Sci., 39, 49 (1974). (8M) Blass, K. G., Thibert, R. J., Microchem. J., 19, l(1974). (9M) Bosset, J., Blanc, B., Plattner, E., Anal. Chim. Acta., 75, 343 (1975). (10M) Bostroem, C. A., Cedergren, A,, Johansson, G., Pettersson, I., Talanta, 21, 1123 (1974). (11M) British Standards Institution, BS, 757, 30 ( 1975). (12M) Buckee, G. K., J. lnst. Brew., 80, 291 (1974); Anal. Abstr., 27, 3615 (1974). (13M) Butler, M., Darbre, A,, J. Chromatogr., 101, 5 1 (1974). (14M) Buttery, P. J., Soar, J. B., J. Sci. Food Agric., 26, 1273 (1975). (15M) Chaytor. J. P., Crathorne, B., Saxby, M. J., J. Sci. FoodAgric., 26, 593 (1975). (16M) Chrastil, J., Anal. Chem., 47, 2293 (1975). (17M) Concon, J. M., Anal. Biochem., 68, 643 119751. -, (18M) Concon, J. M., Anal. Biochem., 67, 206 (1975). (19M) Coppola, E. D., Hanna, J. G., J. Assoc. Off. Anal. Chem., 57, 1265 (1974). (20M) Couch, J. R., Thomas, M. C., J. Agric. Food Chem., 24, 943 (1976). (21M) Creamer, L. K., Matheson, A. R., Lohrey. E. E., N.Z. J. Dairy Sci. Technol., 11, 96 (1976); Chem. Abstr., 85, 9 2 2 8 1 (1976). ~ (22M) Culmsee, O., Dtsch. Lebensm.-Rundsch., 71, 425 (1975). (23M) Davies, M. G., J. Food Technol., 9, 265 (1974). (24M) Dinarieva, G. P., Solntseva, G. L., Khoroshkova, I. D., Surkova, A. N., Tr., Vses. Nauchno-lssled. lnst. Myasn. Prom-sti., 27, 120 (1973); Chem. Abstr., 82, 84560m (1975). (25M) Dohan. D. A,, Standing, K. G., Bushuk, W., CerealChem., 53, 91 (1976). (26M) El Din Awad, A. M., El Din Awad, 0. M., J. Chromatogr., 93, 393 (1974). (27M) El-Hamalawi, A-R. A,, Thompson, J. S., Barker, G. R., Anal. Biochem., 67, 384 (1975). (28M) Erskine, R. L., Steedman, T. A,, J. Appl. Chem. Biotechnol., 25, 221 (1975); Chem. Abstr., 83, 77076a (1975). (29M) Fleck, A.. CRCCrit. Rev. Anal. Chem., 4, 141 (1974). (30M) Frischkorn, C. G. B., Frischkorn, H. E., Z. Lebensm.-Unters.-Forsch, 158, 295 (1975). (31M) Fritz, A., Baumer, M., Ulonska, E., Lenz. W.. Nucl. Tech. Seed Protein lmpr.. Proc. Res. Coord. Meet., 371 (1973); Chem. Abstr., 81, 118623f (1974). (32M) Gerstl, R., Ranfft, K., Mitt. Geb. Lebensmittelunters. Hyg., 65, 399 (1974). (33M) lbid., 66, 413 (1975). (34M) Glowa, W., J. Assoc., Off. Anal. Chem., 57, 1228 (1974). (35M) Golovnya, R. V., Zhuravleva, I. L., Zh. Anal. Khim., 29, 1406, (1974); Anal. Abstr., 29, 3C19 119751. - -, (36M) Guilbault, G. G., Lubrano, G. J., Anal. Chim. Acta, 69, 183 (1974). (37M) Gupta, U. C., Misra, S. C., Rao. U. S.,Use Radioisot. Stud. Plant Proc. Symp., 161 (1974); Chem. Abstr., 84, 1 4 9 3 1 3 ~ (1976). (38M) Hall, G., J. SOC.Dairy Technol., 28, 192 (1975); Anal. Abstr., 31, 2F9 (1976). (39M) Hendrik, A., Husipar, 23, 263 (1974); Chem. Absfr., 83, 7259p (1975). (40M) Higuchi, M., Yoshida, F., Anal. Biochem., 65, 591 (1975). (41M) Holmes, M. G., Food Technol. Aust., 27, 14 (1975); Anal. Abstr., 30, 6F12 (1976). (42M) Honikel, K. O., Sauer, H., Fleischwirfschaft, 5 5 , 1724 (1975); Chem. Absfr., 84, 88054p (1976). (43M) Hossain, M. A,, Kiel. Milchwirfsch. Forschungsber., 28, 27 (1976); Chem. Abstr., 85, 450102 (1976). (44M) Husek. P., Macek, K., J. Chromatogr., 113, 139 (1975). (45M) Joerin, M. M., N.Z. J. Dairy Sci. Technol., 9, 17 (1974); Chem. Abstr., 82, 845289 (1975). (46M) Jones, R. A,, Daiby, A,, Tsai, C. Y., Cereal Chem., 52, 279 (1975). (47M) Kaplan, E. R., Sapeika, N., Moodie, I. M.. Analyst (London), 99, 565 (1974). (48M) Kirkman, M. A., J. Chromatogr., 97, 175 (1974). (49M) Kolakowski, E.. Nahrung, 18, 371 \
~
(1974). (50M) lbid., 19, 621 (1975). (51M) Kuck, J. C., J. Am. OilChem. SOC.,52,230 (1975). (52M) Kushnir, I., Feinberg, J. I., Pensabene, J. W.. Piotrowski, E. G. Fiddler, W., Wasserman, A. E., J. Food Sci., 40, 427 (1975). (53M) Lakritz, L.. Spineill, A. M., J. Agric. Food Chem., 23, 344 (1975). (54M) Lehmann, G., Neumann, B., 2.Lebensm.Unters.-Forsch, 156, 32 (1974). (55M) Lerke, P. A., Bell, L. D., J. FoodSci., 41, 1282 (1976). (56M) Makita, M., Yamamoto, S., Kono, M., Sakai. K., Shiraishi, M., Chem. lnd., 355 (1975). (57M) March, J. F., Anal. Biochem., 69, 420 (1975). (58M) Matheson, N. A., Br. J. Nutr., 31, 393 (1974); Anal. Abstr., 28, 3D129 (1975). (59M) Matoba, T., Komori, N., Doi, E., Agric. Biochem., 39, 2359 (1975); Anal. Abstr., 31, ID59 (1976). (60M) Merbach, A. E., Chastellain, F.. Hirsbrunner, P., Mitt. Geb. Lebensmittelunters.Hyg., 66, 176 (1975). (61M) Mertz. E. T., Misra, Prem. S., Jambunathan, R., CerealChem., 51, 304 (1974). (62M) Mitsuda, H., Mitsunaga, T., Agric. Biochem., 38, 1649 (1974); Chem. Abstr., 82, 2737n (1975). (63M) lbid., 2265 (1974); Chem. Abstr., 82, 84544j (1975). (64M) Moss, C. W., Lambert, M. A,, Anal. Biochem., 59, 259 (1974). (65M) Nanjo, M., Guilbauit, G. G., Anal. Chim. Acta., 73, 367 (1974). (66M) Nau, H., Angew. Chem. lnt. Ed. Eng., 15, 75 (1976). (67M) Noll, J. S., Simmonds, D. H., Bushuk, W., Cereal Chem., 51, 610 (1974). (68M) Norman, G. A,, Follett, M. J., Hector, D. A,, J. Chromatogr., 90, 105 (1974). (69M) 0 hAlmhain, L., 0 Danachair, D., Analyst (London), 99, 21 1 (1974). (70M) Park, D. L., King, R. L., J. Assoc. Off. Anal. Chem., 57, 42 (1974). (71M) Pearson, D., Analyst (London), 99, 612 (1974). (72M) Pearson, D., Pertz, G. A,, J. Food Technol., 11, 423 (1976). (73M) Penke, B., Ferenczi, R., Kovacs, K., Anal. Biochem., 60, 45 (1974). (74M) Pokorny. S., Coupek, J., Phan Trong Tai, Pokorny, J., Z. Lebensm.4hter.s. Forsch., 159, 43 (1975). (75M) Pomeranz. Y . , Moore, R. B., Baker's Dig., 49, 44 (1975); Chem. Abstr., 82, 153898s (1975). (76M) Puhan, Z., Milchwissenschaft, 29, 459 (1974); Anal. Abstr., 29, 3F13 (1975). (77M) Quinn, J. R., Boisvert, J. G. A,, Wood, I., Anal. Biochem., 58, 609 (1974). (78M) Reinefeld, E,, Bliesener, K. M., Kutschke, H..Zucker, 28, 72 (1975); Anal. Abstr., 31, IF18
.
(8lM) Robel, E., Poultry Sci., 52, 604 (1973); Anal. Abstr., 28, 3G4 (1975). (82M) Ruiter, A,, Proc. lnt. Symp. Nitrite Meat Prod., 37, (1974); Chem. Abstr., 83, 56829h (1975). (83M) Ruiter, A., Weseman, J. M.. J Food Technoi., 11, 59 (1976). (84M) Sandler, L., Warren, F. L.. Anal. Chem., 46, 1870 (1974). (85M) Sasaki, T., Abrarns, B., Horecker, B. L., Anal. Biochem., 65, 396 (1975). (86M) Schafer, H. W., Olson, N. F., Anal. Chem., 47, 505 (1975). (87M) Schreier, P., Drawert, F., Junker, A,, Z. Lebensm.-Unters.-Forsch., 157, 34 (1975). (88M) Sherbon, J. W., J. Assoc. Off. Anal. Chem., 58, 770 (1975). (89M) Singer, G. M., Lijinsky, W., J. Agric. Food Chem., 24, 550 (1976). (90M) Sornorin, O., J. Food Sci., 41, 458 (1976). (91M) Srivastava, K. N., Mehta, S. L., Curr. Sci., 45, 283 (1976); Chem. Abstr., 85, 191709 (1976). (92M) Statter. S., U.S. Patent 3,936,271 (1976). (93M) Sturm, W., Thaler, H., Mitt. Geb. Lebensmittelunters. Hyg., 66, 159 (1975). (94M) Sundqvist. B., Goenczi, L., Bergman, R.. '
ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
219R
Lindh, U., lnt. J. Appl. Radiat. /sot., 25,277 (1974); Anal. Abstr., 28, 1 G 1 (1975). (95M) Vandercook, C. E., Price, R. L., J. Assoc. Off. Anal. Chem., 57, 124 (1974). (96M) Vigue, J., Li, P. H., Hort. Scl., IO, 625 (1975). (97M) Vitztum, O., Werkhoff, P., J. Chromatogr., 95,39 (1974). (98M) Voigt, M. N., Eitenmiller,R. R., J. FoodSci., 39, 420 (1974). (99M) Von Lengerken, J., Mueller, V., Wetterau, H., Nahrung, 18, 551 (1974). (100M) Wall, L. L., Gehrke, C. W., J. Assoc. Off. Anal. Chem., 57, 1098 (1974). (101M) Wall, L. L., Gehrke, C. W., Neuner, T. E., Cathev. R. D.. Rexroad. P. R.. J. Assoc. Off. Anal. Chem:, 58,81 1 (1975). (102M) Wall, L. L., Gehrke, C. W., J. Assoc., Off. Anal. Chem., 58, 1221 (1975). (103M) lbid., 59, 219 (1976) (104M) Westgarth, D. R., Williams, A. P., J. Sci. FoodAgric., 25,571 (1974). (105M) Wildanger, W., Dtsch. Lebensm. Rundsch., 72, 160 (1976). (106M) Wisk, T. J., Slebert, K. J., Proc. Am. SOC. Brew. Chem., 26 (1973); Anal. Abstr., 28, 6F24 (1975). (107M) Zadow, J. G., Hill, R. D., J. Dairy Res., 42, 267 (1975). (108M) Zscheile, F. P., Brannaman, B. L., J. Agric. Food Chem., 22, 537 (1974). Vitamins (1N) Abe, K., Yuguchi, Y., Katsui, G., J. Nutr. Sci. Vitaminol., 21, 183 (1975); Chem. Abstr., 84, 88045m, (1976). (2N) Abe, K., Yuguchi, Y., Katsui, G., Eiyo To Shokuryo, 27, 329 (1974); Chem. Abstr., 82, 1 5 3 8 8 8 ~(1975). (3N) Atuma, S. S.,J. Sci. FoodAgric., 26,393 (1975). (4N) Atuma, S.S.,Lundstroem, K., Lindquist, J., Analyst (London), 100,827 (1975). (5N) Baczyk, S., Swindzinska, K., Mikrochim. Acta, I, 259 (1975). (6N) Bayfield, R. F., Anal. Biochem., 64, 403 (1975). (7N) Bell, J. G., Christie, A. A,, Analyst(London), 99,385 (1974). (EN) Beiliot, J. P., Bourgeois, C. F., Mainguy, P. R., Kieffer, M., George, P., Rev. Fr. Corps Gras., 22, 17 (1975); Anal. Absb., 29,6F44 (1975). (9N) Boatella Riera, J., An. Bromatol., 27, 287 (1975); Anal. Abstr., 31,4F37 (1976). (ION) Bourgeois, C. F., Mainguy, P. R., lnt. J. Vitamin Nutr. Res., 45,70 (1975); Chem. Abstr., 82, 168938d (1975). (1IN) Cavins, J. F., Inglett, G. E., Cereal Chem., 51,605 (1974). (12N) De Ritter, E., Cereal Foods World, 20,33 (1975). (13N) Dompert, W. U., Beringer, H., Fefte, Seifen, Anstrichm., 78, 108 (1976). (14N) Edwin, E. E., Jackman, R., Hebert, N., Analyst (London), 100,689 (1975). (15N) Egberg, D. C., Potter, R. H., J. Agric. Food Chem., 23, 815 (1975). (16N) Fiedlerova, V., Davidek, J., 2.Lebensm.Unters.-Forsch., 155,277 (1974). (17N) Gross, A. F., J. Assoc. Off. Anal. Chem., 58, 799 (1975). (18N) Grys, S., Analyst (London), 100, 637 (1975). (19N) Gupta, D., Sharma, P. D., Gupta, Y. K., Talanta, 22,913 (1975). (20N) Hassan, S.S.M., Abd Ei Fattah, M. M., Zaki. M. T. M., Fresenius' 2. Anal. Chem., 277, 369 1197.51 I -,.
(21N) Holasova, M., Blattna, J., J. Chromatogr.,
123,225 (1976). (22N) Hood, R. L., J. Sci. FoodAgric., 26, 1847 (1975). (23N) Karayannis, M. I., Anal. Chim. Acta, 76,
220R
121 (1975). (24N) Karlsson, R., Talanta, 22, 989 (1975). (25N) Kirk, J. R., Ting, N., J. FoodSci., 40,463 (1975). (26N) Kirk, J. R., J. Assoc. Off. Anal. Chem., 57, 1081 (1974). (27N) lbid., p 1085. (28N) Kraszner-Berndorfer, E., Telegdy-Kovats, L., AbBi. A., Z.Lebensm.-Unters.-Forsch.,154,257 (1974). (29N) Lindquist, J., Analyst (London). 100, 339 (1975). (30N) Marchesini. A., Montuori. F., Muffato, D., Maestri, D., J. FoodSci., 39, 568 (1974). (31N) Matthews, E. W., Byfield, P;G. H., Colston, K. W., Evans, I. M. A., Galante, L. S., Maclntyre, I., FEBSLei?., 48,122 (1974); AnaLAbstr., 29,3D110 (1975). (32N) Moros, S. A., Hamilton, C. M., Heveran, J. E., Donahue, J. J., Oliveri-Vigh, S.,J. Pharm. Sci., 64, 1229 (1975). (33N) Mueiler-Mulot, W., 2.Lebensm.-Unters.Forsch., 154,321 (1974). (34N) Nakata, Y.. Mita, Y., Khono, S., J. Pharm. SOC. Jpn., 96, 53 (1976); Anal. Abstr., 31, 2E31 (1976). (35N) Ogasa, K., Kuboyama, M., Kiyosawa, I., Suzuki, T., Itoh, M., J. Nutr. Sci. Vitaminol., 21, 129 (1975); Chem. Abstr., 83,145916b (1975). (36N) Owen, R. S.,Smyth, W. F., J. Food Techno/., 10,263 (1975). (37N) Parrish, D. B., J. Assoc. Off. Anal. Chem., 57,897 (1974). (38N) lbid., p 903. (39N) Pelletier, O., Madere, R., J. FoodSci., 40, 374 (1975). (40N) Perisic-Janjic, N., Petrovic, S.,Hadzic, P., Chromatographia, 9, 130 (1976). (41N) Petrova, E. A., Ulanova, N. A,, Vop. Pitan., 53 (1974); Chem. Abstr., 82,2721c (1975). (42N) Pfeilsticker, K., Marx, F., Chromatographia, 7, 366 (1974). (43N) Pippen, E. L., Potter, A. L., J. Agric. Food Chem., 23,523 (1975). (44N) Quackenbush, F. W., Banes, D., Derse, P. H., J. Assoc. Off. Anal. Chem., 58,330 (1975). (45N) Randall, V. G., Pippen, E. L., Potter, A. L., McCready, R. M., J. Food Sci., 40,894 (1975). (46N) Ralls, J. W., J. Agric. FoodChem., 23,609 (1975). (47N) Reeder, S. K., Park, G. L., J. Assoc. Off. Anal. Chem., 58, 595 (1975). (48N) Roe, B., Bruemmer, J. H., Proc. fl.State. Hort. Soc., 87, 210 (1975); Chem. Abstr., 83, 1301009 (1975). (49N) Roy, R. B., Conetta, A,, Food Techno/., 30, 94 (1976). (50N) Rymal. K. S.,Rice, C. A,, HortScience, 11, 23 (1976); Chem. Abstr., 84, 1341789 (1976). (51N) Sarwar, M., Iqbal. Z., Zaidi. S..Mikrochim. Acta, It, 699 (1975). (52N) Schlack, J. E., J. Assoc. Off. Anal. Chem., 57, 1346 (1974). (53N) Schmidt, K., Holfelder, E., 2.Le6ensm.Unters.-Forsch., 157,217 (1975). (54N) Senyk, G. F., Gregory, J. F., Shipe, W. F., J. Dairy Sci., 58, 558 (1975). (55N) Soederhjelm. P.,J. Sci. Food Agric., 26, 1469 (1975). (56N) Szasz, G., Gimesi, O., Period. Polyfech., Chem. Eng., 18,203 (1974). (57N) Tortolani, G., Mantovani, V., J. Chromatogr., 92,201 (1974). (58N) Tripet. F. Y., Kesselring, U. W., Pharm. Acta Helv., 50, 312 (1975); Anal. Abstr., 30,5E26 (1976). (59N) Vahlquist, A., lnt. J. Vitam. Nutr. Res., 44, 375 (1974); Anal. Abstr., 29,2D94 (1975). (60N) Waters, R. D., Kesterson, J. W., Braddock, R. J., J. FoodSci., 41,370 (1976). (61N) Wiggins, R. A,, Proc. Anal. Div. Chem. SOC., 13, 133 (1976). (62N) Williams, A. K., Cole, P. D., J. Agric. Food Chem., 23, 915 (1975). (63N) Yao, T., Musha, S.,Bull. Chem. SOC.Jpn.,
ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
48, 435 (1975); Anal. Abstr., 29,4F20 (1975). (64N) Yasumoto, K., Tadera, K., Tsuji, H., Mitsuda, H., J. Nutr. Sci. Vitam., 21, 117 (1975); Anal. Abstr., 30,3D117 (1976). (65N) Zandi, P., McKay, J. E., J. Sci. FoodAgric., 27,843 (J976). (66N) Zhnobibi, A., Firenzuoli, A. M., Bianchi, A,, Boll. SOC.ltal. Biol. Sper., 50, 887 (1974); Anal. Abstr., 29, IF68 (1975). Miscellaneous (1P) Amorim, H. V., Cruz, V. F.. Teixeira, A. A,, Malavolta, E., Turrialba, 25,25 (1975); Chem. Abstr., 83,7515.1(1975). (2P) Bihari, V., Ghosh, P., Chem. Agelndla, 25, 167 (1974); Chem. Abstr., 81, 118562k (1974). (3P) Buckee, G. K., Hickman, E., J. lnst. Brew., 81,399 (1975); Anal. Abstr., 30,4F28 (1976). (4P) Carballido, A., Garcia Olmedo, R., Sousa del Arco, M. P., An. Bromatol., 26, 293 (1974); Anal. Abstr., 29,5F1 (1975). (5P) Chaytor, J. P., Saxby, M. J., Lab. Pract., 24, 407 (1975); Anal. Abstr., 30, I F 2 (1976). (8P) Elkins, E. R., J. Assoc. Off. Anal. Chem., 57, 1193(1974). (7P) Finley, J. W., J. Food Sci., 41, 882 (1976). (8P) Ganzlin, G., Brauwissenschaft, 28, 205 (1975). (9P) lbid., p 231. (IOP) "Instrumentation in Food Analysis", Brit. Food J., 77, 148 (1975); Anal. Abstr. 31, 4F2 (1 976). (11P) Iwasa, K., JARQ, 9, 161 (1975); Chem. Abstr., 84,420882 (1976). (12P) Lees, R., "Lab. Handbook of Methods of Food Analysis", 3rd ed.,Leonard Hill Books, London, 1975, 245 pp. (13P) MacLeod, A. J., Rep. Prog. Appl. Chem., 59,425 (1974); Anal. Abstr., 30,5F1 (1976). (14P) Malkus, Z., Nahrung, 18, 323 (1974); Chem. Abstr., 81,1346562 (1974). (15P) "Methods for Chemical Analysis of Cheese", Brit. Stand. lnst., BS 770: Part 1 (1976); Anal. Abstr., 31, IF23 (1976). (16P) "Official Methods of Analysis of the Association of Official Analytical Chemists", 12th ed., W. Horwitz, Ed., Assoc. Offic. Anal. Chem., Washington, D.C., 1975, 1094 pp. (17P) Olson, N. F., Richardson, T., J. FoodSci., 39, 653 (1974). (18P) "Quality Control Methodology", Society of Soft Drink Technologists, Washington, D.C., (1975). (19P) Salzer, U-J, lnt. Flavours f o o d Addit., 6, 151 (1975); Anal. Abstr., 30,2F32 (1976). (20P) Schaal, M., Bach, R., Rueter, H., Arch. Lebensmiftelhyg., 25, 11 1 (1974); Chem. Abstr., 81, 103319n (1974). (21P) Schaefer, J., Stejskal, E. O., J. Am. Oil Chem. SOC., 51,562 (1974). (22P) Sloman, K. G., Foitz, A. K., Yeransian, J. A., Anal. Chem., 47,56R (1975). (23P) Sterken, E., Kempton, A. G., Develop. lnd. Microbiol.. 15, 226 (1974); Chem. Abstr., 82, 8 4 5 4 8 ~(1975). (24P) "Symposium on Analytical Considerations Pertaining to the Food Labeling Regulations", J. Assoc. Offic. Anal. Chem., 57, 1181-1204 (1974). (25P) "Symposium on Computers in Flavour Chemistry, Chicago, ill., U.S.A.; August 1973", J. Agric. Food Chem., 22,736-770 (1974). (26P) Thielemann, H., Sci. Pharm., 42, 179 (1974); Anal. Abstr., 28,5E10 (1975). (27P) Watt, B. K., Murphy, E. W., Gebhardt, S.E. in "Nutr. Qual. Fresh Fruits Veg.", ARS, pp 29-49 (1974); Chem. Abstr., 83,7196r (1975). (28P) Weetall, H. H., Anal. Chem., 46, 602A (1974). (29P) Wi ldanger, W., Z.Le6ensm.-Unters-Forsch, 159, 165 (1975). (30P) Williams, P. C., Cereal Chem.. 52, 561 (1975).
