Food - Analytical Chemistry (ACS Publications)

A N A L Y T I C A L CHEMISTRY, VOL. 51, NO. 5, APRIL 1979

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Food James A. Yeransian, Katherine G. Sloman, and Arthur K. Foltz” General Foods Technical Center, White Plains, New York 10625

In this review, the authors have again surveyed the literature for advances made in the analysis of foods. The period covered is essentially from October 1976, the end of the interval of our last report ( 9 P ) ,to October 1978. We have continued our practice of citing domestic and the more widely circulated foreign journals in preference to less available publications when work of a similar nature has been reported. “Food Analysis: Analytical and Quality Control Methods for the Food Manufacturer and Buyer” by Lees appeared in its third edition ( I 7 P ) and a revised edition of “Food Analysis: Theory and Practice” was also issued with new sections on HPLC, affinity chromatography, immobilized enzymes, and near IR reflectance spectroscopy (22P). Other reference texts are the seventh edition of “The Chemical Analysis of Foods” by Pearson ( 2 1 P ) , “Developments in Food Analysis Techniques-1’’ edited by King (16P),and the “Manual of Analysis of Fruit and Vegetable Products” by Ranganna (24P). Resources for the food analyst for GLC analysis are “Gas Chromatography in Food Analysis” by Dickes and Nicholas ( 7 P ) and “Analysis of Foods and Beverages: Headspace Techniques” edited by Charalambous (5P).

ADDITIVES Methodology for additives has become as sophisticated as that applied to the determination of harmful contaminants because, indeed, a substance permitted in one country might be the cause for confiscation of foodstuffs in another. Cantafora ( 9 A )prepared a review on analysis of antioxidants in fats. Dilli et al. (14A)detected BHA in the steam distillate of foods by fluorescence at 323 nm after excitation at 293 nm. BHA, BHT, PG, and NDGA from oils and plastic containers were separated by TLC before color development, spot elution, and spectrophotometry in work published by Jayaraman et al. (28A). Hammond (21A) reported BHA, BHT, and three gallate esters to be separable and measurable in a single HPLC oil analysis. A direct GLC separation of BHA and B H T followed acetonitrile hexane partitioning in a method for oils by Senten et al. (49 ). Maruyama et al. (38A)also did direct GLC separation of BHA and B H T , but after steam distillation/solvent trapping.. Buxtorf et al. ( 8 A ) improved extraction efficiency of antioxidants from foods with CH3CN/hexane extraction and partition, following it by GLC of methyl ester derivatives. Dilli et al. (15A) improved both detection sensitivity and GC separation of BHA from B H T by forming the TFA ester of the former antioxidant. T h e heptafluorobutyric acid esters formed from 2-BHA, 3-BHA, TBHQ, and P G enabled Page et al. (44A) to determine these antioxidants in oil samples by electron capture GC. The TAS process of initial volatilization before TLC was used by Winkelmann et al. (64A)to separate and estimate 0.01% BHA in oils. Miyakoshi et al. (41A)analyzed for citric acid and its decomposition products present in oils as antioxidant coingredients by extraction, butyl ester formation, and GLC separation on a DEGS column. Organotin stabilizer compounds were separated by TLC by Woidich et al. (65A). Laub e t al. (35A) used a TAS method before T L C to determine BHA, B H T , as well as various flavors and preservatives amenable to a preliminary vapor separation. Preservatives in milk were determined by Wahbi et al. (63A) by first derivative spectrophotometric techniques. Karasz et al. (31A)reported a fast screening procedure for preservatives in ground beef utilizing spectrophotometric and titrimetric methods subsequent to phosphoric acid extraction. A false positive thiobarbituric acid (TBA) test for sorbic acid in pickled cucumber melon was found due to ethanol by Seto et al. (5OA) and a remedy suggested. Caputi et al. (10A)tested and found satisfactory the “ruggedness” of UV and TBA tests for sorbic acid in wine. Use of H,PO, vapor to codistill acidic

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food preservatives before infrared spectrophotometry was explored by Sudraud et al. (54A). Bennett et al. (6A) injected filtered citrus juice directly into a Partisil 10-SAX column in their HPLC method for sorbate and benzoate. Sorbic acid in wine was directly liquid chromatographed on Zipax SAX by McCalla et al. ( 4 0 A ) . Eisenbeiss et al. (16A) showed separation of sorbic and benzoic acids in wine by direct HPLC on Lichrosorb RP-8. Veta e t al. ( 6 I A ) reported agreement between UV, GC, and their anion-exchange HPLC method for benzoic acid, sorbic acid, and saccharin in foods. A gas chromatographic method for dehydroacetic, sorbic, and benzoic acids was declared more accurate using p-toluic acid as internal standard in work by Ito et al. ( 2 7 A ) . Stark et al. (53A) claimed ability to estimate sorbic acid in cheese at 1 ppm using steam distillation and partition before GC. Toyoda e t al. (60A) worked on methods of separating and extracting sorbate, dehydroacetate, benzoate, salicylate, and p-hydroxybenzoates from solid and liquid food matrices before GLC. Steam distillation was used by Matuzawa et al. (39A) to first separate 4-hydroxybenzoates from soya before GC of trifluoroacetate esters. “Tego” preservatives in gelatine were extracted and identified by TLC of their dansyl compound patterns in an investigation by Hess e t al. ( 2 2 A ) . Alkaline hydrolysis before photometric or titrimetric estimation was employed by Kainz et al. (30A) to find bromine-containing preservatives in wine. Methyl and propyl-hydroxybenzoate separation on paper and thin-layer chromatograms was the subject of a n effort by Thielemann ( 5 9 A ) . A reductochromotropic acid method for bromate in flour, valid in the presence of persulfate and nitrite, was reported by Lotez Fernandez et al. (37A). O’Neill e t al. (42A) employed ‘P Fourier-Transform NMR to detect polyphosphate changes in chicken and fish. An AOAC nitrite collaborative study was reported by Fiddler (18A) where substitution of N-l-naphthylethylenediamine and sulfanilamide for Griess reagent were recommended. Hilsheimer et al. (23A) also recommended safer alternative color reagents for modification of the AOAC nitrite method. Perryman (45A) discussed a faster extraction of nitrite from meat using a paddle homogenizer. A method for nitrites and nitrates in meat based on nitration of benzene before EC-GLC was developed by Wu et al. ( 6 6 A ) . Ishizaki et al. (26A) reacted nitrite with o-phenylenediamine after ion-exchange cleanup and before GC determination. The use of a nitrite ion-selective electrode gave good recovery results for smoked fish samples examined by Sherken ( 5 1 A ) . High sensitivity and selectivity for nitrite traces were reported by a differential pulse polarographic approach taken by Chang et al. ( I I A ) . Emulsifiers consisting of polyglycerol esters were fractionated on silica gel before their components were GC analyzed by Schuetze (47A). Lehmann et al. (36A) performed TLC separation before and after hydrolysis to identify extracted diacetyl tartrate esters and Ca stearyl-lactate from baking samples. A scheme for elucidation and measurement of food polyglycerol ester emulsifiers using extraction, saponification and GC of TMS derivatives was published by Dick et al. (13A). Coupek et al. (12A)detailed ways to analyze for glycerol ester emulsifiers using adsorption or gel-permeation chromatography as a first stage. A method for silicone in vegetable oil using sample saponification before extraction and graphite furnace atomic absorption was given by Jundu (34A). Beer was hydrocarbon-extracted and then the solvent evaporated and the residue dissolved in MIBK before nitrous oxide flame atomic absorption in the Baker et al. (3A) method for silicone antifoam. Silicone in soluble coffee was chloroform extracted, wet ashed, and measured as molybdenum blue in Kacprzak’s (29A) method. IC 1979 American Chemical Society

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A comprehensive review of analytical methods for artificial sweeteners in food was compiled by Page et al. (43A). Kat0 (32A) discussed various approaches to saccharin analysis in his review. Visible extinction at 510 nm was used by Tanaka et al. (57A) in their saccharin method wherein a beverage extract was reacted with phenothiazine. Saccharin was polarographically determined in beverages and chocolate after a column-type extraction in a technique by van der Dungen (62A). Photometric cavity emission of S2at 384 nm was used by Belcher et al. ( 5 A )t o analyze beverages for saccharin. A method by Hoshino e t al. (24A) methylated saccharin with NJV-dimethylformamide dimethylacetal before FID or EC gas chromatography. A sulfur specific photometric detector was used by Hosoya e t al. (25A) to detect methylated saccharin subjected to GC. Eng et al. ( 17 A ) performed a reverse phase H P L C separation of saccharin from chewing gum after toluene/water partition and filtration. Takatsuki et al. (56A) reported an anionic liquid column separation along with preservatives. Wine samples were analyzed by reverse phase H P L C in a paper by Tenenbaum e t al. (58A). Szinai et al. (55A) employed pyrolysis/GLC to identify saccharin in beverages. Roll e t al. (46A) recommended methyl stearate as internal standard in the Codex method for G- and p sulfonamides in saccharin. An isotope dilution technique was published by Shimada e t al. (52A) where they measured Na cyclamate in canned seafoods. A strong cation-exchange column and medium pressure liquid chromatography gave a method for the sweetener L-aspartyl L-phenylalanine in a paper by Fox e t al. (20A). Reverse phase C-18 separation allowed Fisher (19A) to resolve neohesperidine dihydrochalcone from grapefruit juice in a H20/CH3CNmobile phase. Schwarzenbach (48A) used reversed phase HPLC with MeOH H 2 0 for this sweetener in drinks, yogurt, and chewing gum. ato (33A) reviewed analysis of sweeteners including sugars and sugar alcohols. Bark ( 4 A ) gave a method for sorbitol in foods based on thermometric titration with NaI04. Techniques of precipitation and colorimetry composed a method for alginate, carageenan, and furcellaran in beer in work by Buckee et al. (7A). Armand et al. ( I A )extended TLC and enzymic methods for monosodium glutamate to new foodstuffs types. Armoux et al. ( 2 A ) adapted an enzymic method for MSG to an automatic centrifugal analyzer.

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ADULTERATION, CONTAMINATION, DECO MP 0S IT1 0 N Some interesting approaches have been published capable of detecting adulteration by the presence of species from a logical adulterant. Oke e t al. (146B) found a carotenoid pigment, separable by TLC and contributed by red pumpkin when present in tomato ketchup. Benk et al. (15B)detected marigold extract in orange juice products, adopting an alumina-HPLC method for the separation of the xanthophyll dipalmitate fraction. Schmidt e t al. (185B)distinguished natural and synthetically derived acetate in vinegar by diisopropyl ether extraction and 14Ccounting. Sandoval (180B) employed polarography to detect other co-occurring compounds in differentiating natural and synthetic vinegars. In a method to detect colophony in asafoetida, Banerjee et al. (9B)separated abietic acid by TLC. Bhagya (16B) claimed superior selectivity in his TLC method for capsaicin in ginger. A thin layer method permitted Sen et al. (194B) to detect 1% of black caraway in caraway using a 2,4-DNPH reagent. GLC separation was used by Tateo (222B) to determine the quality of peppermint oils as well as the presence of some specific adulterants. Balderstone et al. (8B) found that they could detect argemone oil in other edible oils by a TLC technique for sanguinarine. A way to detect argemone oil by solvent extraction and spectrophotometry of its alkaloids was given by Pundlik et al. (166B). A phosphoric acid reagent developed the TLC spot color used by Sengupta et al. (196B) to detect tobacco seed oil in sesame oil. Various other oils were screened for pongam oil adulteration in a TLC-fluorescent spot method by Srinivasulu et al. (207B). Leone e t al. (113B) discussed the utility of profiling sterols by GLC as means of detecting olive oil adulteration. Mani et al. (124B)used selective enzyme hydrolysis to detect esterified olive oil by increased 2-position palmitate. Bracco et al. (23B) found that higher 2-position palmitate abundance in lard allowed him to detect 5% of suet in lard by a TLC-GC procedure. A standard test (24B) was published for detection of vegetable fat in dairy products by

microscopically identifying phytosterol crystals. Foreign fats in dairy products were also detected by a GC reference method (25B) wherein 0-sitosterol was identified by retention time. Carisano et al. (28B),in looking for adulteration of butter, separated triglyceride fractions by TLC before enzyme hydrolysis to eventually profile the fatty acids of the monoglycerides created. A fast colorimetric test enabled Mittal et al. (135B)to detect ammonium sulfate added to buffalo milk. These authors (136B)also showed a colorimetric way to detect urea added. T h e presence of 1%vegetable protein in meat was shown detectable by Lacourt et al. (108B) in their polyacrylamide gel-electrophoretic separation. Baudner et al. (13B)gave a method for soya protein in heated meat products based on carrier-free electrophoresis and then immunoassay. Beljaars et al. (14B) compared techniques of electrophoresis and immunodiffusion for caseinate and soy isolates in meat, concluding that both are valid. Fischer et al. (55B) analyzed for canavanine as specific indicator of soy protein in meat. T h e Ouchterlony immunodiffusion test for soya in meat was evaluated critically in a study by Hammond et al. (72B). Foreign proteins in meat, with emphasis on soy, were examined by a polyacrylamide gel-electrophoretic separation in work by Homayounfar (80B). Kotula et al. (104B) reported soy-in-cooked beef electrophoretic patterns. The presence of spleen added to ground beef was measured by Bittel e t al. (I 7 B ) by determination of insoluble iron as hemosiderin. Blood added to ground beef was measured by Karasz et al. (99B)by differentially precipitating hemoglobin from myoglobin in water extracts before reading the former as cyanomethhemoglobin at 422 nm. Rangely et al. (168B) used ion exchange to separate methylamino acids as indices of meat-protein content. Contamination in the food supply continues to provide challenge to many researchers, since traces of materials formerly considered innocuous become significant in light of biological studies published. A large review by Bruni e t al. (26B) discussed analytical methods for many types of food contaminants. A review of sampling plans and method for aflatoxins already collaboratively studied was compiled by Schuller et al. (186B). Kingston (103B) reviewed the use of mass spectrometry for mycotoxin analysis. Shotwell (200B) reviewed methods and data for aflatoxins in corn. Higher aflatoxin recoveries were found for AOAC method 26.037 than 26.020 when they were applied to corn by Shotwell e t al. (201B). Barabolak (10B) combined several other methods to produce a procedure for aflatoxins in corn and its products, extracting with acetone, partitioning into benzene, and cleaning up on silica gel-alumina before TLC. A procedure by Seitz et al. (193B) for aflatoxins in corn, claimed to give results equivalent to AOAC procedures but by using safer solvents. Alexander et al. ( 3 B ) used a two-dimensional TLC separation accomplished in less than an hour in their aflatoxin in corn method. A screening method for mycotoxins in feeds where a dialysis tube was used as a clean-up step was reported by Patterson et al. (157B). A new benzene-ethanol-water solvent system for separating aflatoxins extracted from roasted peanut products was developed by Waltking e t al. (237B). A correlation between the diffusate through a cellulose dialysis tube from groundnut 3 and aflatoxin levels by the Pons method were shown by Basappa et al. ( I I B ) . Pons et al. (164B)gave further purification and clean-up steps necessary to eliminate HPLC aflatoxin interferences in a cottonseed method. A clean-up routine to make HPLC analysis of groundnut extracts less interference prone was detailed by Lansden ( I I I B ) . Blanc et al. (18B) in their HPLC aflatoxin separation on silica gel, claimed double the sensitivity of TLC. Isohata et al. (88B) obtained good individual aflatoxin HPLC separations on silica gel and could use porous polymer bead columns to separate B and G groups from patulin and penicillic acid. Trucksess et al. (231B) released aflatoxin B1 from egg protein with salts of urea in their thin-layer method. A TLC method for animal tissue aflatoxin contamination was described by Jemmali et al. (96B). Thurm (227B)compared thin-layer separations of aflatoxins B1 and GI and MI and M2on coated aluminum foil plates vs. glass plates and concluded the former to be faster and more sensitive. Issaq et al. (89B) described methods t o distinguish between interfering ethoxyquin and aflatoxin Bl, primarily by the difference in their fluorescence excitation maxima, 348 nm vs. 366nm, respectively. Fritz et al. (59B) analyzed milk and dairy products for Ml and B1 by a mod-

ANALYTICAL CHEMISTRY, VOL. 51, NO. 5, APRIL 1979

Arthur K. Foitz, Senior Research Specialist at General Foods Central Research Analytical Laboratory, has a background of past experience as an analytical "generalist" concentrating heavily on chromatographic approaches. He now heads a group specializing in new analytical methodology and special request analyses for research and quality control applications. The exploration and evaluation of new instrumental and computer automation developments are among his recent responsibilities, as well as trace additive and environmental problems. Memberships include ACS and ASTME-19. 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 a 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 quality 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 U S delegaton of the Codex Alimentarius CommMee on Analysis and Sampling. Katherine G. Sloman, Senior Research Speclalist, 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 w t h the problems encountered both in method 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

ification of the method of Schuller et al. (187B) after evaluating methods for M1 in milk, favored two-dimensional TLC and densitometry. Takahashi (221B)modified an earlier HPLC separation for aflatoxins in wine and fruit juice by conducting a preliminary cleanup on silica gel before the analytical silica adsorption column. This author (220B)also investigated several reversed phase columns reporting them more satisfactory for the separation of Bl, B,, G1, G2, and also B,, and G2, generated by trifluoroacetic acid treatment. Stubblefield et al. (218B) reported using HPLC on CISreversed phase to separate MI, M2, B1, B2, GI, and G, in a method for corn and also used preparative HPLC to isolate aflatoxins. Hunt et al. (83B) subjected aflatoxins and ochratoxin A to HPLC separation with fluorescence detection on 5-pm silica after first separating fluorescent bands by TLC in a method applied to various foods. A large improvement in detection sensitivity was reported by Panalaks et al. (155R)when they used a flow cell in their fluorescence detector packed with the same silica gel as their analytical column. Zimmerli (248B)packed his spiral flow cell with 0.1 to 0.2 mm silica gel and reported sensitivity gains of three to several thousand, depending on the aflatoxin species. A study by Haddon et al. (69B)stated that because of losses suffered by adsorption after extensive cleanup. better trace aflatoxin confirmation by mass spectrometry was accomplished by partial cleanup and selected ion monitoring. Holaday (76B) published a rapid screening method for aflatoxins and ochratoxin A using simple apparatus and suitable for field use. Josefsson et al. (98B) described a screening method for cereals using sephadex LH-20 before TLC to detect aflatoxins, ochratoxin, patulin, sterigmatocystin, and zearalenone. Levi et al. ( I 16B) reported investigations relevant

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to the occurrence of mycotoxins in coffee. Hald et al. (70B) made use of silica gel mini-columns to screen barley for ochratoxin A. Engstrom et al. (48B) separated aflatoxin B1 and GI as well as ochratoxin A, zearalenone. rubratoxin B, patulin, and penicilic acid on a C18 reversed phase column using UV detection. Hult et al. (82%) made use of carboxypeptidase A-induced hydrolysis to differentiate ochratoxins A and B by relative fluorescence changes when both were present. An improvement in specificity for a thin-layer method was reported by Sarudi (181B) by reducing zearalenone with NaBH, before spotting. Methods using both reversed phase HPLC and EC-GLC as pentafluoropropionyl derivatives were given for zearalenone and zearalanol by Holder et al. ( 7 7 B ) . A reagent of bis-diazotized benzidine gave Malaiyandi et al. (122B)a more specific reaction for visualizing zearalenone on TLC plates. Hunt et al. (84B)analyzed foods for zearalenone, patulin, and penicillic acid by following a silica gel cleanup by HPLC on an Alox column before final HPLC on Lichrosorb. A method by Isohata et d. (87B)determined patulin and penicillic acid in mouldy rice by HPLC on a porous polymer column with UV detection. Salem et al. (178B),after a silica gel column cleanup and TLC, intensified the patulin fluorescence with ammonia before fluorodensitometry in a method for apple juice. Chlorobenzidine as a spray reagent permitted Meyer et al. (132B)to detect down to 5 pg of patulin on a TLC plate by UV long wave fluorescence. Stinson et al. (216B)formed the 2,4-dinitrophenylhydrazoneof patulin on a column before a TLC separation and absorbance measurement. Polzhofer (161B)developed his TLC plates with two solvents followed by densitometry at 273 nm in a method for apple juice. This author (162%) also determined patulin in other fruits and vegetables down to 40 pg/kg. Frank et al. (57B)also reported patulin occurrence in fruits affected with spontaneous brown rot. After formation of the acetate, Ralls et al. (167B) measured patulin in cider vinegar by GC-MS, monitoring the 136 m / e response. A combination of GPC and reversed phase HPLC was employed by Stack et al. (208B) to determine down to 10 pg/kg of sterigmatocystin in corn and oats. Shannon et al. (198B) extracted this mycotoxin from grains and soya beans with methanol-4% KC1 solution and cleaned up on Florisil before an AOAC TLC separation. An improved TLC method for sterigmatocystin in grains was developed by Athnasios et al. ( 5 B ) which avoids column cleanup through solvent partitioning and enhances fluorescence with an A1C13 spray reagent. Engel ( 4 7 B ) after TLC, used AlCl, and heating to form a sterigmatocystin fluorescent derivative for measurement. A GC-MS procedure by Salhab et al. (179B) could detect down to 5 ppb of this toxin after extraction and partition cleanup from grains. Toxins resulting from Fusarium sporotrichiella growth in grain were detected by UV exposure of a developed TLC plate in a technique by Olifson et al. (147B). Pober et al. ( I 5 9 B ) utilized a conditioning step for rabbit anti-staphylococcal enterotoxin B along with some cleanup to increase sensitivity of a radioimmunoassay method for food samples. A colorimetric measurement at 555 nm after peroxide and diacetyl reactions enabled Gershey et al. (60B)to analyze for saxitoxin in clams. Pareles et al. (156B) reported a method for T-2 and HT-2 toxin in milk based on monitoring ion fragments a t m / e 436 and 350 in a gas chromatograph-mass spectrometer. Nitrosamines in foodstuffs was the subject of a review by Crosby (31B)in which methods were discussed. Tinbergen et al. (228B3 edited the "Proceedings of the Second International Symposium on Nitrite in Meat Products", in which various analytical techniques for nitrosamines were included. Walker et al. (236B) edited the presentations made at a conference on "Environmental N-nitroso compounds analysis and formation". Fine ( 5 4 B ) compared chromatographic GC detectors useful for volatile nitrosamine analysis, namely GC-MS, Coulson conductivity, and thermal energy analysis. Dressel (40B) described his analysis of vegetables for volatile nitrosamines by GC-alkali flame detection. Dough et al. (63B) screened for volatile nitrosamines by decomposing them to nitric oxide at the exit of a GC column but ahead of a mass spectrometer. Groenen et al. (65R) coupled capillary GC with MS to analyze meat products for eight volatile nitrosamines, tuning to the specific m / e fragment for each. Five nitrosamines were measured in raw and cooked bacon and luncheon meat using GC-thermal energy analysis by Fine et al. (53B).

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Gough e t al. (62B) found, in comparing thermal energy and MS detection of GC separations, that parent-ion monitoring with peak matching was most accurate for the latter. Eisenbrand et al. (46B) analyzed for volatile nitrosamines by direct GC and pyrolytic electrolytic conductivity detection as well as by forming heptafluorobutyramides before GC-MS with detection of the CBFT m / e 169 fragment. Eisenbrand et al. (45B) also formed fluorinated-TMS derivatives of nitrososarcosine, nitrosoproline, and N-nitroso-2-hydroxyproline before GC with FID or MS single-ion monitoring. A method for N-nitrosoamino acids in meat products was given by Dhont (37B) t h a t yielded a cleaned-up extract for photolysis, polarographic, or GC final measurement. Sen et al. (195B),in their GC-mass spectrometric method for 3-hydroxy-1nitrosopyrrolidine traces, methylated it to the o-methyl ether before chromatography and monitored a t high resolution for m l e 29.9980 and m l e 130.0742. Janzowski et al. (94B) analyzed for this nitroso-amino acid by direct GC-thermal energy detection and confirmed t h e levels by GC-MS of its trifluoroacetyl derivative. Kubacki et al. (206B) detected nitrosopyrrolidine in meat at the ppb level, modifying a GC-EC method to use a steam distillation. Hansen et al. (73B)used GC-thermal energy and HPLC with UV and photohydrolysis detection to investigate whether nitrosoproline is a precursor of nitrosopyrrolidine. The photohydrolytic technique for H P L C detection of N-nitro compounds was described by Iwasoka e t al. (90B),who used Griess reagent to react with the NO2- formed. A simplified chemiluminescence detector for GC screening food extract for nitrosamines was built by Gough et al. (61B),decomposing them to NO on a hot W 0 3 catalyst before the ozone interaction. Wolfram et al. (247B) gave two methods for sensitive analysis for N-nitrosoproline; one a n HPLC-fluorescence detection of the NBD-proline formed after denitrosation; and the second, FID-GC of the methyl ester of nitrosoproline. Baker e t al. (6B)analyzed for this compound in meat samples. Ray ( 170B) determined cyclic N-nitrosamines in fish by direct GC of hexane extracts. Sebranek et al. (189B) investigated water soluble reaction products of nitrite in cured meat, profiling Sephadex G-10 separation of I5N labeled fractions. A chemical method by Olsman e t al. (148B) released protein bound NO2- from meat extracts with Hg2+ before final determination using Griess reagent. T h e formation of N-ethoxycarbonylproline and N-ethoxycarbonylglycine in wine and model systems from interaction of diethylpyrocarbonate and the precursor amino acids was shown by GC-N-specific separation method results obtained by Baker et al. (7B). Ough et al. (150B) investigated the chances of forming methyl carbamate in wine from dimethylpyrocarbonate. Joe et al. (97B)confirmed the presence of urethan in wines detected by GC-alkali flame ionization with GC-MS. Quantitative procedures for 5-hydroxytryptamide-carboxylic acid compounds in green and roasted coffee were discussed by Kummer et al. (107B)and two alternates of their own T L C procedure given, one with spectrofluorimetric measurement after spot extraction and the other by color absorbance on the plate after Gibbs reagent reaction. Dyer e t al. (43B) determined p-asarone in wines and flavors by distillation, hexane partition a n d GC on SPlOOO and the results of the collaborative study of the method reported by Dyer (4223). Liddle et al. (I27B)gave a method for P-asarone, thujone, safrole, and coumarin in vermouth based on liquid-liquid extraction before GC-MS. d-Asarone was determined spectrofluorimetrically by Wojtowicz (246B)after steam distillation and hexane partition. Merat et al. (130B) examined aperitifs for P-aserone and a- and P-thujone by extracting distillates with ether-pentane before GC and confirmed identities by TLC. Pons (163B) reviewed analytical methods for free and total gossypol. Shain et al. (197B)used T L C separation, developing fluorescent spots with H 3 P 0 4in a method for sapogenins. Solanine alkaloids were extracted and measured by TLC and also as T M S derivatives by GC in a method applied to potatoes and leaves by Roosen-Runge et al. (174B). Osman et al. (149B),after extraction, hydrolyzed solanidine and demissine glycoalkaloids with H2S04before GC of solanthrene and demissidine. Total glucosinolates in vegetables of the mustard family were separated first by anion exchange and then hydrolyzed on the column using thioglucosidase by Van Etten et al. (235B),who then measured liberated glucose. T h e aglycones from the preceding were

determined by temperature-programmed GC by Daxenbichler et al. (34B). A method to estimate vicine and convicine in extracts of fava beans was outlined by Collier (30B) and was based on UV spectrophotometry. A review by Guenther (66B) discussed hormonal residues in meat associated with fattening. Ryan e t al. (175B) confirmed the presence of stilboestrol in beef liver, first by GC of its trifluoroacetate, followed by hydrolysis and conversion to heptafluorobutyrate with GC again for measurement. Lawrence et al. (122B) investigated electrolytic conductivity and electron capture for GC detection systems for heptafluoro derivatives of stilboestrol in beef and carbofuran in turnips. An EC-GC method for melengestrol acetate in meat was studied collaboratively and reported by Krzeminski et al. (105B). Residues of oestrogens in meat and organs were measured by Jarc et al. (95B)using one- and two-dimensional TLC. Ingerowski e t al. (85B) utilized competitive uterine receptor binding behavior between oestrogens and radiolabeled oestradiol to screen meat samples, counting the cytosol fraction by liquid scintillation. A GC procedure by Holland (78B) for melengestrol in feeds and meat utilized EC detection after extraction, partition, and column cleanup steps. Winkler et al. (243B) examined tissue for progesterone residues, first performing a TLC separation and then either radioimmuno assay or GC with chemical ionization MS detection. Estradiol in feeds was analyzed in a scheme by Bowman et al. (22B) with extensive partition and column cleanup before EC-GC as pentafluoropropionyl derivative. Trenbolone traces in meat were detected by fluorescence of TLC spots by Laitem et al. (109B). Oxytetracycline residues in meat and fish were measured fluorimetrically in a borate buffer after extraction, XAD-8 chromatography and acid conversion into apo-oxytetacycline in the procedure of Sasaki et al. (182B). Honikel et al. (81R)gave a fast method for chlortetracyline based on fluorimetry of t h e Ca2+-barbitone complex. Polger et al. (160B)discussed methodology details for tetracycline residue analysis by fluorimetry. A polarographic method for robenidine traces in chicken was published by Smith et al. (205B). Seefeld et al. (290B)used tritium EC-GC to measure trimethylsilylated chloramphemicol extracted from potatoes. Natamycin on cheese surfaces was shown to be estimable by spectrophotometry in the paper by Frede (58B). Bossuyt et al. ( 2 I B ) employed TLC followed by bioautography to detect various antibiotics in milk. Milk was examined for levamisole residues by Smith e t al. (204B) who detected their GLC effluent thermionically. Bogan (20B) measured diethylcarbamazine in meat, extracting first before FID-GC. Ritchie et al. (172B)converted extracted nitrofuran drug traces into 5-nitro-2-furaldehyde hydrazones before partition, cleanup, hydrolysis, and EC-GC. A method to recover 2-(2-furyl)3-(5-nitro-2-furyl)acrylamide from sausages by TLC analysis was reported by Kawana et al. (101B). XAX was detected down to 0.1 pg in animal fat in a thin-layer method by Luckas (129B). Residual nicotine in milk and blood was determined using TLC, GC, and MS by Bluethgen et al. (19B). Triclosan contamination of blood and fish was quantified by EC-GC after solvent cleanup in the procedure of Hoar et al. (75B). Quarternary ammonium disinfectants finding their way into milk products were measured with fewer interferences as eosin complexes in a method by Wildbrett et al. (240B). Gupta et al. (68B) modified a titanium-complex method for H 2 0 2in milk to improve sensitivity. Ohhashi et al. (144B)described the operation of a commercial analyzer for H202 in foods that used a n oxygen electrode. Ackermann et al. ( I B ) gave a procedure for hydroxyzine in meat and milk based on a TLC separation and sensitive to sub-ppm amounts. Remaining traces of refrigerant-12 in prawns frozen by immersion were measured in a headspace GC technique by Carter et al. (29B). Page e t al. (152B) gave their procedure for residual methylene chloride and trichloroethylene solvents in coffee, employing GC-EC and halogen conductivity detectors after a vacuum distillation. Maini (121B) detected anthraquinone on plants by electron capture GC after extraction and cleanup on silica gel. Remaining food traces of 1,3-dichloropropene, 1,2-dibromoethane, and 1,2-dibromo3-chloropropane fumigants were acetonitrile extracted, hexane partitioned, and determined by Newsome et al. (142B) after Florisil cleanup. Stijve e t al. (215B) investigated ethylene chlorohydrin incidence in ethylene oxide treated foods, using gas chromatographic and TLC methods. Azodicarbonamide

ANALYTICAL CHEMISTRY, VOL. 51, NO 5, APRIL 1979

levels in wheat flour were determined by conversion to hydrazine which was then reacted with 4-dimethylaminobenzaldehyde for spectrophotometry in a procedure by Weak et al. (239B). Van Cauwenberge et al. (234B) compared colorimetric and X-ray fluorescence methods for bromine residues in crops grown in bromomethane-treated soil. Stijve (214B) modified a GC procedure for determining inorganic bromide from fumigated foods as 2-bromoethanol, so interferences were lessened. A capillary GC method to detect 2-phenylphenol in citrus essences was reported by Rispoli et al. ( 1 7 I B ) . Nose et al. (143B) quantified traces of this fungicide by forming the pentafluorobenzyol derivative for electron capture detection. Thiourea in citrus rind was measured by colorimetry and TLC methods by Mandrou et al. (123B). Farmer et al. (SOB) used a copper wire test to detect sulfur dust in copra. Cyanide from amygdalin was reacted with picric acid in a colorimetric test by Egli (44B). Nahrstedt (138B)reported replacing benzidine with safer anthranilic acid in the Aldridge method for cyanide traces. Wisser (244B) examined wine for cyanide traces using differential pulse polarography in the presence of thallium ion. A GC procedure for cyanide in wine was described by Bates et al. (12B) that formed cyanogen bromide for EC detection. Vinyl chloride monomer traces transferred to oils were determined in a headspace GC method by Page et al. (153B) where they used electrolytic conductivity halogen detection. Morano et al. (237B) studied partition of VCM t o food simulation model systems to predict behavior. VCM residues in foods and packaging was determined by GC after gas stripping or solvent dissolution in work by Kat0 et al. (IOOB). A headspace method was also used by Diachenko et al. (38B) to measure VCM in corn oil and simulating systems. P u et al. (165B) used solvent extraction techniques to analyze foods, containers, and simulating systems. Figge (52B) described apparatus and techniques for following the migration of food substances into packaging and vice versa using radiolabeled tracers. Spectrophotometry of tin as a quercetin complex was utilized by Uhde e t al. (233B) to monitor the transfer of organotin stabilizers into food system simulants. An acetonitrile-hexane partition-extraction and Florisil cleanup enabled Saito et al. (1 77B) to study phthalate migration into oils without pesticide interference. Traces of phthalates in fish were recovered by Ueta et al. (232B) in developing their method based on solvent, extraction and GC. Maruyama et al. (125B) used a volatile oil distillation apparatus to separate phthalates from food samples before GC, also adding zinc to the refluxing solution and a Florisil cleanup t,o eliminate pesticide and P C B interferences. Plasticizers that had transferred from PVC films to meat were extracted, saponified, and monitored by GC of their alcohols in a report by Daun et al. (33B). Benzophenone-type UV stabilizing chemicals used in polyethylene were tested for migration tendencies by TLC analysis of food simulant systems in the work of Mazur et al. (129B). Roesli et al. (1 73B) used a reflux distillation-extraction into a hexane trap to determine styrene residues in milk by GC. Withey ( 2 4 j B ) reported analyzing for styrene monomer levels in yogurt and containers. A method for polyethylene in fats was described by Seher et al. (191B) using infrared spectra for identification. Twenty-six amines were separated by TLC in the method of Herraiz et al. (74B)who investigated contaniinatioii of beer and wine by epoxy-lined containers. T h e contamination of chicken meat by chlorophenols was studied by Farrington et al. (51B) who derivatized them with l-fluoro-2,4-dinitrobenzene in an extract before EC-GC. Erne?; (49B) reported pentachlorophenol (PCP) residues in milk, determined by GC of the acetate derivative. Lamparski et al. (11OB) analyzed for P C P , and hexa- as well as octadichlorodibenzo-p-dioxins in milk using GC-EC and MS after methylation of PCP. A TLC investigation for phenols and substituted phenols as causes of milk taint was reported by Stannard et al. (209B). Luride et al. (120B)studied fat-soluble chlorinated compounds in fish, analyzing solvent extracts by neutron activation analysis for halogens and by EC-GC for chloro compounds. Khan et al. (102B) in a review, cited methods for PCB determination in foods. PCBs from meat were separated before chromatography by Kawamura et al. (145B) using a continuous steam distillation--heptane trap apparatus. Trotter (230B) employed a UV photolysis--decomposit,ion t,reatment to confirm hexabroniobiphenyl traces derived from foods. Sawyer (184B)reported on a collaborative

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PCB method study comparing total response to individual peak measurement and found both valid. A preliminary study (183B) to the collaborative one had indicated an advantage for individual peak quantification. Rice oil was studied for polychlorinated dibenzofuran contamination by Rappe et al. (169B) using splitless glass capillary GC and single ion monitoring by MS. Shiraishi (199B) reviewed methods for benzo[a]pyrene analysis. A large review on the analysis of smoked foods was prepared by Hamm (71B) covering polycyclic compounds. Residual contamination of fats and feed meal from rendering plants was investigated by Ingr (86B)who injected headspace samples t o analyze for tetrachloroethylene and gasoline hydrocarbons by FID-GC. Watanabe et al. (238B) reported as GC method for linear alkyl benzenesulfonates as contaminants of water and plant material that followed ionexchange separation with PClj reaction to form the alkyl benzenesulfonyl chlorides for chromatography. A technique by Nakamura et al. (139B) identified dibenzothiophenes in oysters as sulfur-containing pollutants from oil contamination, using FPD-GC or MS after an alumina column separation step. Tissues were analyzed for organolead content by Sirota et al. (202B) using flameless AA after benzene extraction and H N 0 3 digestion. Various methods for detecting aliphatic and aromatic hydrocarbons in marine organisms were compared by Gritz et al. (64B),namely direct vs. extract-saponification as clean-up steps preceding a column cleanup and GC. Nakanishi et al. (140B) detected paraffin type hydrocarbons in fish and meat by GC peak patterns and also employed chromate oxidation in establishing base-line levels. Panalaks ( l 5 4 B ) used HPLC-spectrophotometric and fluorescence variations to identify and quantify polycyclic aromatic hydrocarbons in many smoked and charcoal broiled foods. Jahr et al. (92B) looked specifically for benzo[a] and [elpyrene in smoked meats, employing GC-MS with ion fragment monitoring to provide specificity. A method for detecting benzo[a]pyrene and benzo[ghz]perylene in shellfish was reported by Guerrero et al. (67B),separating on CI8 reversed phase with UL‘ detection at 383 nm during H P I L D u m (41B) digested marine meat samples in KOH before isooctane extraction, column cleanup. TLC separation, and spectrofluorimetry. A method by Saito et al. (176B)for benzo[a]pyrene in foods used an intermediate partition into concentrated H 2 S 0 4and silica gel column cleanups before spectrofluorimetry. The stability of benzo[a]pyrene on TLC plates was investigated by Seifert (192Bi to deduce if fluorescence scanning changed the species responding, and a treatment to stabilize the plates was given. Skinner et al. (203B)discussed special apparatus to selectively adsorb polycyclic hydrocarbons from mineral oil during its analysis. Capillary GC provided resolution necessary to identify 14 polycyclic aromatics isolated from corn in the work of Winkler et al. (242B). hlasuda et al. (127B) added 3H labeled benzo[a]pyrene to food extracts in their method and after TLL measured the total by fluorescence and the “spike” by scintillation counting to determine recovery. Wilks et al. (241B)reported an improvement in the analysis of caramel color for 4-methylimidazole, extracting on an alkaline celite column with methylene chloride and measuring by GC against 2-niethylimidazole internal standard. Stavric (213B) identified 11 major impurities extractable from saccharine by solvents, using FID-GC and MS. A liquid chromatographic procedure for traces of CT- and p-sulfamoylbenzoic acids in saccharine by Nelson (141B) accomplished separation on a high resolution anion-exchange column. Residues of o-toluenesulfonamide in saccharin were measured by direct GC in the method of Janiak et al. (93B). Pachla et al. (151B)inferred insect infestation in grain products and sugar by the uric acid they could measure by ion-exchange HPLC, detecting this species by thin-layer amperometry a t +0.8 V vs. Ag/AgCl. Asbestos fibers were membrane-filtered from beer, ashed, and refiltered on 0.1-pm membranes before scanning electron microscopy by Maurer et al. (128B). Sperduto et al. (206B) used microscopic fluorescence to differentiate amphibole and serpentine asbestos fibers after morin treatment. The two surfactants, IgepalC0630 and Na dodecyl sulfate, were found equivalent in use for defatting in analyzing chocolate liquor for extraneous matter by Mastrorocco et al. (126B). Thrasher et al. (226B) reported a collaborative study for light filth in paprika. A flotation method variation for light filth in capsicum was

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reported by Thrasher et al. (225B) to be superior to AOAC 44.123. Thrasher (224B) also listed collaborative results for a ground mace and caraway method. Canned crabmeat was subjected to a collaborative study by Dent et al. (36B) to determine light filth. This author (35B) also reported collaborative study of modifications to AOAC 44.120 to improve performance in spice analyses. Decomposition in foods is usually difficult to quantify objectively, except by count of microbiological growth, since most tests are based on amounts of normal substances differing from a “norm”. Albrecht e t al. (2B)used an enzyme method to correlate pyruvate with milk spoilage. Meydav et al. (131B) measured 5-hydroxymethylfurfural with thiobarbituric acid in an effort to assess browning precursors in orange juice products. The compound octa-l-cis-5-diene-3-one was identified by Swoboda et al. (219B) as a “metallic” odor in oxidized butterfat. Stockhausen et al. (217 B ) detected irradiated meat by a decrease in thiol groups as measured by photometry. Factors important in the accuracy of a resazurin test for meat quality were discussed by Holly et al. (79B)and Dodsworth et al. (39B) covered its industrial utility. Andrews e t al. ( 4 B ) measured formaldehyde in mechanically deboned turkey meat with a 3-methyl-2-benzothiaolinone reagent. A simple test for fish freshness was given by Jahns et al. (91B) which used resaurin-xanthine oxidase test strips dipped into acid-homogenized sample filtrate. Schutz e t al. (188B) described a TLC screening method, detecting histamine with ninhydrin. Lin et al. (118B) did TLC of tuna extract, measuring the histamine-ninhydrin spots by densitometry. Cantoni et al. (27B)used ion exchange to remove interferences before histamine-phthalaldehyde reaction and spectrofluorimetry. Lerke et al. (111B) reported a rapid version of a fluorimetric histamine-in-tuna method. Staruszkiewicz et al. (212B)gave the background for their fluorescence histamine method for tuna and this first author (210B) reported the collaborative study results. A paper chromatographic procedure giving both histidine and histamine levels in fish was shown by Foo et al. (56B). Taylor et al. (223B) claimed simplied elimination of histidine interferences by extraction stages. T h e dansyl derivatives of amines and polyamines extracted from fish and shellfish were quantified by HPLC by Mietz e t al. (134B). These authors (133B) also correlated tuna quality with amines determined by HPLC. A GC method for indole in shrimp was modified by Staruszkiewicz et al. (211B),adding three internal standard compounds in case of chromatographic interference with any one. Lerke et al. (115B) considered ethanol useful as a tuna fish quality index. Cosgrove (32B)injected a canned salmon extract directly onto a Porapak GC column to measure ethanol for quality assessment.

CARBOHYDRATES The tenth edition of the “Cane Sugar Handbook” has been issued by Meade et al. ( 5 1 C ) ,and a book on “Examination and Analysis of Starch and Starch Products” has been edited by Radley (68C). Southgate ( 8 2 C ) has published on “Determination of Food Carbohydrates”, and Dean (27C)has described a method for the estimation of available carbohydrates in foods. Methods for the analysis of brewing sugars and syrups have been recommended by the American Society of Brewing Chemists, Inc. ( I C ) . Methods for the measurement of residual carbohydrate in beer ( I 5 C ) , and a review of the measurement of carbohydrates in wort and beer (16C) have been discussed by Buckee et al. Studies of the determination of sugars in foods and drinks (98C),and of different methods of sugar determination (97C)have been described by Zuercher et al. Vanadium pentoxide has been proposed by Haldorsen (35C) as a general chromogenic spray for carbohydrates. Color reactions for the determination of reducing sugars include the use of 1,5-dihydroxy-4,8-dinitroanthraquinone2,6-disulfonic acid for glucose, fructose, or galactose, described by Soloniewicz et al. (81C);the use of p-hydroxybenzoic acid hydrazide for the determination of reducing sugars in potatoes has been described by Grassert et al. (33C);and the use of 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole as a color reagent for invert sugar in sugar juices has been proposed by Reinefeld et al. (69C). A spectrophotometric method for glucose, mannose, and xylose has been proposed by Scott (78C) utilizing the dehydration of the sugars to furans in concentrated sulfuric acid. An automated fructose assay has been

described by Kennedy et al. (45C) and applied to fructoseglucose mixtures based on the formation of colored products from the reaction of fructose and hydrochloric acid. Another automatic method for fructose in soy has been proposed by Besle (9C) using the reaction with resorcinol in concentrated hydrochloric acid. A method of eliminating the interference of excess reagent, 3,5-dinitrosalicylic acid, has been described by Meur et al. (55C) which uses readings a t two p H values. Various analytical methods for the determination for invert sugar in sugar juices have been compared by Reinefeld et al. (7OC) including an iodimetric method, three colorimetric methods, and an enzymatic method; the last method gave the lowest results. A copper-ion selective electrode has been suggested by Papastathopoulos et al. (63C) to detect excess copper after the reaction of reducing sugars with Stanley-Benedict reagent. An electrochemical enzymic sensor has been built by Mor et al. (57C) using glucose oxidase as a means of measuring glucose. The use of the Boehringer Reflomat as a means for the rapid determination of D-glucose in foods has been evaluated by Birch et al. (12C). The details of the preparation of nylon-tube glucose oxidase derivatives have been described by Campbell et ai. ( 1 8 3 , these tubes can be used in Autohalyzers for glucose analysis. Another immobilized enzyme system for glucose described by Miller et al. (56C) uses immolized glucose oxidase on diazotised poly(aminostyrene), beads in a glass coil. Another glucose oxidase method proposed by Kirstein (47C) uses kinetic measurement of the p H change caused by the gluconic acid formed. Sugars are converted into their oximes for gas chromatographic determination in a procedure described by Jamieson (42C). Column chromatography of sugars in borate form on DEAE-Spheron has been described by Chytilova et al. (22C). Interferences due to phenolic compounds have been shown by Palu et al. (62C) to give false readings when refractive index detection is used after chromatography on anion-exchange resin. Avigad (4C)has suggested dansyl hydrazine as a fluorimetric reagent for the detection of reducing sugars after thin-layer chromatography. T h e use of high pressure liquid chromatography for the determination of sugars continues to develop. Theoretical aspects of detection systems have been discussed by Cox et al. (25C) who propose optical rotation detection. Monosaccharides in confectionery products have been analyzed by Timbie et al. (85C) using pre-column clarification. Other applications of HPLC include analysis of glucose syrup, fruit juices, and honey described by Schwarzenbach (75C), and the analysis of sugars in foods by Jones et al. (43C)who describe column preparation of an amino bonded phase. HPLC has also been applied by Hurst et al. (40C) to the analysis of sugars in milk chocolate, by Hunt et al. (39C) to the quantitative determination of sugars in foodstuffs, and by Cegla et al. (19C) to the analysis of soluble carbohydrates in de-fatted oilseed flours. A new polar bonded-phase material for carbohydrate separation has been suggested by Rabel et al. (67C). Basker (7C)has calculated correction factors for converting refractive index readings of sucrose solutions a t high temperatures to the standard temperature of 20 “C. A review of methods for the determination of lactose, glucose, and galactose in milk has been published by Bosset et al. (14C). A method for the rapid enzymic determination of lactose applicable to a variety of foods has been described by Cheng et al. (2OC). A similar enzyme method for lactose in cheese has been proposed by Frater et al. (32C)and applied to Cheddar cheese. Lactose hydrolyzed by an enzyme procedure and sucrose hydrolyzed by acid have been determined by Peeples et al. (64C)in ice cream. A thin-layer chromatographic method has been proposed by Siegenthaler et al. (80C) for the detection of mono- and disaccharides in milk drinks and yogurt. A chromatographic-polarimetric technique for quantitative determination of sugars has been described by Vidal-Valverde et al. (93C) which includes TLC and column chromatographic separations. Rhamnose has been determined by Hadzija et al. (34C) by a simple colorimetric method with which other sugars do not interfere. Isotope dilution determination of sucrose has been discussed by Piper covering isolation of the sucrose (65C) and procedures for control of errors (66C). Specific enzyme systems have been evaluated by Schoenrock et al. (74C) for the determination of sucrose in sugar beets and sugar beet products. Another


enzyme method has been described by White (95C) for the specific determination of sucrose in honey. Sucrose, and other sugars, in honey have been separated by Thean et al. (84C) using HPLC. A gas chromatographic method for sucrose described by Nurok et al. (60C) uses open tubular columns and trehalose as internal standard. Gas chromatography has been applied by West et al. (94C) to the quantitative determination of saccharides in enzyme-converted corn syrups, by Toba et al. (86C) to disaccharides using the trimethylsilylated oximes, and by Schwind et al. (76C) who describe procedures for di- and trisaccharides including formation of methoximes and acetylation, reduction with sodium borohydride and acetylation, and trifluorocetylation of the methoximes. Studies of the efficiency of procedures for the extraction of carbohydrates from soybean feeds have been performed by Besle et al. ( I O C ) using anion-exchange chromatography for detection. A modified amino-acid analyzer has been used by Kennedy et al. (44C) for the determination of neutral monosaccharides and oligosaccharides. Detection was accomplished with orcinolsulfuric acid. Oligosaccharides have been determined by HPLC by Have1 et al. (36C)with emphasis on stachyose determination. These sugars have also been determined by Covacevich et al. (24C) using thin-layer chromatography. Nurok et al. (61C) have described the separation of maltooligosaccharides by HPLC a t temperatures of 22 to 70 "C. Operational parameters for HPLC analysis of glucose oligomers in corn syrup have been studied by Sabbagh et al. (71C). A completely automated HPLC system has been described by Scobell e t al. (77C) for the analysis of carbohydrate mixtures. Maltosaccharides containing up to 25 saccharide units have been fractionated by Umeki et al. (88C) using multiple descending paper chromatography. The use of derivatization with 4-nitrobenzoates has been proposed by Nachtmann et al. (59C) as means to a sensitive HPLC determination of mono-, di-, and trisaccharides. Substituted carbohydrates have been separated by McGinnis et al. (50C) by HPLC on a microparticulate silica gel column. Gas chromatography of trifluoracetylated mono- to tetrasaccharides has been applied by Sullivan et al. (83C)to sugar syrups and processed foods. A one-step silylation procedure has been described by Leblanc et al. (49C) for the analysis of sugars and sugar phosphates. A colorimetric method for the separation and determination of glucosamine has been suggested by Yonekichi et al. (72C), and a n improved Elson & Morgan method for hexosamines has been reported by Van de Loo (89C). An automatic analyzer for amino sugars has been described by Dawson et al. (26C) which is a hybrid between a conventional amino acid analyzer and the usual liquid chromatographic procedure. Gas chromatography has been proposed by Varma et al. (90C) for the determination of neutral sugars, hexosamines and alditols; sugars are determined as aldonitrile acetates. Sugars and sugar alcohols have been determined by ion-exchange chromatography by Verhaar et al. (91C) using a Technicon AutoAnalyzer detection system, and by using UV detection a t 200 nm (92C). Gel chromatography on Sephadex G-200 or Sepharose 6B has been examined by Fleet et al. (31C)for the separation of various polysaccharides, particularly P-D-glUCanS. A method for the determination of 6-glucan in oats and barley has been described by Wood et al. (96C). Enzyme methods for starch include a semi-automated method for starch content in meat products reported by Arneth et al. (2C) using acid hydrolysis and glucose dehydrogenase, and a procedure for the measurement of total and gelatinized starch in foods reported by Chiang et al. (21C) using glucoamylase. Conway et al. (23C) have compared spectrodensitometric and colorimetric methods for quantifying starch hydrolysis products after separation by thin-layer chromatography. The use of the "amylose number" for the determination of starch damage has been studied by Seidemann (79C) who proposes modifications of the procedure. T h e effect of particle size and p H on the measurement of dietary fiber by the Van Soest method has been studied by Heller et al. (37C). A method for the determination of dietary fiber in plant foods described by Elchazly et al. (30C) uses enzyme treatment to remove starch and protein. The AOAC asbestos-free method for crude fiber has been submitted t o a collaborative study by Holst (38C), and accuracy and precision were satisfactory. Carrageenan in infant formulas

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has been determined by Kleckner et al. (48C) by reaction with phenolsulfuric reagent after precipitation with a quaternary ammonium salt. A turbidimetric method for colloid titrations has been described by Toei et al. (87C) and applied to carrageenan and sodium alginate. Methods for the analysis of pectin for degree of esterification and polyuronide content have been examined by Baeuerle et al. (5C). Schemes for the separation of pectin, polygalacturonic acid, and galacturonic acid in black-current juices have been discussed and applied by Bartholomae et al. (6C). A procedure for the fractionation of pectins by their degree of esterification has been described by van Deventer-Schriemer et al. (28C)using chromatography on DEAE-cellulose and determination of the uronide content of the fractions by the Dische reaction. The kinetics of the demethylation of pectin in isopropanol has been studied by Kim et al. (46C). Methods for the chemical analysis of hydrocolloids in foods have been described by Mergenthaler (52C) using thin-layer chropatography or gas chromatography after separation on DEAE-cellulose. Procedures for gas chromatographic analysis of gums have been developed by Mergenthaler et al. (53C) which convert the hydrolysis products into aldoximes and then into aldonitrile acetates. Further work by the same authors (54C) has been to apply gas chromatography to the identification of hydrolysis products of uronic acid containing polysaccharides. High polymer compounds in molasses have been separated and determined by Bugaenko et al. ( 17C) by p H adjustment and solvent treatment which separates pectic substances and colorants. Mannitol and sorbitol have been determined in sugarless chewing gum by Samarco (73C) by HPLC after extraction with a 2-phase water-toluene system. Sorbitol in cooked sausage has been determined by Moseley et al. (58C) by gas chromatography of the trimethylsilyl ether. Maltitol, sorbitol, maltose, and glucose have been detected in orange juice by Ida et al. (41C) by thin-layer chromatography. Drawert et al. (29C)have studied the gas chromatographic determination of hexoses, alditols, and polyhydric alcohols with special emphasis on the preparation of the trimethylsilyl derivatives. Another gas chromatographic method has been applied by Borys et al. (13C)to the determination of sugars and sorbitol in fruit juices, beverages, and preserves. Enzyme methods have been described by Beutler et al. ( I I C ) for D-sorbitol and xylitol in foods. Sorbitol in wines has been analyzed by gas chromatography of its acetyl derivative after column chromatographic cleanup of the sample by Bertrand et al. (8C). Methods for the determination of glycerine in wine that have been studied by Avellini et al. (3C) include gas chromatography, colorimetry for formaldehyde after periodate oxidation, a volumetric method, and a fluorimetric determination of the formaldehyde formed by use of the Hantsch reaction.

COLOR Methods for the identification of anthocyanins include pyrolysis gas chromatography described by Lanzarini ( 2 3 0 ) , and the use of gas-liquid chromatography and mass spectrometry suggested by Bombardelli et al. ( 7 0 ) . Anthocyanins and anthocyanidins in red wine have been determined by Drawert et al. ( 1 3 0 ) by gas chromatography as their trimethylsilyl derivatives. High pressure liquid chromatography has also been applied by Wilkinson et al. ( 4 6 0 ) to the analysis of anthocyanins. Chan et al. ( 1 0 0 ) have reported on the anthocyanin composition of taro corns using thin-layer chromatography after extraction and adsorption on poly(vinylpyrrolidinone). Two dimensional thin-layer chromatography has been used by Torre et al. ( 4 1 0 ) to determine the anthocyanin distribution in Rubus fruits. Beet pigments have been separated by Vincent et al. ( 4 3 0 ) using high pressure liquid chromatography, by Adams et al. ( I D ) on Sephadex G-25 and Bio-Gel P-6 columns. Computer examination of a mixture of beet pigments has been proposed by Saguy et al. ( 3 3 0 )as a means of determining all major beet pigments. Chlorophylls and other yellow plant pigments have been separated by Shiraki et al. ( 3 5 0 ) using thin-layer chromatography. Mixtures of copper pheophytins, chlorophylls, and pheophytins have been analyzed by White et al. ( 4 5 0 ) by means of calculations from fluorescence and spectrophotometric readings. Flavanones and 3-hydroxyflavanones in plant material have been analyzed by Schmidtlein et al. ( 3 4 0 ) by

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thin-layer chromatography after extraction and clarification. A colorimetric method for phenolic chromogens in sunflower products has been described by Bittoni et al. ( 5 0 ) . Column chromatography on polyamide has been used by Blenda ( 6 0 ) to determine leucoanthocyanins in plant material. Studies on the pigments of paprika include a rapid method using spectrophotometric measurement and calculation from the wavelength maxima described by Haspelova-Horvatovicova et al. (17 0 ) , another spectrophotometric plus calculation procedure has been proposed by Fekete et al. ( 1 4 0 ) , and a spectrophotometric method based on the reduction of the red pigments by sodium borohydride has been described by Baranyai et al. ( 2 0 ) . Recommended procedures for analysis of the oleoresins of paprika have been described by Bennesar Bibiloni et al. ( 4 0 ) and values for eight samples of Spanish origin tabulated. The reaction of tannins with proteins (bovine serum albumin) has been used by H a erman et al. ( 1 6 0 )to determine tannins quantitatively, and %y Hoff et al. ( 1 8 0 ) . T h e latter authors react the tannin with immobilized bovine serum albumin at pH 4. Price et al. ( 3 1 0 )have determined tannins in sorghum grain by the formation of the Prussian Blue complex. Thearubigens from whole tea brews have been separated by Cattell et al. ( 9 0 ) on Sephadex LH-20 columns with aqueous acetone. Xanthophylls in vegetable oils have been determined by Vogel (44D) by extraction, column clarification, and thin-layer chromatography. Pigments such as zinc pheophytins, chlorophylls, and pheophytins have been estimated by Jones et al. ( 2 1 0 )from spectrophotometric data using linear equations. A procedure for the detection and identification of natural water-soluble coloring matters in foods using the benzalkonium method has been described by Perdik e t al. ( 3 0 0 ) . Three-component mixtures of food colors have been analyzed by Honkawa ( 1 9 0 ) using two-wavelength spectrometry. Added coloring matter in meat products has been determined by McNeal ( 2 5 0 ) after water or ethanol extraction by spectrophotometry and paper chromatography. Tracer dyes in milk have been detected by MacIntosh et al. ( 2 4 0 ) by collecting the dye on Dowex AGl-X2 resin. A method for the detection of foreign coloring matter in hibiscus extract has been developed by Tanner et al. ( 3 8 0 ) using a thin-layer-paper-chromatographic procedure. Cochineal dye and lac dye have been separated and identified by Kenmochi ( 2 2 0 ) in the presence of amaranth by amino-ethylcellulose chromatography. Improvement in the error in extractable color measurements has been reported by Woodbury ( 4 7 0 ) when N.B.S. calibrated glass filter standards are used to correct for spectrophotometer error. A modified clarification procedure has been proposed by Meydav et al. ( 2 8 0 ) for the determination of browning in citrus products. Thin-layer chromatography has been used by Thielemann ( 4 0 0 )to detect 8’-apo’-@-carotenalin orange rind or orange juice. The analytical chemistry of synthetic dyes is the subject of a book by Venkataram ( 4 2 0 ) . Uncombined intermediates in Orange B ( 3 7 0 ) and in FD&C Red No. 40 ( 3 6 0 )have been determined by Singh, using high pressure liquid chromatography. Spectra of the subsidiary dyes of FD&C Red No. 40 have been published by Bell (30).Diphenylamine has been determined spectrophotometrically in D&C Yellow No. 1 by Dantzman ( 1 2 0 ) . Impurities in azo dyes used for food have been determined by Malkus ( 2 6 0 ) by thin-layer chromatography on silica gel. Column chromatography on 2-(diethy1amino)ethylcellulose has been described by Fratz (150) for the determination of 4,4’-diazoaminodi(benzenesu1fonic acid) in FD&C Yellow No. 5. Marmion ( 2 7 0 ) has used high pressure liquid chromatography to determine the same compound in FD&C Yellow No. 6. Thin-layer electrophoresis has been applied by Tewari et al. ( 3 9 0 )to the separation and identification of synthetic dyes in liquors. A spectrometric procedure has been described by Pallotti et al. ( 2 9 0 )for the simultaneous determination of synthetic water-soluble dyes in foods and beverages, and Yeh ( 4 8 0 )has separated coal-tar dyes by the use of polyacrylamide gel electrophoresis. Resonance Raman Spectra have been found by Brown et al. ( 8 0 ) to be useful for the identification of FD&C Reds No. 2, 4, and 10. A method for checking the purity of food dyes has been proposed by Cuzzoni et al. (110)which uses programmed multiple development thin-layer chromatography. A mathematical approach for the determination of the con-

centration of dyes in mixtures has been described by Saguy et al. ( 3 2 0 ) . The effect of irregularities in foods on their color evaluation has been discussed by Hunter et al. ( 2 0 0 ) .

ENZYMES Speed and accuracy, sometimes combined with automation, are the trend in analytical methods for enzymes in foods. Kleyn et al. have described methods for alkaline phosphatase activity in cheese (5E)using aqueous butanol extraction, and for alkaline phosphatase reactivation in milk products (6E) after treatment with magnesium chloride. An automated method for a-amylase in wheat flour proposed by Marchylo et al. ( 7 E ) uses @-limitdextrin anthranilate, which yields fluorescent products, as substrate. Zuercher et al. (16E)have recommended procedures for both a kinetic method and the Phadebas method for a-amylase in high energy foods. A gel-diffusion assay of a-amylase in bisected ungerminated wheat grains has been described by Gothard (1E). Rapid colorimetric detection of a-amylase using Phadebas tablets has been used by Mathewson et al. ( 8 E ) to detect sprouted wheat. The Phadebas tablets have been used by John et al. ( 4 E ) to determine a-amylase in malt; these authors use maltotitraitol as a substrate for @-amylase. Protein a-amylase inhibitors have been extracted from wheat flour by Pace et al. (IOE). A rapid method for the determination of the diastatic activity of cereal flours which uses the Ottawa starch viscometer has been described by Paton et. al. (11173). A simple, quick method for determining a-glucosidase in honey, developed by Siegenthaler (14E) uses p-nitrophenyl-a-D-glucopyranoside as substrate. A method for the determination of calf rennet in cheese has been proposed by Stadhouders et al. (15E),using the clotting time of reconstituted skim milk powder after addition of a freeze dried cheese extract. Hobson (2E) has detected 6-phosphofructokinase in plant extracts after separation on polyacrylamide gels. Polyphenol oxidase has been determined in fruits and vegetables by Mihalyi et al. ( 9 E )using chlorogenic acid as substrate, and by Jerumanis et al. ( 3 E ) in barley malt by measuring the oxygen consumed by an enzyme extract with an oxygen selective electrode. The effect of water activity on the enzymic changes in freeze dehydrated muscles has been studied by Potthast et al. who discuss the breakdown of muscle lipids (12E) and the changes in the activity of glycolytic enzymes during storage (13E).

FATS, OILS, AND FATTY ACIDS Perkins et al. review recent advances in the instrumental analysis of lipids (62F),and Deroanne (14F) describes the use of differential scanning calorimetry for the fractionation of palm oil and for the determination of the solid fat index (SFI). Comparisons are made of the fusion curves (SFI vs. temperature) of cocoa butter and several commercial vegetable oils by Desarzens et al. (15F) who found that identical results are obtained when the amount of solid phase present was determined by low-resolution NMR and pulsed NMR but report that dilatometry and differential calorimetry gave similar values for SFI, but higher values than those obtained by NMR methods. Madison and Hill (51F) describe a technique for determining the solid fat content of commercial fats by use of pulsed NMR which they report agreed well with dilatometry results, and Hester and Quine give methods for using pulsed NMR to analyze fat in milk powders and cottage cheese (41F). An IR method is described for the quality control of fat in dried milk ( I F ) wherein the ratio of the infrared reflectance values a t 1.74 and 1.65 pm are used to determine fat content from a developed calibration curve, and Miles and Fursey (54F) report on the use of an ultrasonic technique to measure the fat content of meat based on the relationship between the velocities of ultrasonic waves in muscle and fatty tissues, respectively, and the overall fat content of the tissues and suggest the use of this technique for estimating the overall mean percentage of fat in live animals. Hallermeyer (37F) has compared the analysis of fat in meat products by extraction with chloroform-methanol against the conventional Soxhlet and Stoldt-Weibull procedures and reports the former to be quicker and simpler and having the same efficiency and accuracy for the products tested, and a new method is described (36F) for determining fatty material in margarines by placing the molten sample on


a column of anhydrous N a 2 S 0 4and then eluting the lipids off the column with ether or methylene chloride (leaving water and nonlipid material on the column) and finally evaporating and weighing the residue. Welch (91F) describes a micromethod for estimating the oil content and composition in seed crops wherein the oil is trans-methylated, without prior extraction, by using H,SO,-methanol (1:49) at 80 "C; the resulting fatty acid methyl esters are extracted into petroleum ether and determined by gas chromatography on a packed DEGS column using flame ionization detection and heptadecanoic acid as an internal standard and the method is reported as applicable to a wide range of samples including field beans, cereals, and linseed and can be used with individual seeds or half-seeds. Kapoulas et al. (45F) describe the sequential TLC and GC methods used for the identification of the lipid components of honey after their extraction and separation on a silicic acid column, and Spencer et al. (74F) provide both HPLC and GC-MS analytical procedures for determining and comparing compositions of jojoba liquid wax esters. Folstar (24F) has applied TLC, GC, UV, IR, NMR, and MS techniques to determining the composition of wax and oil in green coffee after fractionation by column chromatography and provides a method for the quantitative extraction of coffee oil from the beans, and Fishwick and Wright (23F) have examined various methods for the extraction of lipids from plants by measuring the phospholipid, glycolipid, sterol lipid, and total acyl lipid content of the extracts and specify methods to used for spinach, tomato, potato, peas, and cereal seeds. Stahl et al. (75F) describe apparatus (TASOMAT) and a microanalytical technique (TAS) for the rapid analysis of lipid mixtures by use of carrier gas distillation to carry fractions of lipid mixtures onto a TLC plate over a temperature range (thermofractography) and discuss applications of this technique to the analysis of fats and oils, dairy products, mayonnaise, and chocolate. Clements reports on his quantitative studies (1OF) of the wheat flour lipids extracted with various solvent systems, wherein the flours were mixed with Celite 545 and the mixture was slurried with hexane to transfer to columns after which the lipids were eluted with the solvents being studied, thus, providing a convenient method for comparing solvent efficiencies for various types of flours. Adsorption column chromatography with gradient elution was employed by Cavina et al. (7F) on silica columns to effect separations of various lipid fractions (hydrocarbons, sterol esters, triglycerides, fatty acids, non-esterified sterols, 1,2- and 1,3-diglycerides,monoglycerides, and phospholipids) using a linear gradient of ethyl ether-light petroleum (1:l) in light petroleum, with flame ionization detection, and Duenges (20F) suggests the use of 4-bromomethyl-7-methoxycoumarinas a new fluorescence label for fatty acids stating that as little as 50 pmol of these derivatives could be detected by fluorescence under 360-nm radiation after separation on a TLC silica gel plate. Marszall (52F) suggests that the determination of the minimum emulsion inversion point of water-in-oil emulsions be used as a sensitive and rapid method for evaluating the effects of formulation variables on the hydrophile-lipophile balance of emulsion systems, and Trumbetas et al. make use of pulsed NMR to measure the solid fat content in oil-in-water type emulsions (85F),selecting from the data obtained an optimized type and amount of emulsifier for each system, and they also describe their work in applying pulsed NMR to a rapid and accurate method for determining the stability of emulsions (86F). Aston (4F) reports on a FORTRAN computer program for the processing of fatty acid data obtained by the analysis of fats and oils by gas chromatography (which is primarily designed for analysis of butter fat and margarine fat but can be adapted to other fats and oils) where fatty acids are calculated as wt 7'0, mol % , and the glycerol concentration and theoretical iodine values are also provided, and a subsequent correction is given by DeBrabander and Verbecke (13F) who point out that the original program did not allow for the water lost during the esterification of fatty acids with glycerol. Koman et al. (4727) have developed a FORTRAN computer program which permits the calculation of some 40 theoretical and industrially important chemical and physical values of fats and oils from data obtained by GLC determined fatty acid composition, acid value, and the titre test, and also (48F,49F)

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make use of input data from qualitative and quantitative GLC analysis of fatty acids after their stereospecific pancreatic lipolysis from the 1,3 positions of triglyceride molecules for the computer determination of all individual structures of triglycerides. Murata described the application of GC chemical ionization-MS to the analysis of peanut, rapeseed: and mustard oils and milk fat (56F) to determine the type and distribution of the triglycerides using NH, as reagent gas and also described application of this technique to the analysis of fatty acid methyl esters (57F) and GC-MS was used by Dommes et al. (18F) for determining the structure of polyunsaturated fatty acids by oxidizing them with 0,04in benzene-methanol (4:l) and then forming derivatives of the resulting polyhydroxy compounds prior to GC-MS analysis, reporting that only the trimethylsilyl ether derivatives (of those studied) yield fragmentation patterns from which chain lengths and the numbers and positions of double bonds can all be determined. Characterization of some 45 fatty acid methyl esters was done (32F) by subjecting them to GLC on four different liquid phases and tabulating retention indices and equivalent chain lengths so that these could be used for identification purposes. Iverson et al. (43F) report on butyl ester preparation for GLC determination of fatty acids in butter, finding conversions to butyl esters to be quantitative by the BF,, H2S04,and NaOBu procedures and recommending the use of butyl esters as a way to avoid losses of the volatile short-chain acids and the water soluble acids when one uses methyl esters, and Geiko et al. (29F) make use of pancreatic lipase to hydrolyze triglycerides separated from rice lipids by TLC and then determine the fatty acids liberated by gas chromatography (noting that only 0.86% of the total glycerides were completely saturated and that the bulk of the unsaturated glycerides contained an unsaturated fatty acid in position 2). A method is given (77F) for the automated measurement of free fatty acids of milk by continuous flow analysis where the FFA are extracted with isopropanol-heptaneN H2S04(lOO:lOO:8) and are determined with phenol red indicator, and Stetina and Luck (76F) determine the FFA of milk by extraction with CsHs and measure them spectrophotometrically at 533 nm with rhodamine, noting that lactic acid does not interefere but also that this method is not suitable for use on sour milk (below pH 6.3) because of the production of organic acids by bacteria which the method would determine as FFA. Takagi and Itabashi have developed a GC method (80F)for the GC separation of triglycerides based on their degree of unsaturation on Silar 1OC columns after separating them by argentation TLC on silicic acid, reporting relative retention times and equivalent chain lengths of C36to C, to triglycerides with up to 9 double bonds, and have also similarly analyzed polyunsaturated wax esters (CZ8to C4J containing up to 'idouble bonds (79F) prepared from the fatty acids of linseed and anchovy oils on a glass column of Silar 1OC on Gas-Chrom Q (100 to 120 mesh) a t 200-250 "C. Shoolery (72F) reports on a study of two methods used to overcome problems in I3C NMR intensity measurements and provides examples of I3C NMR applications to the analysis of animal and vegetable oils and the determination of cis and trans isomers in partially hydrogenated edible oils, and Rutar et al. (68F)make use of Fourier Transform I3C NMR to determine the relative quantity of unsaturated fatty acids as well as the content of linoleic acid in individual sunflower seeds, peanuts, soybeans, and bulk samples of rapeseed to assess their quality and suggest that one should use a superconducting magnet ,L('3C) 167.9 MHz for seeds with a low oil content. Pfeffer and co-workers (63F) describe the use of Fourier Transform 13C NMR for determining the cis/trans composition in partially hydrogenated and isomerized unsaturated lipids, and also describe (64F)application of this technique to determine butyrate in a complex mixture of butter oil triglycerides. Karleskind et al. (46nhave analyzed unsaturated triglycerides by treating them with Wijs solution in chloroform and aqueous KI to form chloro-iodo derivatives which are then separated by HPLC and detected by their strong absorption a t 265 nm, Perkins et al. (61F) and Otterstein et al. (600provide GC methods for the determination of trans-unsaturation by analysis of prepared methyl esters of fats and provide examples on the application of these to margarine oils, and Gray (33F) has made use of a GLC technique to determine the free fatty acids in dairy products.

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The combined use of HPLC followed by GLC was applied to the determination of the triglycerides of soybean oil (90F) using a column packed with p-Bondapak CIS with MeOHCHC13 (9:l) to separate the triglycerides into six peaks, and McCreary et al. (5329 have applied a novel and rapid method to the preparation of methyl esters of fats and oils for GC, using 0.2 N-methanolic (m-trifluoromethylphenyl) trimethylammonium hydroxide. Tur’yan et al. (88F) describe a novel titrimetric method for the determination of the iodine number of fats, and Koops and Klomp (5017) make use of a copper soap method for determining the free fatty acids in milk by a rapid colorimetric determination after reaction with sodium diethyldithiocarbamate. A rapid microprocedure for fatty acids by GLC is presented (30F)wherein total and free fatty acids are extracted into hexane from a range of biological materials and food homogenates after hydrolysis and are then quantitated with an internal standard method as their methyl esters by an “on-column” methylation procedure, Barrette (6F) and Heisz (39F) provide methods for the GLC determination of erucic acid with the former directed toward the certification of low erucic acid varieties of rapeseeds and the latter method using automated gas chromatography after formation of the methyl esters of vegetable oils. An equation is given by Hela1 and Ahmed (40F) for the direct calculation of the iodine value of buffalo-milk fat from its refractive index, Murthy et al. (58F) make use of refractive index measurements before and after iodination with Wijs reagent (using mercuric acetate as catalyst) to calculate the iodine number of milk fat and vegetable fats (finding the avera e ratio of the RI change to iodine number to be 50.7 X 10- ), and Asakawa and Matsushita (3F) provide a colorimetric determination of peroxide value by complexing the iodine liberated from a KI-silica gel reagent with starch and measuring the blue color a t 560 mp. Nielsen (59F) describes a n NMR procedure for determining the iodine value of butter fat, and use is also made of infrared absorption spectra for measuring the unsaturation of milk fat and vegetable oils (2F), finding a nonlinear but significant correlation between the absorption a t 3.3 wm (olefinic C-H stretching band) and the degree of unsaturation as measured by iodine number. Johnston et al. (44F)give techniques for analyzing mixtures of dienoic fatty acids, such as occur in hydrogenated fat products, employing ozonization, reduction to alcohol fragments with sodium borohydride, GC analysis, and then use of a computer procedure to give the analysis of the diene isomers, and Frankel et al. (25F) describe GC-MS methods used to determine the autoxidation products of methyl oleate after forming their T M S derivatives and extend the procedure to the analysis of the autoxidation products of methyl linolenate prepared from linseed oil (26F). A simple and rapid method for the assessing of oil rancidity based on the complex formed by hydroperoxides with T i is given (2IF) which is reported to correlate well with peroxide number and thiobarbituric acid values as well as with odor intensity values, Chan and Levett (8F) describe the HPLC analysis of a mixture of methyl hydroperoxide isomers formed by the autoxidation of methyl linolenate, and Barnard and Wong (5F) have developed a procedure for determining small amounts of organic hydroperoxides (in their studies on the autoxidation of palm oil components) by reducing the sample with an excess of triphenylphosphine and then analyzing by GLC using hexacosane as an internal standard. Methods for the evaluation of heat-treated frying oils are given for soybean oil used for frying various foods (89F) where the polar (P) and nonpolar (NP) fractions of either the oil or its free fatty acid methyl esters are separated on TLC plates and the ratio of P / N P fractions are compared by use of a UV chromatoscanner, and further procedures are given (I 7F) by which components in subfractions of polar triglycerides from heat-treated soybean oil were fractionated by sequential column chromatography and were then identified by GC-MS. Gertz ( 3 1 0 reports on a procedure for evaluating frying oils by separating the polar fraction on a silica gel column and weighing it (with a 23-2470 polar fraction described as being the upper limit for reuse of the fat), and Sano et al. (69F) measure the oxidation degree of edible fats and oils by direct gas chromatography, finding that the level of 2,4-dienal isomers correlates well with the oxidation degree of fats and oils containing linoleate. Guhr and Waibel (35F) describe procedures for the analysis of deep-frying fats by determination of oxidized fatty acids

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insoluble in light petroleum, by column-chromatographic determination of the polar and non polar fractions, by liquid chromatographic determination of substances more polar than the unchanged triglycerides, and by gel permeation chromatography of the polymeric triglycerides, and Smoczkiewiczowa et al. (73F) report on IR spectroscopy techniques for monitoring changes in heated vegetable oils, noting little change up to 200 “C but finding sharp changes above that temperature. A comparison was made (87F) of eight photometric tests for analysis of the oxidative deterioration of fats with respect to their sensitivity as used on autoxidized methyl linoleate and methyl linolenate (the ferrous isothiocyanate test was found to be the most sensitive test followed by the measurement of diene absorption), and Porter et al. (65F) report that the color in the 2-thiobarbituric acid test for peroxidation of lipids (at 532 nm) can be produced by various monocyclic peroxides and that the color can be greatly enhanced by the addition of ferric salts. Fritsch and Gale (28F)make use of the GC determination of hexanal as a measure of the degree of rancidity of low fat foods (e.g., cereals, dehydrated potatoe, defatted wheat germ and soya products, etc.), Totani et al. ( 8 4 0 provide a colorimetric test for the quantitative analysis of cyclopentadiene compounds in the presence of cyclohexa-1,3-diene and other products of the thermal treatment of unsaturated fatty acids and triglycerides, reporting that cyclopentadiene compounds were formed from ethyl linolenate but not from ethyl linoleate, and Scrimgeour (70F) describes a method for determining the furanoid fatty (F1-Fs) acids in cod liver oil using squalane as an internal standard (added prior to isolation of the furanoid esters by argentation TLC). The determination of neutral lipids by TLC with flame ionization detection was accomplished (82F) by dissolving samples in CHC13, applying them to coated silica rods and, after development, chromatograms are recorded by placing the rods in a scanning apparatus containing the detector (Thinchrograph TFG-10). Huyghebaert and Hendrickx report on the analysis of sterol esters in a number of animal and vegetable fats (42F) performed by extracting the free sterols on a digitonin-containing Celite column, saponifying and determining the sterols in the unsaponifiable fraction by gas chromatography, and Tamura et al. @ I F ) describe both a TLC method and a digitonin precipitation coupled with GLC method for the determination of sterols in fats and oils, giving also the results of a collaborative study of these methods. Fedeli et al. (22F) have determined the methoxy derivatives of sterols from the unsaponifiable fraction of olive oil and sunflower seed oil by GLC after preparing the derivatives by treatment with dimethyl phosphite in the presence of toluene-4-sulfonic acid, and an HPLC method is described ( 1 I F ) for the analysis of unsaponifiable matter of vegetable oils which is reported as being more reliable and rapid than combined TLC-GLC procedures. A simple and efficient method for the GC determination of sterols in oils and fats is given (92F) where the unsaponifiable fraction is silylated with heptafluoro-N-methyl-N-trimethyl-silylbutyramide in pyridine solution and determined on a 5% OV-17 on GasChrom column using cholestane as internal standard, and Tiscornia et ai. (83F) report on column and GC-MS methods used to determine the sterol fraction of tomato seed oil and find that the sterol fraction contains relatively large amounts of cholesterol (7 to 27%). Sweeney and Weihrauch (78F) review methods for the separation and determination of cholesterol in foods and provide data for the cholesterol contents of various meats and dairy products, enzymatic spectrophotometric methods are given for determining free and esterified cholesterol in serum and tissues (55F) and for estimating cholesterol in milk fat when large numbers of determinations are to be performed (34F), and a GLC procedure is given for the determination of cholesterol and other sterols in foods (7123 after formation of their butyryl esters. Rainey and Purdy (66F) describe their work in optimizing separations of phospholipids by HPLC, using a 180-cm column packed with Corasil I1 and an eluting solvent mixture of chloroform-methanol-ammonia (50:35.9:7, v/v/v), and a column-chromatographic separation is also described for the separation of fractions of phospholipids from egg-yolk followed by their analysis on Kieselgel G TLC plates (67F) using Dragendorff reagent and ninhydrin for detection. Di Mucclo and Delise (16F) provide chromatographic methods for the


fractionation and determination of phospholipids in milk, with the final analysis done by 2-dimensional TLC on Adsorbosil 5 , and a one-dimensional TLC method is presented for the rapid analysis of a mixture of phospholipids and neutral lipids, using three solvents for development by Frederiks and Broekhoven (27F). Duden and Fricker (19F) have determined t h mono- and digalactosyl diglycerides and lecithin in spinach by TLC, and a TLC method is also given for the densitometric analysis of ethanolamine and serine containing phosphoglycerides (38E),which is applied to raw soya-bean lecithin. Cho et al. (9E) make use of two-dimensional TLC to separate the lysophosphatides of butter serum prior to further analysis by GLC to determine the positional isomers, and Daun ( I Z F ) describes a rapid procedure for the determination of chlorophyll in rapeseed by reflectance spectroscopy after grinding the seed in a specially designed grinder.

FLAVORS A N D VOLATILE COMPOUNDS Parliment and Scarpellino (71G) describe the use and importance of modified sensory flavor profile techniques for the evaluating of gas chromatographic flavor fractions isolated during the analysis of food flavors, and Aishima and Nobuhara ( I C , 2G) make use of multiple-regression analysis of gas chromatographic profiles to effect quality evaluations of soy sauce, obtaining correlations of better than 0.9 with sensory data. A convenient method is given for the multiple extraction of volatile flavor components from food slurries and pulps using a two-chambered glass bomb extractor and dichlorodifluoromethane (Freon 12) solvent ( 8 G ) ,and Chang et al. (21G) describe various techniques and apparatus for the isolation of trace volatiles from various foods and discuss sample selection and formation of artifacts during the isolation procedure. Methods are given for the gas chromatographic assessment of the flavor quality of vegetable oils by Jackson et al. ( 4 4 G ) and Dupuy et al. (31G)which are applied to monitoring aging effects on soya oil under controlled conditions, using GC-MS analyses to define major volatiles and finding good correlations with sensory tests. Waltking and Zmachinski (92G)describe a GC quality control procedure for evaluating vegetable oils which they apply to corn oil aged under various conditions, using octadecane as a n internal standard. Kaufmann et al. (50G) provide a TLC method for the quantitative determination of the boar taint substance, androstenone, in fat reporting that as little as 0.02 pg can be detected, Hirayama and Imai (42G) make use of a pyrolyzer-GC method for determining residual hexane in oils (weighing the oil sample into a small platinum dish which is placed in the pyrolyzer), and Bigalli ( 7 G ) makes use of a Dean and Stark type still and hexane as a carrier solvent to isolate pentane formed during autoxidation of oils contained in solid food samples (e.g., nuts and chocolate) for GC analysis. Chang and Peterson (20G) review recent developments in the analysis of cooked meat flavor including isolation, fractionation by gas chromatography, and identification by IR and mass spectrometry and also provide a discussion of the importance of heterocyclic and pyrazine compounds in the flavor of meat, with suggestions of possible mechanisms of formation. Min et al. (62G)report on the analysis of the volatile components of roast beef which were isolated by a specially designed gas entrainment apparatus, separated into acidic, basic, and neutral fractions, and the last fraction was then further separated by repeated GLC on two stationary phases into subfractions which were analyzed.by:GC-MS, and MacLeod and Coppock (59G) analyze and 66"fnpare the chemical compositions of boiled and roasted beef aromas by GC-MS by using a modified Likens a n d Nickerson extraction procedure followed by low temperature-high vacuum distillation. GC-MS techniques are described by Caporaso et al. ( I 7G) which were used in a study designed to isolate and identify compounds from ovine adipose tissue (lamb fat flavor) which contribute to the characteristic flavor of the meat. Stark et al. (83G) have determined the free fatty acids and free &lactones in butter oil by cold-finger molecular distillation a t 35 "C followed by silicic-acid column chromatography of the distillate and then gas chromatography of the fatty acid and lactone fraction, and they also apply similar techniques (84G)to the GC determination of phenolic compounds as their trimethylsilyl derivatives and also indole and skatole and report that the latter two compounds are important contributors to butter flavor. A GLC headspace

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method is given (86G)for the determination of H2S in heated milks using a flame photometric detector and a Teflon column containing 40-60 mesh Haloport-F treated with 12% polvphenyl ether and 0.5% H3P04,and Cant and Walker (16C;) have developed a method for regenerating monocarbonyls from their 2,4-dinitrophenylhydrazonederivatives by passing a pentane solution of the hydrazones through a column of Celite impregnated with sulfuric acid (thus avoiding the use of heat and long contact with sulfuric acid) and then concentrate the compounds by column chromatography on activated silica gel, elute them with ethyl ether, and determine them by GLC, with an example given of an application to the regeneration and determination of carbonyls from whole milk powder. Thomasow et al. (87G) provide colorimetric methods for the determination of hexamine (used as a preservative) and volatile aldehydes in cheese and other milk productq, Piergiovanni and Volonterio (72G) have determined the carbonyl compounds from cheese by reversed- phase liquid chromatography of their 2,4-DNP derivatives with spectrophotometric detection at 360 nm, and Dumont et al. report on GC-MS methods (30G) used to determine a number of minor aroma compounds from Camembert cheese which were obtained by the Freon 11 extraction of an aqueous solution of volatiles isolated by low temperature vacuum distillation. A n d r e w et al. ( 4 G )describe a technique for the recovery of formaldehyde from turkey meat by a nitrogen sweep using acidic aqueous 3-methyl-2-benzothiazolinone hydrazone reagent as a trapping solution and finding correlation of formaldehyde levels with storage time, Sin et al. (79G)report on the separation and determination of dicarbonyl compounds by gas chromatography after transformation into quinoxaline derivatives on a Celite 545 (8Ck100mesh) column coated with 57, Silicone SE-30, and a differential pulse polarographic procedure is given (67G) for the determination of crotonaldehyde in ethanol. A gas chromatographic technique is described (25G) for assessing the ethanol levels in canned salmon by direct injection of filtered aqueous juices, and an apparatus and technique are provided by Lerke and Huck (57G) for collection and analysis of ethanol in canned tuna by GC analysis as an objective quality determination (ethanol levels increase with deterioration of samples). A volumetric determination is provided for the determination of mercapto groups (82G)by titration with 2-(diacetoxyiodo) benzoate, and Warner (93G)has applied GC analysis to the determination of aliphatic and aromatic hydrocarbons in marine organisms (e.g., clams and oysters). A potentiometric method based on use of a SO2 sensing probe (32G) is recommended as a new approach to determining sulfur dioxide in beer. a simplified technique is described for the determination of volatile acidity in wines (77G) after oxidation of sulfurous acid before steam distillation and titration, and HPLC is applied (22G) to the determination of nucleotides from beer flavor. Grigsby and Palamand (39G) make use of the complex formed between dimethyl sulfide and sodium nitroprusside in alkaline solution to measure dimethyl sulfide in water, wort, and beer, Anders et al. ( 3 G ) make use of proton NMR to determine ethanol in wine, wine-like beverages and spirits. and the diacetyl content of beer is analyzed (5G) by sweeping with nitrogen, condensing with a dry ice-acetone trap and determining the diacetyl by gas chromatography. A GC method is given ( 6 G ) for the analysis of 2-butanol, 1-butanol, 1-pentanol, and 1-hexanol in distilled alcoholic beverages (a survey of 198 brands indicated 1-hexanol to be the best parameter for characterizing the beverages), glycerol is determined in wines by use of TLC followed by spectrophotometric measurement ( I s G ) ,and Dima and Ghimicescu (27G) report on the colorimetric determination of volatile acids by the yellow color formed by NH,V,03 addition after they are steam distilled from wine treated with HZ02 and NaAsO,. Drawert et al. (29G) have analyzed the organic acids of Tokay wines by use of GC-MS, Jameson et al. ( 4 5 G ) make use of a direct injection GC technique. permitting the easy use of internal standards, to obtain reproducible results in the determination of carbon>-1sand other volatiles in beer by use of their 2,4-DNP products, and Kojima (54G) describes a simple headspace GC technique for determining ethanol in spirits. Otvos and Szep (69G)provide a GC method for the determination of fusel oils, Nelson et al. (64G) describe their work in the extraction (Freon 113), separation, and determination of volatiles from Catawba wines

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by GC and GC-MS methods, and Tress1 and co-workers report on their work in the analysis of volatile phenolic compounds of beer, smoked beer, and sherry by column chromatography and GC-MS (90G).Strukova et al. (85G) describe the POlarographic determination of carbonyl compounds in an alcohol distillate based on its reaction with hydrazine, Williams e t al. (94G) provide apparatus and a procedure for reproducible high resolution GC analysis of alcoholic beverage headspace volatiles, and methods are given for the determination of methyl anthranilate in wine by GC after extraction with Freon 113 (65G) and by HPLC with fluorescence detection (76G). A rapid liquid chromatography procedure is given for the determination of quinine in soft drink beverages (36G) by use of a silica column and 0.5% “,OH in MeOH as a mobile phase, and Sontag and Kainz (81G) describe a procedure for the determination of quinine in tonic waters by differential pulse polarography. Todd et al. (8%) report on a method for the GC analysis of capsaicinoid compounds which are extracted and determined as their silyl derivatives using N-vanillyloctanamide as an internal standard, a spectrophotometric determination of capsaicin (74G) is given where ethyl acetate extracts of paprikas are treated with VOCl, and the absorbance is read a t 720 nm (with a sensitivity of 0.05%), and Pankar et al. (70G) describe a new method for determining capsaicin extracted from chillies by using a multiband TLC procedure (silica gel G, Kieselguhr G with 8% active carbon, and silica gel G bands, respectively). Grushka and Kapral (40G)report a GLC analysis of capsaicinoids which provides a good separation of capsaicin and its dihydro and nordihydro derivatives and makes it possible to characterize the oleoresins from various sources without requiring derivatization, and a TLC method is given (56G) for determining the capsaicin in raw green paprika which can also be adapted to a spot test screening method and makes use of Gibbs reagent or FeC13-K3Fe(CN)6for detection. Orsi (68G) describes a technique for determining the content of active ingredients in garlic which depends on the measure of pyruvic acid which accompanies the liberation of alliicin from garlic, and a method is given by Devani et al. (26G) for the colorimetric determination of allyl isothiocyanate in mustard seed using 2,3dichloro-1,4-napthaquinoneas reagent. A procedure is given (37G)for the determination of piperine extracted from black pepper by dichloroethane using HPLC on Porasil A with CHC1, as solvent and UV detection, Glasl et al. (38G)make use of GLC on a glass column packed with 10% of UCCW 982 on Chromosorb W to determine trans,trans-piperine in black pepper and white pepper, and methods are given by Clark et al. (23G) for the GC-MS analysis of paradols (as in some varieties of ginger). Rode1 et al. (75G) report on the testing of various methods for the isolation and concentration of volatile substances present in roasted coffee for the purpose of gas chromatographic analysis with special regard to their reproducibility and time requirements, and Quijano-Rico et al. (73G)report on apparatus and methods used to study the pyrolysis (roasting) of coffee beans by combining DTA on-line with mass spectroscopy in special combined apparatus. Kawabata et al. (49G) describe the determination of dimethyl sulfide in the volatile aroma of green tea by headspace GC, Hoeffler and Coggon (43G) present methods for determining theaflavins and flavanols in tea by reversed-phase HPLC, GC-MS techniques are employed (41‘2) in making comparisons of aroma components of green and black tea, and Cattell and Nursten (19G) make use of Sephadex LH-20 chromatography to fractionate and analyze the ethyl acetate soluble thearubigins from black tea. Phenolic compounds and aromatic hydrocarbons were analyzed in the thermal reaction products of food model systems and of barley (91G) by gas chromatography with MS and IR identification, Bories et al. ( 9 G ) provide a versatile method for determination of normal alkanes in foods (using a “clean-up” column packed with layers of silica gel, Florisil. and alumina from which the hydrocarbons are eluted prior to final GC analysis), and Obretenov and Hadjieva (66G)make use of GC-MS techniques to identify 29 bread aroma compounds. Corradi and Micheli (24G) provide rapid methods for the TLC determination of vanillin, ethylvanillin, and their corresponding acids in flavored food products on silica gel, Meili

and Chaveron (61G) describe techniques for isolation and concentration of flavor compounds from vanilla extracts and of products flavored with these extracts and their analysis by TLC and GC methods, and Kan et al. (47G) describes the GC determination of vanillin and coumarin in foods (applications are given to chocolate, biscuits, ice cream, cocoa, and caramel). A procedure is also presented (48G) for the HPLC analysis of vanillin and coumarin in foods by use of a Permaphase E T H column and hexaneeethanol(49:l) as mobile phase, and Braun and Hieke (10G)apply GC-MS methods to the determination of the trimethyl silyl ethers of vanillin and ethylvanillin in foods. Klines and Lamparsky ( 5 l G ) have used GC-MS to determine about 170 components of Bourbon vanilla beans by use of headspace and high vacuum transfer techniques as well as using solvent extraction for concentration of volatiles. A preparative GLC method is given for the separation of the cis and trans isomers of “strawberry aldehyde”, a synthetic aroma substance (ethyl 3-methyl-3-phenyl glycidate) followed by their identification by NMR and IR (63G),a GLC method is given by Braun and Hieke for the determination of 4(4-hydroxypheny1)butan-%one (raspberry ketone) in raspberries and raspberry products ( I I G ) ,and Frattini et al. (35G) describe the GLC, GC-MS, and IR methods which they used to determine some 63 compounds not previously identified from heated licorice essential oil. Methods are given for the application of derivative UV spectrophotometry (15G)to the analysis of lemon essence, and Cababro and Curro (14G) describe a technique for the spectrofluorimetric determination of coumarin in lemon essence after separation by TLC on silica gel. Fisher (33G) reports on an improved method for measuring limonin in citrus juice by HPLC on PBondapak CN (with methanolwater as mobile phase), and a volumetric method is presented (78G) for the determination of total aldehydes in citrus oils based on the quantitative reaction of citral with semicarbazide hydrochloride. Korany et al. (55G) have developed a colorimetric procedure for measuring thymol and eugenol in volatile oils which is based on their reaction with Na3Co(No2j6 in aqueous acetic acid, and a GLC procedure is given for determining neral and geranial in essential oils (46G) using phenethyl alcohol as internal standard and by running chromatograms before and after conversion of the aldehydes into the alcohols and calculating the nerd and geranial content by difference. Lund and Bryan (58G) compare methods of analysis for commercial orange essences and compare results with organoleptic evaluations, concluding that GC analysis using directly injected essence is promising as a rapid and objective technique for quality control. McKeag et al. (60G) have applied GC methods to determining the varietal differences in the aroma essence of maize kernals and quantitate these differences for five varieties, Bullard and Holgiun (12G) have analyzed and identified some 7 3 components of unprocessed rice by GC-MS, and Flath and Forrey (34G)have determined 106 compounds in the volatile aroma of papaya by GC-MS techniques. Koehler and Hoehn (53G) report on their studies in analyzing n- alkanes and acetylated fatty alcohols (including those from coconut) by the direct coupling of a glass capillary gas chromatograph to a mass spectrometer. Methods are given for isolating the volatile aromas of tomato, apple, and strawberry on Tenax and then performing a GC-MS analysis as a means of evaluating aroma qualities (%GI,and Yamashita et al. (95G)make use of headspace GC to analyze the volatile alcohol and esters formed during the ripening of strawberries. Knee and Hatfield (52G) compare methods for measuring the volatile components of apple fruits by gas chromatography and observe that the concentrations of volatiles in the air passing over apples were influenced by tissue permeability, concentrations in peel or cortex, and effects of enzymic hydrolysis, thus making it difficult to assess the importance of compounds in apple flavor and suggest by their work that measurements of aroma concentrations for apples be made above cortical disks. Smagula and Bramlage (BOG) provide a method for determining acetaldehyde in apple tissue by TLC of its 2,4-DNP derivative, more than 100 constituents of flavor components of cooked asparagus have been isolated and identified by adsorption chromatography and GC-MS techniques (89G), and Buttery e t al. (13G) have analyzed the volatile aroma fraction of cooked artichoke using a Likens-Nickerson steam-distillation, continuous extraction head and combi-

A N A L Y T I C A L CHEMISTRY, VOL. 51, NO.

nations of liquid chromatography and GC-MS analysis to characterize a total of 32 components.

IDENTITY This section covers articles on the analysis of authentic samples of foods and the determination of foods in foods. Total nitrogen and phosphate values have been shown by Schur et al. (70H) to indicate the presence of raw maize or rice in the brewing of beer. The ratio of isobutyl and isopentyl alcohols in whiskies has been found by Hall (24H) to provide a means of identification of types of whiskies. Types and origins of whiskies have been distinguished by Reinhard (68H) by means of isoamyl alcohol-isobutyl alcohol ratio. Analysis data on the major congeners of Australian and other brandies has been compiled by Hogben e t al. (27H). T h e proteins of Brazilian Comun cacao have been analyzed by Timbie et al. (75H) and their amino acid pattern may be used in classifying various cacaos according to genetic origins. The use of theobromine measurement to determine cocoa solids in chocolate has been found imprecise by Pusey ( 6 5 H ) except for quality control purposes. A series of papers on the constituents of coffee has been published in the “Seventh International Colloquium on the Chemistry of Coffee” (7111) covering volatile constituents, potassium content, mineral analyses, carbohydrates, and fatty acids. Constituents that decrease with the extraction yield of coffee have been found by Maier et al. (42H) to be potassium, sulfated ash, and normal ash. A test for chicory in coffee has been described by Promayon e t al. (64H) which uses fructose as an indicator of chicory content. An enzymic method for cholesterol has been described by Beutler et al. ( 4 H ) as a means of determining the egg content of foods. The selective cleavage of fatty acids in the terminal positions of triglycerides by means of enzymic hydrolysis has been proposed by Movia et al. (49H) for identifying butter adulteration or butter substitutes. Enzymic hydrolysis has also been suggested by Mani et al. (44H) as a means of detecting esterified olive oil. T h e determination of critical solution temperature has been proposed by Maiti (43H) as a means of identification of vegetable oils. A study of the tocopherols in coffee oil by Folstar et al. ( 2 I H ) showed the presence of c y , p, and/or y-tocopherol. A chromatographic method for detecting butter adulteration with tallow or vegetable fat has been described by Carisano et al. (8H)using thin-layer chromatography and pancreatic lipase hydrolysis. Components in cocoa-shell fat have been identified by Bracco et al. (7H) and may be used to detect the presence of this fat in cocoa butter. T h e serotonin, dopamine, and noradrenaline contents of bananas, dates, and figs have been determined by Stachelberger et al. (74H) who found only serotonin in dates and figs and all three amines in bananas. Standard values for a range of constituents have been listed by Faethe et al. (I7H) for juices and nectars of black currents and sour cherries. The contents of some amino acids in orange juices have been used by Niedemann (53H) as criteria of purity. The betaine and albuminoid ammonia nitrogen have been suggested by Khanwalker et al. (32H) as measures of the juice content of orange beverages. An additional criterion for the evaluation of orange juices, a-amino nitrogen, has been suggested by Hils (25H). Carotenoid measurement has been proposed by Benk et al. (3H)as a means of detecting Tagetes extract in orange juice. Proline in various fruit juices has been determined by Wallrauch (8011) by a colorimetric procedure, and the method has possibilities for detecting adulteration. T h e validity of electrophoresis for the identification of soft-wheat flour in pasta has been shown by D’Arrigo to be vitiated when the flour has been treated with formaldehyde (IOH), or with other chemical agents ( I I H ) . Soft wheat in pasta has been detected by Kobrehel et al. (36H) by determining the peroxidase content. The usefulness of electrophoresis for detecting soft wheat in durum wheat products has been discussed by Menger (47H). Disc electrophoresis patterns for water-soluble wheat proteins have been shown by Nitsche e t al. (5511) to provide a means of identification of some varieties. Species differences in some wheat varieties have been found by Nierle (54H) in the gliadin fraction. Bourdet et al. (6H)have reported similar results. Differences in protein extractability have been shown by C h u g et al. (9H) to differentiate poor and good flours. Wheat and rye mixtures

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have been differentiated by McCausland (41H) based on the distinctive patterns of their prolamine proteins. Procedures for the analysis of chewing gums and ranges observed have been presented by Delaveau et al. ( 1 3 M ,and the same authors ( 1 4 H ) have presented an analytical protocol for the analysis of water-soluble products, flavors, and mineral elements in chewing gums. Amino acid analysis has been suggested by Davies (12H) as a means of identification of the geographical origin of honey. A review of the data on the average composition of the disaccharides of honey has been presented by Doner (15H). A method for the determination of S-methyl-cysteine sulfoxide in kale has been shown by Matheson et al. (46H) to reveal varietal differences within a species. Ethanol has been identified by Lerke et al. ( 3 9 m as a potentially useful indicator of quality of canned tuna. A standard nitrogen factor of 3.7 has been proposed by Wood ( 7 9 H )for cooked shrimp meat. Differences between breast muscle proteins of fresh and aged broilers of different ages have been noted by Kitamura et al. (34H) using gel electrophoresis. Chicken meat in meat products has been detected by Tinbergen et al. (77H) by measurement of the anserine to carnosine ratio. Isoelectric focusing in polyacrylamide gels has been used by Tinbergen et al. (76H) to identify meat and fish species including flatfish, beef, pork, horsemeat, and chicken. Meats of different species such as buffalo, sheep, dog, and rat have been found by Ramdass et al. (66H) to give species-specific protein band patterns when analyzed by polyacrylamide gel electrophoresis. Immunological analysis has been applied by Gabucci et al. (22H) to the determination of raw and cooked beef, pork, and horsemeat. Kat0 et al. (31H) have also applied polyacrylamide gel electrophoresis to meat species identification. Their studies include meats of cattle, pig, horse, whale, chicken, and turkey. Methylamino acids, determined by chromatography by Poulter et al. (62H) and by Skurray et al. (7211) using HPLC, have been proposed as a means of determining meat in food products. Added blood in meat products has been assayed by Karasz et al. (30H)by measuring the hemoglobin content. Spleen added to ground beef has been assayed by Bittel et al. ( 5 K ) by determination of water-insoluble iron from hemosiderin in spleen. An improved method for analytical control of cured pork production has been proposed by Perrin et al. (57H) using a fat-corrected protein content. Proximate analysis and lipid analysis data on frankfurters and other meat and poultry products have been determined by Newkirk et al. (52H). Collaborative studies of the detection of caseinate and soy protein by gel electrophoresis in meat products have been conducted by Beljaars et al. (2H). A simple precise electroimmunoassay for whey proteins in frankfurters has been described by Dougherty (16H). Gel electrophoresis has been described by Persson et al. (58H) for the determination of whey concentrate, blood, soya, and egg white in meat products, and by Valas-Gellei (78H) for the detection of soya and milk proteins in the presence of meat proteins. The determination of phosphatide phosphorus in meat products made with bread crumbs has been applied by Lange (38H)to the determination of lactalbumin in these products. Gel diffusion tests with antisera have been found by Appelqvist et al. (IH)to be effective in determining egg and milk proteins in mixed meat products. Canavanine content has been found by Fischer et al. (18H) t o be a means of detecting soya-bean protein a t the 2 % level in a meat product. Preparative electrophoresis of a characteristic protein zone has been suggested by Fischer et al. ( I 9 H ) as a confirmatory test for soy in meat. Stereological tests have been proposed by Flint et al. (20H for the determination of texturized soy protein in meat products. Special extraction procedures have been described by Guy et al. (2314)for the estimation of soy proteins in meat by gel have described the electrophoresis. Hofmann et al. (26H) detection of foreign proteins in meat by their characteristic patterns on gel electrophoresis. T h e qualitative detection of soy derivatives in meat products by gel electrophoresis has been described by Hyslop (28H). T h e effect of added soy protein on the electrophoretic patterns of the water-soluble proteins of cooked beef has been investigated by Kotula et al. (3711). Isoelectric focusing has been applied by Llewellyn et al. (40H) to the detection of soy proteins in food products that have not undergone extensive heat treatment. Laser

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densitometry after gel electrophoresis has been proposed by Parsons et al. (56H) to the quantitative identification of plant proteins in food products. Five percent of cows’ milk in sheeps’ milk has been detected by Ramos et al. (67H) using polyacrylamide electrophoresis. This same technique has been used by Prager (63H) to differentiate rennet from other milk-clotting enzymes. Factors affecting the precision of the electrophoretic method for the determination of cows’ milk in goats’ milk and cheese have been discussed by Pierre (60H). Gelatin in milk and yogurt has been determined by Klostermeyer et al. (35H) by hydroxyproline measurement. The whey protein fraction in milk powders has been assayed by Mrowetz e t al. (50H) by polarography. T h e same authors (51H) have used a similar technique to measure the degree of heating of skimmed milk powders. Iodine number, linoleic acid content, and saturatedkinsaturated fatty acid ratios have been suggested by Piero et al. (59H) as a means of differentiating between human and bovine milk. Linear discrimant analysis has been applied by Smeyers-Verbeke et al. (73H) to gas chromatographic data for the identification of pure milk from different species. Methods of determining the true protein content of mushrooms have been investigated by Weaver et al. (8123 and nine strains of mushrooms examined. Methods for the evaluation of purity and quality of nuts have been discussed by Zuercher et al. (82H). Rocket electrophoresis has been found by Merkl (48H) to provide a means of distinguishing soybean protein and ground mustard in sausage. A screening method for proteins described by Pinto et al. (61H) uses circular paper chromatography and provides a profile sufficient for identification purposes. Chemical evaluation and electrophoretic patterns have been studied by Kapoor (29H) for three varieties of soy beans. Tables of amino acid analyses for 312 proteins have been compiled by Kirschenbaum (33m. Data useful for the determination of the authenticity of vanilla extracts have been compiled by Martin e t al. ( 4 5 H ) . The measurement of specific carbon-14 activity has been used by Schmidt et al. (69H) to distinguish between vinegar made by fermentation and t h a t made from synthetic acetic acid.

INORGANIC In view of the very large number of publications reporting results for inorganic components of foods, the size constraints of this review have made critical selection necessary. Therefore, of those papers coming to the authors’ attention, selection was made on the basis of solutions offered to problems confronting the food analyst, as well as new and innovative techniques already taken to some stage of applicability. Crosby ( 3 1 4 compiled a large review on metals determination in foods. Schuller ( 9 9 4 extensively reviewed methods for cadmium, lead, mercury, and methylmercury. Simultaneous multielement instrumental techniques have been applied to food more often but the equipment is still beyond the financial reach of small laboratories. Schelenz (9RJ) used neutron activation analysis (NAA) followed by chemical separation to estimate 25 elements in a normal human diet. Yeh et al. (1144 reported results for 22 elements in unpolished rice, acid digesting and separating interfering elements after neutron irradiation. Meloni et al. ( 8 4 4 also analyzed rice using columns of Sb2O5,Cd, SnO,, and MnOz to separate nuclides. The elements As, Cd, Cu, Sn, and Zn in beef extract were determined in an NAA scheme of analysis by Korob et al. ( 6 9 4 . Yang e t al. ( 1 1 3 4 used dinonylnaphthalenesulfonic acid to concentrate trace elements before NAA. The X-ray fluorescence method was applied to milk samples by Langhorst et al. ( 7 3 4 , compressing freeze-dried solids into disks. King ( 6 8 4 applied this X-ray technique to a variety of foods, analyzing 10 to 15 samples for five or more elements per day. Norrish et al. ( 9 0 4 reported on X-ray analysis of foods for low atomic number elements while Hutton et al. ( 5 5 4 covered those above 20. Menke (864, after acid digestion, separated metals from food samples by ion exchange and deposited them on carriers before an X-ray measurement. Gabriels et al. ( 4 2 4 employed a triggered intermittant dc arc to determine 11 metals in plant ashes by direct reading emission spectrometry. Sample preparation, including organic matrix destruction, has always been the first obstacle to overcome in minerals analysis. Holak (534 described a temperature programmable

furnace speeding up this process. A low temperature asher useful for small samples was developed by Fukami et al. (404. Jackson et al. ( 6 1 4 modified a Technicon continuous digester as part of an automated wet oxidation-metal chelate extraction system before plasma emission spectroscopy. An apparatus for Wickbold combustion in an oxygen-hydrogen flame was described by Kunkel ( 7 1 4 and used for Cd and P b in foods. Maurer ( 8 2 4 investigated extraction methods suitable for simultaneous atomic absorption (AA) determination of Na, K , Ca, Mg, Fe, Cu, Zn, and Mn in foods. Fry et al. (394 gave their design for a burner nebulizer that allowed direct AA introduction of high solids liquid foods. A glass nebulizer was designed by Ramelow et al. ( 9 7 4 into which fixed volumes of sample digests were injected, enhancing AA sensitivity. Lord et al. ( 7 8 4 diluted mussel solids with naphthalene to introduce them into a graphite furnace for AA analysis. Various digestion procedures were studied by Grobenski et al. ( 4 7 4 to match the best to food sample types intended for graphite furnace atomic absorption. Harbach et al. ( 5 0 4 recommended direct ashing of fruit juices in a n AA graphite furnace for heavy metals analysis. A 50-kL cell was ued by De Angelis e t al. ( 3 2 4 to determine P b , Cd, Zn, Cu, or T1 ions from soya beans and oysters by thin-layer differential pulse voltammetry. The determination of arsenic and arsenicals in foods made up a large part of an extensive review by Lewis ( 7 6 4 . Ihnat et al. ( 5 8 4 reported similar results for his and commercial arsine generators used in hydride evolution atomic absorption measurements. Wauchope ( 1 1 0 4 swept arsine generated from sample solutions into a 1000 “C heated tube for AA determination. An oxygen-hydrogen flame was employed by Siemer e t al. (1034 who dry ashed their samples with Mg(N03), before borohydride arsine generation. The arsenic from a fixed ash was extracted into CHC13as As3+ and then back to an aqueous solvent before graphite furnace AA in Ishizaki’s (604 work. Smith et al. ( 1 0 4 4 built a simplified arsine generation apparatus using a hydrogen diffusion flame a t the ends of a heated silica tube. Fleming et al. ( 3 8 4 described their apparatus incorporating an open-ended heated silica tube capable of detecting 10 ng As as ASH,. Arsenic and mercury were determined by Meloni e t al. (854 by neutron activation analysis after the irradiated samples were digested and mercury was separated by adsorption on copper. Brodie ( 1 8 4 compared carbon rod and hydride generation methods for arsenic and selenium AA determination and gave their respective advantages. As, Co, and Mn in solid samples were low-temperature-ashed by Donohue et al. ( 3 4 4 before spark source mass spectroscopic determination. A photometer with interference filters was used by Pickett et al. ( 9 3 4 to measure the boron emission in an air-hydrogen flame of diol-chelated plant extract. Bhatnagor et al. ( 1 4 4 described preparin a resin from guar gum that was selective to boron and c a p a h e of concentrating that element from dilute solutions. Methodology for cadmium in food and water was reviewed by O’Laughlin et al. ( 9 2 4 , covering a variety of instrumental techniques. A routine for screening foods for cadmium as well as lead, copper, zinc, and arsenic, was given by Allenby et al. ( 2 4 with direct solution or chelation/concentration and AA as the end step for all but arsenic which was done by Gutzeit. Jones et al. (635) employed a dry ashing procedure before electrochemical analyses for Cd, Cu, Pb, and Zn in which the first three were simultaneous differential pulse anodic stripping and the latter was cathodic scan differential pulse voltammetry. Bajo et al. ( 1 1 4 reported a liquid-liquid extraction with cadmium chelated with diethyldithiocarbamic acid to effect a separation after neutron irradiation. A Io8Cd “spike” added to analytical sample ash enabled Chow et al. ( 2 7 3 to ratio i t to and thereby calculate the ”‘Cd in fish samples by a mass spectrometric method. Calcium in meat hydrolysate was reacted with metalphthalein in a semi-automated method described by Arneth et al. (7J). T h e elimination of a MnO, precipitation problem in the final MIBK solution for AA analysis was shown by Kumpulainen et al. ( 7 0 4 in their publication on chromium analysis of cereals. In analyzing milk and cream for Cu and Fe, Haenni et al. ( 4 9 4 dispersed solids in ammoniacal dioxane before graphite furnace AA. A method for copper in meat based on a luminescence reaction with luminol was reported by Angelova et al. (64. Copper in sugar samples was chelated with 2’-pyridylhydrazone and extracted into amyl alcohol before


flame AA in the procedure of Lee et al. ( 7 4 4 . Copper determination in palm oil was accomplished in several ways by Fung e t al. ( 4 1 4 including flame and furnace AA as well as cupric-selective electrode. Gelman ( 4 4 4 reported a modification to an atomic absorption method for cobalt where he first extracted with cupferron to remove iron interference from liver samples. A pressure digestion vessel was used for nitric acid digestion of trout samples before APDC extraction and graphite furnace AA in the work of Harms et al. ( 5 1 4 . Karlsson et al. ( 6 6 4 determined iron by coulometric titration of iodine released in a cell in a method applied to cocoa. Boehm et al. ( 1 6 4 used the polarographic wave at 4 . 8 to -0.9 V to calibrate for iron in wine after nitric acid-peroxide digestion and electrolyte addition. A collaborative study on P b , Cd, Zn, and Ar in clams and oysters was reported by Capar ( 2 2 4 in which, after sulfated dry ashing and chelation into I-pyrrolidinecarbodithioate, the elements were aspirated for atomic absorption in butyl acetate. Bruhn et al. ( 2 0 4 low-temperature dry ashed milk and, after masking other ions, aspirated the APDC complexes of P b and Cd into an AA apparatus. A collaborative study ( 4 4 on a method for P b in beer down to 0.2 ppm recommended addition of Na dioctyl sulfosuccinate to aid solvent separation during extraction/chelation before atomic absorption. Carbonated drinks were analyzed for lead using 4-benzoyl3-methyl-1-phenylpyrazolin-5-one as complexant before AA spectrometry in the work of Akama et al. ( 1 4 . Shamsipoor et al. ( 1 0 0 4 ashed plants in silica boats in an oxygen stream and then sublimed the lead in another tube a t 1000 "C in hydrogen before dissolving it in acid for AA measurement. Mercury analysis in food and environmental samples by neutron activation (NA) was reviewed by Zmijewska (1165). A NA method for Hg in wheat flour by Polkowska-Motrenko (94.4, reported as sensitive to the ppb level, acid-digested the samples after irradiation, and used columns of trioctylphosphine oxide and Dowex 1-X8 resin to separate and count, respectively, the lg7Hg. Another NA method by Zmijewska ( 1 1 5 4 for Hg in foods irradiated samples in capsules wrapped in Al foil, followed by sample digestion, cleanup, and extraction of Hg with 2-mercapto-N-2-naphylacetamide for counting. A collaboratiLe study reported by Munns et al. (895) found V 2 0 j catalyzed fish sample digestion for Hg analysis equivalent to, but safer than that of AOAC method 25.103. A committee recommendation ( 2 6 4 was for peroxide wet oxidation of fish samples followed by cold vapor Hg AA. Brun et al. (214 modified a mercury vapor generation apparatus for the reducing reagent addition. Mercury in oils was determined by Tsai et al. ( 1 0 7 4 by Schoniger type combustion before flameless AA. A technique for atomic fluorescence of cold Hg vapor after combustion, collection on gold, and thermal release was published by Cavalli et al. ( 2 5 4 . Ohkawa et al. (915) modified a Hg method for combustion, trapping on gold powder, and cold vapor AA in which samples were alternately valved for combustion or spectrometry every 10 min. Horimoto et al. ( 5 4 4 described their apparatus for samples of up to 1.2 g of fish in which pyrolysis in N2 was followed by combustion of vapors in O 2 before silver amalgamation and flameless AA. A method for organic mercury was given by Matsunaga et al. (81.4involving a long ambient HCl digestion before benzene extraction and conversion to Hg vapor for gold adsorption/desorption cold vapor AA. Watts et al. ( 1 0 9 4 acidified defatted fish, extracted methylmercury with benzene, and performed EC-GC. Matsunaga et al. (805) also reported using Cu2+directly on homogenized fish tissues to free Hg2+ before SnC12 reduction and cold vapor AA. Gladney et al. ( 4 5 4 modified a method by Rook to permit detection of nanogram amounts of mercury by a carrier-free flameless AA measurement. Dogan et al. (334investigated ways of utilizing copper powder to trap Hg vapor before thermal release and cold vapor AA. Coppon et al. ( 2 4 4 determined both inorganic Hg and organic Hg by EC-GC of benzene extractables before and after a tetramethyltin reaction. Auslitz ( 1 0 4 evaluated a Teflon-line autoclave for digestion and found mercury results higher than by a wet digestion. A titrimetric method based on inhibition of the iodine-azide reaction by the nickel-diethyldithiocarbamate complex was reported by Kurzawa et al. (72.a which had a range of 0.14 to 1.4 pg Ni. Sodium in cheese was determined by AA directly on the sample dispersed in ammonia/MIBK in a paper by Maurer (834.Dufek et al. (354in analyzing oils for rhodium both by H 2 S 0 4digestion

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and direct AA aspiration in MIBK, reported equivalent results for both. A variety of approaches to trace selenium analysis have been successful. Shimoishi ( 1 0 1 4 , after acid digestion of dairy products, formed the 4-nitro-u-phenylenediamine complex and subjected it to EC-GLC. Poole et al. ( 9 5 4 also formed this selenium derivative for electron capture GC, but dry-ashrd solid samples, fixing the ash with Mg(N0J2.6H20. Another electron capture method by Stijve et al. ( 1 0 5 4 made use of reaction with 4-bromo-u-phenylenediamine before isooctane extraction. Shimoishi ( 1 0 2 4 investigated various 1.2-diaminobenzene derivatives of selenium for spectrophotometric and electron capture utility. Fluorimetric methods using selenium complexation are also very sensitive. Mitchie et al. ( 8 7 4 compared digestion techniques and made recornmendations for that and the formation of the naphthalene diamine complex as per the AOAC fluorimetric method. Brown et al. ( 1 9 4 automated a fluorimetric selenium method and cited some interferences. Sydlowski (1064 reported his < ~ ) n parative study of flameless AA and fluorimetric selenium methods, using the same decalin solution of compieu alii1 finding equivalent end results. Ihnat ( 5 6 4 employed a c a1,t1011 rod furnace to atomize selenium separated from wet ash solution by ascorbic acid precipitat.ion. This author (57J) also reported his test of carbon rod atomization vs. a hydrogen selenide generation technique. A carbon furnace AA niethiid by Ishizaki ( 5 9 4 began by oxygen flask combustion and followed through ion-exchange separation before dithizone complex extraction. Andrews et al. (5.5) reported a flow where selenium emerging from an ion exchange columii was alternately plated and anodically stripped from a gold electrode. The 3,3'-diaminobenzidine complex was septirard by solvent extraction before cathodic stripping voltammetry in a paper by Blades et al. (154. Tin traces were separated from foods by Manolov et al. ( 7 9 4 as Brilliant green -SnUr6' complex before conversion to the pentahydroxyflavone complex for spectrophotometry. A graphite furnace scheme by Hocquellet e t al. ( 5 2 4 for tin utilized st,andard addition and gave other steps for interferences or very low levels. Amakawa et al. ( 3 4 co-precipitated tin with zirconium hydroxide for a separation stage after wet sample ashing a n d before flameless AA. An isotope dilution method by Wals et al. (108Jadded the "F isotope before organic solvent extraction and scintillation counting. Yamada ( 1 1 2 4 reported a fluoride ion-specific electrode measurement on tea as agreeing with a combustion-distillation alternate. Vickery et al. ( I I I J ) shobved ways to suppress interfering ions from plant samples tiy using masking reagents with a fluoride electrode. The discontinuance of AOAC method 14.129 was recommended hy Brammell ( 1 7 4 because of loss of chloride during ashing and the 32.A01 potentiometric one favored. A version of the Hg chloranilate colorimetric method for Cl-, using Schoniger t1a.k combustion, was used by Likussar et al. ( 7 7 4 for plants. The negative effects of some emulsifiers and st,abilizers on the Volhard titrimetric chloride method for meat were investigated by Kapel et al. (655). Arneth et al. (8J)discussed use of an apparatus to provide semi-automatic analysis of chloride in meat hydrolyzates by spectrophotometry of the ferric complex in perchloric acid. A bromide ion electrode's usefulness for cereal analysis was enhanced by ion-exchange preliminary separation in the work of Banks et al. (13J). Iodometric, potentiometric, and specific ion electrode methods for bromide in brominated vegetable oils were compared by Conacher et al. ( 2 8 4 . Iodine in plaxts was determined by .Johansen et al. ( 6 2 4 using neutron activation irradiation before caustic fusion/ashing, CC14 extraction as I2 and final ccxintiiig as precipitated AgI. An iodide electrode response was compared to X-ray fluorescence by Craven et al. (30.4 for milk analysis. and found similar. Formation of iodobutanone and sensitive detection by EC-GC was used to advantage in the procedure of Bakker ( 1 2 4 for total inorganic 1- in milk. Gahrio p t ai. (434 formed iodoacetophenone, and separated it by flame ionization GLC. A modification of an AutoAnalyzer method for protein bound iodine was used by Gloebel (46.J) for inorganic I in milk and vegetable extract. Automated phosphate analysis in tissue hydrolyzates without complete digestion was achieved by Arneth et ai. ( 9 J ! by reading solutions with and without molybdate--vanadate reagent. Prevot et al. ( 9 6 4 could determine less than i p p n

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of phosphorus in edible oils using AA with an electrodeless discharge lamp. Photometric phosphorus emission in an inductively-coupled argon plasma responded over the range of 5-40 ,ug/mL in a method applied to milk powders by Gunn et al. (484. Kawaguchi et al. ( 6 7 4 also used an ICP-emission technique applying it to milk and starch. A graphite electrode with a plunger, packed with magnesium carbonate-ashed oil residue was sparked and the P emission lines were used in a spectroscopic method by Kantor et al. ( 6 4 4 . A method for nitrite in meat based on the quenching of 4-aminobenzoate fluorescence was reported by Coppola et al. (294. Lew ( 7 5 4 explained how to remove sulfite interference in colorimetric nitrite analysis by use of formaldehyde. A comparison of cadmium reduction and diphenylamine methods for nitrate was undertaken by Mrowetz et al. (884, mentioning sugar interferences with the latter. Sulfur in fats was converted to H2S before reaction with N,N-dimethyl-p-phenylenediamine/FeCl, and colorimetry in the analytical scheme of Dumitru et al. (364. Many methods for the determination of oxygen in beer were reviewed by the European Brewing Convention Analysis Committee (374. An enzymic method for oxygen using ascorbic acid and ascorbic oxidase was applied to brines and solutions by Capietti e t al. (234.

MOISTURE A method is described ( 8 K ) for the rapid determination of water activity in foods wherein weighed samples of foods having low or intermediate moisture contents are placed in a series of desiccators containing saturated salt solutions providing relative humidities over the range of 0 to 987~R.H. After 2 h, the samples are reweighed and the point at which a curve which is drawn by plotting gains or losses in weight vs. R.H. crosses the datum line represents the equilibrium R.H. of the sample. Troller (17K) provides a statistical analysis of a, measurements obtained with the Sina-scope hygrometer for intermediate moisture foods, and Malkki and Salminen (12K)recommend and make use of MgS04.7H20as a model substance to act as a control in their study of variations in experimental conditions in the determination of moisture in cereals by oven drying. A method is described for the determination of the dispersion of water droplets in water-in-oil emulsions (18K) such as occurs in margarine and butter, and a modification has been found to be necessary t o apply the AOAC method for determining moisture in corn syrups ( 3 K ) to those now produced by the wet milling industry. A comparison was made of the ISO, AOAC, and the IAS methods for determining water in meat and meat products (It?? with only slight differences found in the results, with the IS0 method being found the most precise and the AOAC method being rated as the fastest and simplest to perform. Kreiser e t al. (9K) provide data showing the manual Karl Fischer method to be more accurate, more precise, and faster than either the OICC method or the AOAC official method for determining moisture in milk chocolate, and a procedure is given for rapidly measuring moisture in fresh fruits and vegetables (16K) wherein the organic solids are quantitatively oxidized with a Cr03-H2S04reagent and calibrations are given for this chemical procedure against vacuum-oven drying for 18 species of fruits and vegetables with a reported correlation of 0.99 and a precision of &2%. IJse has been made of a commercial type microwave oven for the rapid determination of moisture in canned pet food ( I I K ) with the results obtained comparing favorably against those obtained by conventional oven-drying, Steele (14K) describes microwave methods and conditions for a wide variety of foodstuffs, reporting that up to 6 g of sample can usually be dried within 5 min, and Pieper et al. (13K) describe a microwave oven technique for the rapid determination of moisture in cheese and provide favorable comparative data against data obtained by Official AOAC methods. A system is described for effecting the continuous measure of moisture in foodstuffs by monitoring changes in the dielectric constant ( 5 K ) with a discussion of the factors influencing the measurement, and Feller provides a technique for determining the extract content of beer based on the continuous measurement of dielectric constant by means of a Boonton capacitance bridge ( 4 K ) and demonstrates the applicability of the technique by an evaluation of the results by multiple linear regression analysis and comparison with values obtained by refractometry and density measurements.

Methods are given for the measurement of moisture content in wheats (ZOK) and whole kernel corn and sorghum grains (15K) by near infrared reflectance spectroscopy, and Campbell et al. ( 2 K ) describe a rapid IR method for determining the moisture in walnuts over a range of 3-3070 by blending with absolute methanol and comparing the absorbance with that of standards at 1440 nm. Hester and Quine report on the analysis of water in flour and feedstuffs (7K) and in skim milk powder and cottage cheese curds ( 6 K ) by the use of pulsed NMR techniques and provide comparisons against standard methods.

ORGANIC ACIDS An assay for acetate in wines and fruit juices was reported to be more accurate by a procedure involving coupled enzymic reactions than by steam distillation-titration in a paper by McCloskey (32L). Propionic acid in foods (distillate) was determined by forming the phenacyl ester before GC in the work of Nose et al. (35L). Bergner-Lang ( 7 L ) determined citric and r,-malic acids in wine enzymically, first hydrolyzing polyhydric phenol esters to reduce interferences. Baldesten et al. ( 4 L ) employed isotachophoresis to separate ascorbic, isoascorbic, citric, isocitric, formic, and lactic acids as well as cyclamate from various food matrices. The separation and measurement of pectin, poly-, and monogalacturonic acids was accomplished in a combined ion-exchange chromatography--solubilization scheme by Bartholomae (5L). Drawert et al. ( I I L , 15L) reported group separations of organic acids as well as carbohydrates and amino acids from grape must, wine, work. and beer in their P V P and ion-exchange column preliminary workup before TMS-GC. Gas chromatographic determination of 53 organic foodstuff acids was made as volatile silanized derivatives in a paper by Drawert et al. (13L). ‘The uses of ion-pair reagents to affect HPLC behavior of organic acids was described by Terweij-Groen et al. (46L)and applied to sorbic, benzoic, and salicyclic acid analysis. Nakajima et al. ( 3 4 L ) reported a carboxylic acid analyzer based on ion-exchange chromatography, shcwing separation of ten acids. Kasai et al. (27L)applied an automated ion-exchange chromatography/photometric analyzer to white wine analysis. Automated and manual versions of an enzymic lactate-in-milk analysis were described by Sukren et al. (44L). Total lactate in soya sauce and wine and r>(+)lactatewere determined using an acid analyzer and automated enzymic procedure, respectively. in a publication by Kanbe et al. (26L). List et al. (3OL) employed a long Aminex A-25 ion-exchange column monitored by a refractometric or UV detector to measure raw sausage acid composition. Marsili (31L) used GC of T M S derivatives to show that lactic was the only acid produced in fermenting cucumber juice. Pilone (37.L)found that Bio Beads SM2 decolorized samples of wine better before tartaric acid-vanadate colorimetry than a carbon treatment. T h e oxalic acid content of vegetables was determined by spectrophotometry of a red 1,S-diphenyl formazan finally formed after intermediate conversion to glyoxalic acid hydrazone in the method of Sachse (40L). Roberts et al. (39L) estimated glucuronic acid found in sugar cane. employing stages of dialysis, methanolysis, hydrolysis, and TMS-GC. Ciha et al. ( 9 L ) reported a rapid method of isolating and measuring abscisic acid in soya beans by extraction and HPLC. A thin-layer separation before HPLC allowed Duering (1215)to analyze grapes for abscisic and indole-3-ylacetic acids. Residues of (2-hydroxy-4-(methylthio)butyricacid) in milk and cow tissues were measured with S-photometric detection GC in the method of Pease et al. (36L). Farkas e t al. ( 2 I L ) made use of the first polarographic reduction wave of 3-(5nitro-2-fury1)acrylic acid to measure it in wine. Phytate in vegetable protein products was determined by ion-exchange concentration before hydrolysis and P analysis by Harland et al. ( 2 4 L ) . Esterbauer et al. (20.L) investigated isomeric trihydroxyoctadecenoic acids as cause of beer stale flavor, employing column chromatography and then GC after T M S derivative formation. Volatile phenols in beer and its ingredients were followed using a TMS-GC method by Kieninger et al. (29L)to assess malt changes due to a drying kiln. Wine total phenols analysis was reportedly improved in an automation of a known method according to Slinkard et al. (42.L). A column of polyacrylamide gel fractionated white wine phenolic acids previous to TLC and spectrophotometry in the work of Castino et al. ( 8 L ) .

ANALYTICAL CHEMISTRY, VOL. 51,

Bendelow (615) automated a polyphenol method using 4aminoantipyrine reagent and applied it to beer and ingredients. Tannins from plant extracts were recovered from Sepharose columns of immobilized bovine serum albumin before final measurement in a publication of Hoff et al. (25L). Tea tannins were determined differentially by Folin-Denis reagent color before and after a gelatin-Kaolin precipitation in the technique of Bajoj et al. (3L). Price et al. (38L)claimed rapid results for tannin in sorghum with a direct Prussian blue test. Thirty-seven phenolic components of wine were illustrated by Drawert et al. (14L) in their investigation of T M S derivatives for GLC separation. Similar methods for lower molecular weight phenolics in fermented beverages and ingredients were also discussed by Drawert e t al. (12L). Beer phenolic component analysis was also detailed in work of Drawert et al. (16L) who, after a P V P column separation, chromatographed TMS derivatives on SE-52. Zipax SAX resin chromatography enabled Kenyheroz et al. (28L) to separate and measure beer phenolic components using a polarographic type detection system. Ferulates in rice bran oil were analyzed by Tanaka et al. (45L)by HPLC, calibrating against @-sitosterylferulate. Durkee ( 1 8 L ) surveyed buckwheat seed for the occurrence of polyphenols in the branaleurone fraction using chromatography after hydrolysis. A titanium reagent colorimetric method for total phenols having speed and simplicity was shown applicable to sunflower seed meal by Eskin et al. (19L). Spectrophotometric measurement on TLC plates after extraction and polyamide column cleanup was used by Hanefield et al. (23L)to determine chlorogenic acid and caffeic acid esters in fruits and vegetables. T h e chlorogenic acid change in roasted coffee was studied by Nakabayashi et al. (33L)using differential absorbance at 620 nm in two different buffers. Amperometric/polarographic response a t a carbon paste electrode detector coupled to a polyamide column was used to measure chlorogenic acid in sunflower meal in the work of Felice et al. (22L). Alessandro et al. (1L)distinguished between caffeic and hydrocaffeic acid antioxidants extracted from butter by their spectra after reaction with alkaline methanolic isoniazid and K,Fe(CN) . Components of brewing hops were studied using H P L t ion-exchange, liquid partition, and solid adsorption columns, as well as TLC in group separations obtained by Siebert ( 4 I L ) . Anion-exchange HPLC separated a-acids for Slotema et al. (43L)so their results agreed with a dimethylsulfoxide method for hop bitter acids. A collaborative study (2L)on three a-acid methods for hops reported no statistical difference. Gibberellic acid in malt was detected down to 0.01 ppm in an agar diffusion test by Donhauser (IOL).

NITROGEN This period’s trend in nitrogen methods include the investigation of rapid methods and of automatic methods, and the search for better methods of separating and detecting nitrogen-containing compounds. Emphasis for the Kjeldahl procedure has been on the elimination of polluting catalysts. Hydrogen peroxide has been suggested by Tomonari et al. (118M) as a substitute for copper sulfate and mercuric oxide. Copper sulfate has been substituted for mercuric oxide by Rexroad et al. (99M) and by Manley (BOW. The use of titanium dioxide has been examined by collaborative studies for nitrogen in barley, malt, and beer (5M). Titanium dioxide, copper sulfate, and potassium sulfate has been found by Terada et al. (115M) to give similar results to those obtained by the regular Kjeldahl method, and has been studied collaboratively by Yasui et al. (131M) who also found good agreement with the standard procedure on roasted flours. A version of the standard Kjeldahl method has been proposed by Kubadinov et al. (68M)for the analysis of sugar beet and sugar factory products. A method for the control of mercury from Kjeldahl wastes has been described by Hautala et al. (47M). The ammonia electrode has been used by Eastin (26M) on Kjeldahl digests for the determination of total nitrogen in plants. Felker ( 3 I M ) has determined nitrogen in seed protein extracts a t the microgram level using a colorimetric method on the whole Kjeldahl digest. Automated and macro-Kjeldahl procedures have been compared by Vincent et al. (121M) and the automatic method has been recommended for speed. An AutoAnalyzer has been used by Eastin (27M) for the rapid analysis of total nitrogen in plants. The block digestor technique coupled with AutoAnalyzer colorimetry has

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been described by Hambraeus et al. (44M) for many types of samples. Kaul et al. (60M) have compared the manual micro-Kjeldahl method and the indophenol color reaction and found good correlation between methods. An automated protein-nitrogen combustion method for cereals and grains has been described by Revesz et al. (98M) which measures nitrogen gas with a thermal conductivity detector. The Lowry procedure for protein has been improved by Higuchi et al. (5IM) by the use of chloramine T to give linearity and reduced blanks. An automated modified Lowry method has been applied by Huang et al. (55M) to the determination of protein in milk. A biuret-Folin protein assay has been improved in protein response by Dorsey et al. (23W by the use of heat before the addition of the Folin phenol reagent. T h e biuret method has been adapted by Popineau et al. (95M) to the semi-automated determination of total protein in cereals. Other rapid applications of the biuret reaction have been described by Simmonds et al. (108M) for analysis of cereal grains, and by Sodek et al. (109M) for analysis of Brazilian beans. Chromic acid has been suggested by Swaminathan et al. (113M) as a rapid means of digesting nitrogen for total nitrogen determination. Dye-binding procedures for protein estimation have been described by Medina et al. (83W using a modified Udy method, by Flores (34M) using bromophenol blue, by Romo et al. ( I O I M ) using C. I. Acid Orange 12, and by Sedmak et al. (104M) who recommend the use of Coomassie Brilliant Blue. Infrared reflectance instruments for the determination of protein have been studied collaboratively by Hunt et al. (57M who compared Kjeldahl analyses and IR instruments for protein analysis in wheat and soya beans and found good agreement between procedures. Other studies of IR systems include reports by Fossati et al. (35M) and Watson et al. (125M) on the Technicon InfraAlyzer, studies by Watson et al. (124M) on two NEOTEC Corp Grain Quality Analyzers and a Dickey-john Grain Analysis computer. The IR reflectance method has been shown by Miller et al. (84M) to give results comparable to those obtained by Kjeldahl on hard red winter wheats. The influence of particle size distribution on the response of this type of instrument has been investigated by Calandra ( 1 4 M ) and an optimum size range recommended. The suitability of the near-IR analyzer to large scale wheat testing has been described by Williams et al. (129M). Another IR analyzer, the hlilko-Scan 300 has been found satisfactory by Thomasow (117M) for the analysis of the protein and fat content of milk. Another apparatus, the PROT-0-MAT I11 has been studied by the same author ( 1 1 6 M ) ; this instrument uses the dye-binding principle for protein determination. Analyzers which determine nitrogen and protein, the RAPID N-A and RAPID N-B, after combustion have been evaluated by Kreutzer ( 6 6 M ,who reports good reproducibility and accuracy were found. Other methods of determining nitrogen include gas-phase molecular absorption spectrometry described by Cresser (19M) and applied to kale and barley, and a nephelometric procedure for milk discussed by Beitz et al. (9M). The dye Coomassic Brilliant Blue has been used by Esen (29M) to detect and, after extraction, quantitate proteins separated by paper chromatography. Comparative studies of various methods for the determination of total nitrogen have been reported. LVilliams et al. (130M) have compared Kjeldahl, neutron activation analysis, protein activation analysis, thermal decomposition analysis, Kjel Foss, and Kjel Tec for total nitrogen in wheat and found all reliable, however they report neutron activation analysis in superior in accuracy and precision. Five methods for protein determination in barley and malt have been compared by Pomeranz et al. (94M) including Kjeldahl, dye-binding, biuret, alkaline distillation, and IR reflectance; all agreed well with the Kjeldahl method. Bosset et al. ( I I W have reviewed methods for the determination of the proteins of milk and its derivatives in recent literature. Boudier (12M) has reported that viscosimetry may be used for the determination of protein in milk. An overview of protein separation and analysis by electrophoretic methods has been published by Catsimpoolas (15M). Polyacrylamide gel electrophoresis has been described by Hillier (52M) for the separation and quantitation of whey proteins. Casein proteins have been separated by West et al. (126M) by electrophoresis on cellulose acetate strips. High

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speed ion-exchange chromatography has been proposed by Chang et al. (17M) for separation of proteins. Additional studies by Chang et al. (16M) have described the uses of steric exclusion and anion-exchange supports and a post-column enzyme detector. Casein has been fractionated by El-Negoumy (28W on DEAE-cellulose. A method for t.he determination of the protein value of meat has been suggested by Grigor'ev et al. (43M) which uses the ratio between high-value protein (determined by measuring an unsubstituted amino acid) and low-value protein (determined by measuring hydroxyproline). Plant protein nitrogen has been measured by Gaines (38M) by Kjeldahl after removal of nonprotein nitrogen with 0.5% acetic acid. Muscle protein in beef products has been determined by Herrmann et al. (49M) by its insolubility in 0.1 N sodium hydroxide, and in beef-vegetable protein mixtures by Khan et al. (62M) by measurement of creatinine or by buffer-extraction. Water soluble soy proteins have been separated by Fisher et al. (33M) by a single-step chromatographic procedure. Special extraction procedures for the determination of dissolved and undissolved nitrogen compounds in cheese have been established by Noomen (88M). Normal corn proteins have been reported by Lebedev et al. (7OM) using isoelectric focusing in a density gradient. The quantitative analysis of proteins by the use of sodium dodecylsulfate-polyacrylamide gel electrophoresis has been described by Asad (6M) using a new device which continuously recovers the separated protein fractions. A technique for assaying proteins on Kieselguhr plates has been proposed by Kinoshita et al. (64M using the reaction of sodium hypochlorite on proteins and the reaction of the chlorinated proteins with thiamin to produce thiochrome fluorescence. Conditions for HPLC of peptides and proteins using ionpairing reagents have been discussed by Hancock et al. (46M); these authors also have described the use of phosphoric acid in the mobile phase (45M). Derivatization as an aid in HPLC chromatography has been suggested by Frei (36M) who recommends the post-column detection of peptides with fluorescarnine. Dipeptides have been separated and sequence-determined by Krutzsch et al. (67M by the use of gas chromatography and mass spectrometry. "Gluten-free" foods have been analyzed for trace amounts of gluten by McCausland et al. (74M) using gel electrophoresis. A sensitive assay for biotin analogues and biotin proteins has been proposed by Landman (69M)which adopts the radioisotope dilution method for the assay of biotin to these compounds. Details of the methods of the American Society of Brewing Chemists for the determination of free amino nitrogen in wort and beer have been reported by West (127M). Flow injection analysis has been applied by Sodek et al. (IIOM) to the determination of amino acids by the trinitrobenzenesulfonic acid method. The free a-amino-nitrogen in protein hydrolyzates has been determined by Lieske et al. ( 7 1 M ) by colorimetric measurement of the copper in the amino acid copper complex. Gas-liquid chromatography has been discussed by Nair (87M) as applied to the measurement of amino acids in food samples. The heptafluorobutyryl isobutyl esters of 50 amino acids have been prepared and separated by gas chromatography by Siezen et al. (107M). Protein and nonprotein amino acids have been analyzed by Amico et al. (3M by the gas chromatography of their N-trifluoroacetyl butyl esters. Dansyl derivatives of amino acids have been separated on thin-layer plates by Seiler et al. (I05M) by two-dimensional chromatography. Amino acids in sugar beet and sugar factor). products have been determined by Burba et al. ( 1 3 M ) by t'luorimetric estimation with fluorescamine and phthalaldehyde. Subnanomole sensitivity has been obtained by Lund et al. (73M) on an amino-acid analyzer by the use of 2-phthalaldehyde. Ninhydrin reagent containing titanium trichloride has been used by Rokushika ( I O O M ) in a single wavelength method at 420 nm for the detection of amino acids. T h e practical aspects of reversed phase ion-pair chromatography have been discussed by Gloor et al. (41M including the determination of amino acids and catecholamines. Selected amino acids and amino sugars have been separated by Masters et al. (81M on copper loaded silylated controlled-pore glass. Cysteine and glutathione have been determined in fruit by Saetre et al. (103M by HPLC on Zipax SCX resin; cystine plus cysteine has been determined by de Koning et al. (65M by a n acid ninhydrin method. Polarographic determination

of cysteine and cystine in skim milk powder has been described by Mrowetz et al. (86M). Hydroxxyproline in meat has been determined by Jozefowicz et al. (0'9M) by quantitative carbon-13 Fourier Transform nuclear magnetic resonance spectrometry. Galasinski et al. (39M) have modified the method for hydroxyproline in proteins by changing hydrolysis conditions. Hydroxyproline determination has been suggested by Fey (32M) as a means of establishing the connective-tissue content of meat. Methods for measuring lysine residues in casein have been discussed by Moeller et al. (85M)and the effectiveness of the method for the analysis of sugar-lysine derivatives examined. Procedures for available lysine in processed beef muscle have been studied by Rayner et al. (97M) and the "pronase" method has been found most sensitive. The measurement of free amino groups in proteins by the reaction of fluorescamine has been found by Purcell et al. (96M)suitable for determining available lysine in egg white. A lysine-specific electrode has been used by White et al. (128M for the determination of lysine in grains and foodstuffs. Thin-layer chromatography has been suggested by Datta et al. for the determination of available lysine in pulses (21M) and in dried milk powder (20M). HPLC has been adapted by Wartheson et al. (123M) to the evaluation of free lysine fortified wheat flours. Methionine and histidine have been determined by Kidani et al. (63M) by their reaction with copper and the copper has been determined by atomic absorption spectrophotometry. Methionine has been determined by gas chromatography after reaction with cyanogen bromide in proteins by Varadi et al. (119M). in field beans by Paul (92M), in seed meals by MacKenzie (75M), and in the seeds of legumes by Duncan et al. (25M). Unmodified methionine in intact proteins has been determined by Lipton et al. (72M) by gas chromatography after oxidation by dimethylsulfoxide in hydrochloric acid. The silyl derivatives of methionine hydroxy analogue residues have been analyzed by Pease et al. (93M) by gas chromatography with a sulfur sensitive detector. A specific enzyme electrode for L-phenylalanine has been described by Hsiung et al. (54M). Theanine. glutamic acid, and aspartic acid have been determined in tea by Shiogai et al. (106M) by capillary tube isotachophoresis. A method for tryptophan has been described by Zaitsev et al. (132M) using the reaction with ferric chloride, and this procedure has been automated by Makinde et al. (78M)and applied to a maize-soya fermented food. Another automated method for trjptophan used by Amaya-Farfan et al. (2M) uses the reaction with 4-dimethylaminobenzaldehyde and 1,4dioxan after hydrolysis or homogenization. Coupling with -V-(l-naphthyl)ethylenediamine has been used by Basha et al. (8M)for tryptophan in proteins. The fluorescence of trkptophan has been used by Pajot (9IM) for its determination in proteins, and by Oeste e t al. (89M for its determination in food samples. Hydrolyzing agents for the determination of tryptophan in proteins have been investigated by Creamer et al. ( 1 8 M ) and 2-mercaptoethane-sulfonic acid hydrolysis has been found suitable. An enzymatic determination of creatinine has been found applicable by Ettel et al. ( 3 O M ) to meat extract and foodstuffs containing meat extract. Biogenic amines, tryamine, tryptamine, and histamine in foods have been determined by Voigt et al. (222,W by thin-layer chromatography after extraction. Taylor et al. ( I 14M have described a simplified method for histamine in foods using o-phthaldehyde detection. A study of the volatile amines in tomatoes described by Madarassy-hlersich et al. ( 7 6 M ) collects the amines after steam distillation and analyzes the distillate by gas chromatography. Polyamines and some mono- and diamines in plant extracts have been determined by Villanueva et al. (I2OM) by gas chromatography after acid extraction. Three polyamines, putrescine, spermine. and spermidine have been identified in green and roasted coffee by Amorin et al. ( 4 M ) by thin-layer chromatography. Methylguanidine in food has been determined by Fujinaka et al. (37.W) by a combination of chromatographic techniques, and Kawabata et al. ( 6 1 M ) have determined methylguanidine, guanidine. and agmatine by gas chromatography of their hexafluoroacetylacetonates. Carboxylic acid 5-hydroxytryptamides in coffee have been determined by Hubert et al. (66.447) using column and circular thin-layer chromatography and by Hunziker et al. (68M) by reversed phase HPLC. Acid -soluble nucleotides in citrus juice

A N A L Y T I C A L CHEMISTRY, VOL 51, NO. 5, APRIL 1979

have been measured by Bennett ( I O M ) by HPLC, and by Heyland e t al. (SOW using HPLC on extracts of mushrooms and chicken meat. Polarography, spectrophotometry, and atomic absorption spectrophotometry have been studied by Gawargious et al. (4OM) as indirect methods for mercapto groups. Thiol groups and disulfide bands in flour and dough have been determined by Graveland et al. (42W by amperometric titration. Spectrophotometric titration with copper(I1) in N,N,-dimethylformamide has been applied by Stock et al. ( I I I M ) to the determination of thiols. Ammonium ions have been determined by Devillers et al. (22M) both colorimetrically and by the use of the ammonia specific electrode. Drawert (24M) has used the electrode to measure ammonia in beer, and Helaine (48M) has measured ammonium in milk with this electrode. Spectrophotometric methods for caffeine in coffee and tea have been compared with gas chromatographic methods by Strahl et al. (112M), and modifications to the spectrophotometric method suggested. HPLC has been applied to the determination of caffeine in coffee by Madison e t al. (77M), by Attina et al. (7M) who have also analyzed decaffeinated coffee, and by Adams et al. ( 1 M ) who have analyzed for caffeine and other xanthines. Caffeine, theobromine, and theophylline in tea have been determined by Hoefler et al. (53M) with reversed phase HPLC. A method for caffeine in cola seeds has been proposed by Malingre et al. (79M) using thin-layer chromatography and densitometry. A spectrophotometric assay for caffeine has been suggested by Mattoo e t al. (82M) which measures the difference in absorbance at 273 nm of a neutral caffeine solution and a basic caffeine solution. A rapid method for caffeine in alcohol-free drinks described by Ruick et al. (102M) uses spectrophotometric detection after chloroform extraction. Caffeine in crude caffeine has been determined by Ono et al. (9OM) by gas chromatography. Theobromine and theophylline are also detected by this method.

VITAMINS The need for nutritional data has led to increasing interest in automated vitamin analyses and also to an interest in the use of high pressure liquid chromatography (HPLC) for better separation and detection of the various members of a vitamin complex. Parrish (38N) has reviewed methods for the determination of vitamin A in foods. Colorimetric procedures for vitamin A have been studied by Blake et al. ( I N ) using antimony trichloride and 2,3-dichloropropanol;by Lang et al. (27N) using the reaction of the vitamin with a compound having a free sulfo group in the presence of formic acid, and by Subramanyam et al. (58M who prefer trifluoroacetic acid in methylene dichloride as a replacement for the usual Carr-Price reagent. Two methods for the determination of vitamin A in peaches have been compared by Gebhardt et al. ( I I N ) and the authors warn that the method of analysis may affect nutritional labeling claims. High speed liquid chromatography has been suggested by Dennison et al. (6N) for the determination of vitamin A after saponification and extraction; by Head et al. (17N) after saponification and purification on an alumina column. Reverse phase HPLC has been proposed by Egberg et al. (8,\9 for the determination of all-trans and 13-cis retinol in food products. McCormick et al. (3O~”v?have used straight and reverse phase HPLC to separate cis and trans isomers of vitamin A compounds. Stewart ( K V , 57N) has described HPLC analysis for provitamin A and carotenoids in orange juice. The polarographic behavior of vitamins A and D has been studied by Menicagli et al. (31A9 who found satisfactory recoveries of the vitamins with the use of oscillopolarography. A chemical method for vitamin D in dietetic products has been described by Nabholtz (34N)using column and thin-layer chromatography to separate vitamin D compounds from interfering components. The gas chromatographic determination of vitamin D and related compounds has been proposed by De Leenheer et al. (n‘N) after formation of the methyl ether, and by Kobayashi et al. (26,lr) after separation and trimethylsilylation. High pressure liquid chromatography has been used by Osadca et al. (36.W to determine as little as 2 ng of vitamins D2 and D3, by Ray et al. (45N) for vitamin D3, by Thompson et al. (SON) for vitamin D in fortified milk, and by Wiggins (62N) to separate D, and D3. Oil soluble vitamins in fish and sea crustaceans have been determined

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by Stepanova et al. (53N) using thin-layer chromatography and molybdophosphoric acid detection. A new iron reagent, 3-(2-pyridyl)-5,6-diphenyl-l,2,4-triazine has been suggested by Kanno et al. (23N) as a more sensitive reagent for the determination of tocopherols. A rapid thin-layer chromatographic method for individual tocopherols in oils and fats has been proposed by Mueller-Mulot (33m who has analyzed 24 commercial vegetable oils. Thin-layer chromatography has also been used by Mizobuchi et al. (32N) to analyze oilseed meals for tocopherols. A polarographic method for tocopherols has been studied by Waltking et al. (61N) and found suitable for monitoring the nutritional value of edible oils. Gas-liquid chromatography of butyrated a-tocopherol has been described by Hartman (16N) and applied to the unsaponifiable matter of vegetable oils. Manual and semi-automated methods for thiamin have been evaluated by Defibaugh et al. ( 4 N ) and compared with the microbiological method. Best recoveries of added thiamin were obtained with the semi-automated and microbiological procedures. Ribbron et al. ( 4 6 N ) have compared semi-automated and manual methods for thiamin in baby cereals, and infant and dietary formulas. These authors suggest that for automated methods the thiamin standards must be treated in the same way as the samples. A new compound, having a thiamin odor, formed by ultraviolet radiation of thiamin has been identified by Seifert et al. (SON). Chemical and biological methods for thiamin have been compared by Gregory et al. (13A9 and the need for preliminary tests for the purification methods for each product assayed is stressed. Extraction procedures for thiamin and riboflavin in foods for use in automated methods have been described by Pelletier et al. ( 4 O ~ vA . study of the conditions for the standard fluorescence method for riboflavin has been made by Pickova ( 9 I N and modifications are suggested. The use of an urea-acid system for the extraction for riboflavin before automated analysis has been proposed by Roy et al. ( 4 9 N ) . An improved reagent system for automated riboflavin analysis has been described by Jacobson (2ON) which substitutes hydroxylamine hydrochloride for hydrogen peroxide to reduce excess permanganate. Riboflavin has been determined in foods by HPLC by Richardson et al. ( 4 7 N ) and the results have been compared favorably with the microbiological procedure. Methods for vitamin B,include a spectrophotometric assay tor pyridoxal and pyridoxamine 5’-phosphates described by Suelter et al. (59N) using a chromogenic substrate. Fluorimetric methods for vitamin B, compounds after chromatographic separation on Domex AG 5OW-X8 have been proposed by Gregory et al. (14P.9, and by Fiedlerova et al. (9N)using a similar technique on dried milk, wheat and soya flours. Gas chromatography has been proposed by Patzer et al. (37N)for vitamin B, using derivative formation with N-methyl-bis(trifluoroacetamide). Vitamin B,, has been determined by Herrmann et al. ( 1 8 N ) using an enzymatic procedure, which utilizes adenosylation of the cobalamins by vitamin BL2coenzyme synthetase. Automated separation of B-group vitamins has been achieved by Noe et al. (35N) by automated analysis on a cation-exchange resin. A fluorometric assay for avidin and biotin has been proposed by Lin et al. (29N) by the measurement of the quenching of the tryptophan fluorescence of avidin by biotin. Chromatography of folates on Sephadex G 10 has been used by Kas et al. (24N) to measure these compounds in milk, and HPLC has been applied to the measurements of folates in food by Clifford et al. (31L1.Alternating current polarography has been used by Jacobsen et al. (21,V) to determine folic acid. Methods for ascorbic acid include colorimetry described by Hammam ( I S N ) using dimethoxydiquinone in water solution and by Kamangar et al. (22N) using the same reagent and reading the color after extraction into chloroform. A kinetic method for ascorbic acid has been described by Hiromi et al. (19N) using the reaction with 2,6-dichlorophenol -indophenol in a stopped-flow apparatus. Spectrophotometric measurement has been proposed by Lehnard (28N)by oxidation of the ascorbic acid wiLh N-bromosuccinimide, the excess reagent is in turn determined by its reaction with iodine. The stability of L-ascorbate-2-sulfate and L-ascorbate in wheat foods and milk has been determined by Quadri et al. (42N) by measurement of the extinctions a t 245 and 255 nm after extraction and clarification. Steele et al. (54N) have applied the dinitrophenylhydrazine, indophenol-formaldehyde, and

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ANALYTICAL CHEMISTRY, VOL. 51, NO. 5, APRIL 1 9 7 9

polarographic ascorbic acid methods to potatoes and conclude that interferences with the methods can occur after various processing steps. The reaction of ascorbic acid with bromine chloride has been used by Shukla et al. ( 5 I N ) for the microdetermination of ascorbic acid. The use of azine dyes has been proposed by Rao (43N) as indicators for the titration of ascorbic acid with iodine. Automated flow-through methods for ascorbic acid, and thiamin, and for retinol using HPLC have been reviewed by Kirk (25N). Other automated or semi-automated methods for vitamin C have been described by Egberg et al. (7N) using fluorometric measurement, by Pelletier et al. (39M who compare automated and manual methods, and by Roy et al. ( 4 8 N )who describe an automated fluorimetric method. Ascorbic acid in fruit juices has been determined by Sontag et al. (52M using differential pulse polarography in sodium acetate-oxalic acid buffer, and Ratzkowski et al. (44,V) have used rapid-alternating current polarography to differentiate ascorbic acid from erythorbic acid in foods. A procedure for the determination of ascorbic acid in foods has been described by Sood et al. (53N) using HPLC. Eight water-soluble vitamins have been separated by Wills by et al. (63N) by HPLC with several eluants. Vitamins, thiamin, pyridoxine, and ascorbic acid have been determined by Garcia-Gutierrez (12N) by measurement of transmission values after diazotization. Frouin et al. (ION) have reported that in some products there is a risk of error caused by the masking of vitamins, i.e., riboflavin and thiamin, when determined in food products by standard methods. A review by Christie (2N) has presented progress in determining vitamins; separations and analytical methods are discussed.

MISCELLANEOUS An outline is given (2P) of the principles for thermal analytical techniques along with applications to the examination of food ingredients and packaging materials, and Herrmann (12P)provides a review of the nonessential constituents of selected vegetables with particular emphasis on volatiles, organic acids, phenolics, carotenoids, sterols, bitter principles, and nonprotein nitrogen compounds. Included in “The Proceedings of the Seventh International Colloquium on the Chemistry of Coffee” (23P)are a number of papers of general analytical interest containing methods and data for many aspects of this commodity. Delaveau et al. (6P) report on their testing of standard methods of analysis for chewing gums on 2 2 gum samples, and a aescription is given (25P) of the theory, techniques and trends in flow injection analysis systems. A summary is given (15P)of the Third International Symposium on Column Liquid Chromatography, and Mendenhall discusses apparatus for measuring chemiluminescence (18P)and reviews the uses of such measurements for studying foods .nd polymers. Bowers et al. (3P) review analytical applications of immobilized enzymes, and Gajzago et al. ( I I P ) describe the measurement of the browning rates of various fruits by reflectance spectrometry. Use was made of near infrared spectrophotometry for measuring the ethanol, acid, and sugar in wine ( I 4 P ) ,and Watson (27P) reviews instrumentation and methods which make use of near IR reflectance spectrometry for the rapid and acccurate determination of protein, oil, and moisture in agricultural products. Cervinka and co-workers ( 4 P ) have applied this latter type of instrumentation to the determination of fat, protein, and lactose in milk and have developed a mathematical model for projecting the solids content as well. A comparison was also made (19P) of the performance of two commercial types of these instruments against standard methods for the determination of protein, water, and extract in malt, concluding that the instruments could provide similar results more rapidly. Froede describes new analytical apparatus (IOP) for performing the “chill-haze” and “filtration” tests for the quality control of bottled beers, and Beitz et al. ( I P )provide a nephelometric procedure for determining the fat and protein in milk. A review is presented by Noble (2OP)of instrumental methods for the measurement of the sensory properties of food, and Uriano and Gravatt (26P) discuss the use of reference materials and reference methods in chemical analysis and list the standard reference materials issued by the National Bureau of Standards with examples of their uses. Horwitz discusses principles requiring constant attention from the analyst in the development of sound analytical

methods (13P),and Dols and Armbrecht (8P)define a strategy to maximize the efficiency of method development.

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128R


(95C) White, J. W., Jr., J . Assoc. Off. Anal. Chem.. 60, 669 (1977). (96'2) Wood, P. J.. Paton, D., Siddiqui, I. R.. Cereal Chem., 54, 524 (1977). (97C) Zuercher, K., Hadorn, H., Dtsch. Lebensm.-Rundsch., 72, 197 (1976). (98C) I b i d , Mht. Geb. Lebensmittelunters. w g . , 67, 379 (1976); Anal. Abstr., 32, 3F25 (1977).

Color

Fats, Oils, and Fatty Acids

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.-.

(13E) Ibid., p 18. (14E) Siegenthaler, U.. Mitt. Geb. Lebensmittelunters. Hyg., 68, 251 (1977). (15E) Stadhouders, J., Hup, G., Van der Waals, C. B., Neth. Milk Dairy J . . 31, 3 (1977); Chem. Abstr.. 87, 37457b (1977). (16E) Zuercher, K., Rychen, O., Hadorn, H.. Gordian. 76, 288 (1976); Chem. Abstr., 86. 70176m (1977).

I

- . . I

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. .-

1 1 R 1197fii -,. \ I _ .

(33F) Gray, I. K., N . Z . J . Dairy S o . Technol.. 10, 158 (1975); Anal. Absfr., 31 . . , 6F15 . . 119761 -, (34F) Grossmann. A., Timrnen, H , Klosterrneyer. H., Milchwissenschaff. 31, 721 (1976); Chem. Absfr., 86. 1380659 (1977). 135F) Guhr, G., Waibel, J.. Fette, Seifen, Anstrichm.. 80, 106 (1978). (36F) Guilbumin, R., Forney, M., Bosquet, M. F.. Rev. Fr. Corps Gras, 23, 425 (1976); Anal. Abstr., 32, 3F31 (1977). (37Fl Hallermayer. R . . Dtsch. Lebensm.-Rundsch.. 72, 356 (1976); Chem. Absfr.. 86. 3633v 11977). (38F) Heidemann, G..'Lekim. D., J . Chromatogr., 126, 235 (1976). (39F) Heisz, O., GITFachz. Lab., 21, 22 (1977); Anal. Abstr., 33, 2F48 (1977). (40F) Helal, F. R . , Ahmed, N. S., hlilchwissenschaff, 31, 288 (1976); Anal. Abstr.. 32, 2F26 (1977). (41F) Hester. R. E.. Quine. D. E. C., J . Dairy Res., 44, 125 (1977). (42F) Huyghebaert, A.. Hendrickx, H., Actes Congr. Mond.-Soc. Int. Etude Corps Gras. 73th, Section E , 1 (1976); Chem. Abstr., 87, 199246) (1977). (43F) Iverson, J. L , Sheppard, A . J.. J . Assoc. Off. Anal. Chem.. 60, 284 (1977). (44F) Johnston, A. E., Dutton, N. J., Scholfield, C. R.. Butterfield, R. O., J . Am. Oii Chem. Soc., 55, 486 (1978). 145F) Kaooulas. V . M.. Mastronicolis, S. K . , Galanos. D. S.. Z . Lebensn7.Unters'.-Forsch.,163, 96 (1977). (46Fl Katleskind, A., Valmlle, G.. Midler, O., Blanc, M., Analusis. 5, 79 (1977); Anal. Absfr.. 34, 4F46 (1978) (47F) Kornan. V.. Kotuc. J., J . Am. Oil. Chem. SOC.,5 5 , 563 11976). (48F) Ibid 54, 95 (1977) (49F) Koman, V Kotuc. J , Cslcsayova, M J Am Oil Cheni Soc , 55, 629 119781 (50F)-Koops, J., Klornp, H.. Neth. Milk Dairy J , , 31, 56 (1977); Chem. Abstr., 87, 37459d (1977). (51F) Madison. B. L., Hill, R. C . , J . A m . O i Chem. SOC..55, 328 (1978). (52F) Marszall, i..Cosmet. To/letries, 92, 32 (1977). (53F) McCreary, D. K., Kossa, W. C., Rarnachandran. S..Kurtz, R. R., J . Chromatogr. Sci , 16, 329 (1978). (54F) Miles. C. A.. Fursey. G. A. J.. Food Chem 2, 107 (1977). (55F;) Morin. R. J,, Clin. Chim. Acta, 71. 75 (1976) (56F) Murata, T., Anal. Chem., 49, 2209 (1977). (57F) Ibid.. J . Lipid Res.. 19, 166 (1978). (58F) Murthy, M. K. H., Bhat, G. S., J . A m . OilChem. SOC..53. 577 (1976). (59F) Nielsen. L. V., Milchwissenschaff, 31, 598 (1976); Chsm. Abstr., 86, 41898t (1977). \ . -

ANALYTICAL CHEMISTRY, VOL. 51, NO. 5, APRIL 1979 (60F) Ottenstein, D. M., Wittings, L. A,, Walker, G., Mahadevan, V., Pelick, N., J . A m . Oil Chem. S o c . , 54, 207 (1977). (61F) Perkins, E. G., McCarthy, T. P., O'Brien, M. A.. Kummerow, F. A,, J . A m . Oil Chem. Soc., 54, 279 (1977). (62F) Perkins, E. G., Means, J. C., Picciano, M. F., Rev. f r . Corps Gras. 24, 73 (1977). (63F) Pfeffer. P. E., Luddy. F. E.. Unruh. J., Schooiery, J. N., J , A m . OilChem. Soc..54, 380 (1977). (64F) Pfeffer, P. E.. SamDuana. . - J.. Schwartz, D. P.. Shoolerv. J. N., Lioids. 12, 869 (1977). (65F) Porter, N. A., Nixon, J., Isaac, R., Blochim. Biophys. Acta, 441, 506 (1976): Anal. Abstr., 33, 4D66 (1977). (66F) Rainey, M. L., Purdy, W. C., Anal. Chlm. Acta, 93, 211 (1977). (67F) Richter, H., Srey, C., Winter, K.. Fuerst. W.. Plwrmazie. 32. 164 (19771: Anal. Abstr.. 33, 4D68 (1977). (68F) Rutar, V., Burgar, M., 'Blinc, R., Ehrenberg, L., J . Magn. Reson., 27, 83 (1977); C h e m . Abstr., 87, 116483k (1977). (69F) Sano, H., Yamazaki, M., Agric. B i d . C h e m . , 40, 2485 (1976); Chem. Abstr.. 86. 702000 11977). (70F)~Scrimgeou~ C.7M,, , J . ' A m . Oil C h e m . Soc., 54, 210 (1977). (71F) Sheppard, A. J., Newkirk, D. R., Hubbard, W. D., Osgood, T., J . Assoc. O f f . Anal. C h e m . , 60, 1302 (1977). (72F) Shoolery, J. N., Prog. Nucl. Magn. Reson. Spectrosc., Part 2, 11, 79 (1977); Anal. Abstr., 34, 6J92 (1978). (73F) Smoczkiewiczowa, A., Wienskowski, K., Zalewski, R., Chem. Anal. ( W a r s a w ) , 21, 891 (1976): Chem. Abstr., 86, 153742 (1977). (74F) Spencer, G. F., Plattner. R . D., Miwa, T., J . A m . O i l C h e m . Soc., 54, 187 (1977). (75F) Stahl, E., Werndorff, F., Fette, Seifen, Anstrichm., 78, 395 (1976). (76F) Stetina, B., Luck, H., S. Afr. J . Dairy Technoi., 8 , 111 (1976); Chem. Abstr., 88, 35920u (1978). (77F) Suhren, G., Heeschen, W., Tolle, A,, Milchwissenschaff, 32, 641 (1977); Chem. Abstr., 88, 35949k (1978). (78F) Sweeney. J. P., Weihrauch, J. L.. Crit. Rev. FoodSci. Nutr.. 8. 131 (1977); Anal. Abstr., 33, 4F7 (1977). (79F) Takagi, T., Itabashi, Y., J . Chromatogr. Sci., 15, 121 (1977). (80F) Ibid.. Lipids, 12, 1062 (1977). (81F) Tamura, T., Maruyama, T., Isoda, Y., Sato, S., Suzuki, K., Murui, T., Yonevama, S.. Watanabe. M.. Yukaaaku. 25. 853 (1976): Chem. Abstr.. 86, 70185p (1977) (82F) Tanaka, M , Itoh, T., Kaneko, H., ibid., p 263; Anal Abstr , 32, 3D91 11977), (83F) Tiscornia, E., Camurati, F., Gastaldo, P., Pagano, M.. Riv. Ita/. Sostanze Grasse, 53, 119 (1976); Anal. Abstr.. 31, 5F43 (1976). (84F) Totani, N., Totani, Y., Matsuo, N., J , Am. OilChem. Soc., 54, 403 (1977). (85F) Trumbetas, J., Fioriti, J. A., Sims, R. J., ibid.. 53. 722 (1976). (86F) Ibld., 54, 433 (1977). (87F) Tsoukalas, B., Grosch, W., ibid., p 490. (88F) Tur'yan, Y. I., Malyshev, A. M., Vyskubova, N. K., I z v . Vyssh. Ucheb. Zaved., Pishch. Teknol., 1, 139 (1976); Anal. Abstr., 31, 6F29 (1976). (89F) Urakami, C., Doi, H., Toriyama, S., Asano, Y., Oka, S., Yukagaku, 25, 764 (1976); Chem. Abstr., 86, 41919a (1977). @OF) Wada, S.,Koizumi, C., Nonaka, J., ibid., 26, 95 (1977); Chem. Abstr., 86, 138063e (1977). (91F) Welch, R . W., J . Sci. Food Agric., 28, 635 (1977). (92F) Zuercher. K., Hadorn, H., Strack, C., Dtsch. Lebensm.-Rundsch., 72, 345 (1976).

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Flavors and Volatlle Compounds (1G) Aishima, T., Nobuhara, A., Agric. B i d . Chem., 40, 2159 (1976); Chem. Abstr., 86, 28540a (1977). (2G) Ibid., Food C h e m . , 2, 161 (1977). (3G) Anders, U., Tittgemeier, F., Hailer, G.. Z. Lebensm.-Unters.-Forsch,, 162, 21 (1976). (4G) Andrews, S. J., Ponce, C. G., Mendenhall, V. I., J . Food Sci., 42, 1168 (1977). (5G) Barcelo, C.. Gassiot, M., Ferrer, M., J . Chromatogr., 147, 463 (1978). (6G)Barnett. J. H., Einsmann, J. R., J. Assoc. Off. Anal. Chem., 60, 297 (1977). (7G) Bigalii, G., J , A m . Oil Chem. S O C . ,54, 229 (1977). (8G) Blakesley, C. N., Loots, J.. J . Agric. Food Chem., 25, 961 (1977). (9G) Bories, G. F., Tulliez, J. E., J . Sci. Food Agrlc., 28, 996 (1977). (10G) Braun, G., Hiecke, E., Dtsch. Lebensm.-Rundsch., 72, 393 (1976). (11G) Ibid., 73, 273 (1977). (12G) Bullard, R . W., Holguin, G., J . Agric. food Chem., 25, 99 (1977). (13G) Buttery, R. G., Guadagni, D. G., Ling, L. C., ibid., 26, 791 (1978). (14G) Calabro, G., Curro, P., Essenze, 46, 215 (1976); Anal. Abstr., 32, 5F24 119771. (15'Gj Calapaj, R., Ciraolo, L., ibld., p 224; Anal. Abstr., 32, 5F25 (1977). (16G) Cant. P. A. E., Walker, N. J., J . Chromatogr.. 130, 267 (1977). (17G) Caporaso, F.. Sink, J. D.. Dimick. P. S.. Mussinan.. C. J... Sanderson. A,. J . Agric. f o o d C h e m . , 25, 1230 (1977). (18G) Carballido Estevez, A., Valdehita di Vicente, M. T., A n . Bromat., 27, 357 (1975); Anal. Abstr.. 31, 6F27 (1976). (19G) Cattell, D. J.. Nursten, H. E . , Phflochemistry, 15, 1967 (1976); Chem. Abstr., 87, 375711 (1977). (20G) Chang, S. S.,Peterson, R. J., J . Food Sci., 42, 298 (1977). (21G) Chang, S. S., Vallese, F. M., Hwang, L. S., Hsieh, 0. A. L., Min, D. B. S., J . Agric. Food Chem., 25, 450 (1977). (22G) Charalambous, G., Bruckner, K. J., Hardwick, W. A,, Weatherby, T. J.. J . Tech. Quart. MasterBrew. Assoc. A m . , 12, 203 (1975); Anal. Abstr., 32, 1F36 (1977). (23G) Chrk, J.. Dewan, R., Locksley, H. D., Maynard, R.. J . Chromatogr.. 134, 315 (1977). (24G) Cwradi, C., Micheli, G.. Boll. C h h . Unione Ita/. Lab. Prov., 3, 123 (1977); C h e m . Abstr., 88. 35922w (1978). (25G) Crosgrove, D. M., J . Food Sci.. 43, 641 (1978).

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(26G) Devani, M. E., Shishoo, C. J., Dadia, B. K., Mody, H. J., J . Assoc. Off. Anal. C h e m . , 61, 167 (1978). (27G) Dima, F . , Ghimicescu, G., Ann. Falsif. Expert. Chim.. 70, 35 (1977); Anal. Abstr., 34, 1F48 (1978). (28G) Dirinck, P., Schreyen, L., Schamp, N., J . Agric. FoodChem., 25, 759 (1977). (29G) Orawert, F., Schreier, P., Leupold, G., Kerenyi, Z.,Lessing, V., Junker, A., 2. Lebensm.-Unters.-Forsch.. 162, 11 (1976). (30G) Dumont, J. P., Roger, S., Adda, J., Lait, 56, 595 (1976); Chem. Abstr., 86, 70279x (1977). (31G) Dupuy, H. P., Rayner, E. T., Wadsworth, J. I., Legendre, M. G., J . A m . Oil Chem. S o c . 54, 445 (1977). (32G) Faulkner, S. V., Process Biochem., 5 , 47 (1976); Anal. Abstr.. 32, 4F50 (1977). (33G) Fisher, J. F., J . Agric. food C h e m . , 26, 497 (1978). (34G) Flath, R. A., Forrey, R . R.. ibid., 25, 103 (1977). (35G) Frattini, C., Bicchi, C., Barettini, C., Nano, G. M., ibid., p 1238. (36G) Frischkorn, C. G. B., Frischkorn, H. E., Z . Lebensm.-Unters.-Forsch,, 182, 273 (1976). (37G) Galetto, W. G., Walger, D. E., Levy, S. M., J . Assoc. Off. Anal. Chem., 59, 951 (1976). (38G) Glasl. H., Borup-Grochtmann, I.,Wagner, H.. Dtsch. Apoth. Ztg., 118, 1639 (1976): Anal. Abstr., 32, 5F23 (1977). (39G) G-igsby, J. H., Pahmand, S. R., J. Am. Soc. Brew. Chem.. 35, 43 (1977); Anal. Abstr., 33, 6F72 (1977). (40G) Grushka, E., Kapral, P., Sep. Sci., 12, 415 (1977). (41G) Hara, T.. Kubota, E., C k g y o Giju?su Kenkyu, 50, 68 (1976): Chem. Abstr., 86, 119445q (1977). (42G) Hirayama, S., Imai, C., J . A m . Oil C h e m . Soc., 54, 190 (1977). (43G) Hoeffler, A. C., Coggon. P., J . Chromatogr.. 129, 460 (1976). (44G) Jackson, H. W., Giacherio, D. J., J. A m . OilChem. Soc., 54, 458 (1977). (45G) Jamieson. A. M.. van Gheluwe. G., A m . Soc. Brew. Chem. J . , 35, 73 (1977); Anal. Abstr., 34, 5F35 (1978). (46G) Jones, R. A., Neaie, M. E., Ridlington. J., J. Chromatogr., 130, 368 (1977). (47G) Kan, T., Kamata, K., Mori, K.. Nakamura, Y.. Ueta. T.. Totani. T., Tokyo-toritsu€isel Kenkyushc Kenkyu Nempo, 27, 106 (1976); Anal. Abstr., 34, 1F36 (1978). (48G) Kamata, K.. Kan, T., Yamanobe, H., Mizuishi, K., Yamazoe. R.. Totani, T., ibid.. p 112; Anal. Abstr., 34, 1F37 (1978). (49G) Kawabata, M.. Ohtsuki, K., Kokura, H., Wakahara, Y., Agric. Biol. Chem., 41, 2285 (1977). (50G) Kaufmann, G., Ritter, F., Schubert, K., J. Steroi3 Biochem., 7, 593 (1976); Anal. Abstr., 32, 30104 (1977). (51G) Klimes, I., Lamparsky. D.. Intl. Flavors Food Addit.. 7 , 272 (1976). (52G) Knee, M.. Hatfield, S. G. S., J . Food Technol., 11, 485 (1976). (53G) Koehler, M., Hoehn, M., Chromatographia, 9, 611 (1976); Anal. Abstr., 33, 1C8 (1977). (54G) Kojima, M., J. Ferment. Technol., Osaka, 54, 120 (1976); Anal. Abstr., 32, 1F39 (1977). (55G) Korany, M. A., Abdel-Salam, N., Abdel-Salam, M., J . Assoc. Off. Anal. C h e m . , 81, 169 (1978). (56G) Kozma-Kovacs, E., Kevei-Pichler, E., Lendvai, I . , Acta Aliment. Acad. Sci. Hung.. 6 , 1 (1977): Anal. Abstr., 34, 4F26 (1978). (57G) Lerke. P. A., Huck, R . W., J . food Sci.. 42, 755 (1977). (58G) Lund, E. D., Bryan, W. L., ibid., p 385. (59G) MacLeod, G., Coppock, B. M., J . Agric. food C h e m . . 25, 113 (1977). (60G) McKeag, R. G., Hougen, F. W.. ibid., p 417. (61G) Meili, M.. Chaveron, H., Ann. Falsif. Expert. Chim., 89, 745 (1976); Anal. Abstr., 34, 1F34 (1978). (62G) Min, D. 8. S., Ina, K., Peterson, R. J.. Chang, S. S.,J . Food Sci.. 42, 503 (1977). (63G) Mosandl, A., 2. Le~ensm.-Unters.-forsch., 163, 255 (1977). (64G) Nelson. R. R., Acree, T. E., Butts, R. M.. J . Agric. Food Chem., 26, 1188 (1978). (65G) Nelson, R. R., Acree, T. E., Lee, C. Y., Butts, R. M., J . Assoc. Off Anal. C h e m . , 59, 1387 (1976). (66G) Obretenov, T., Hadjieva, P., Z . Lebensm.-Unters.-Forsch., 165, 195 (1977). (67G) Opheim, L.-N., Anal. Chim. Acta, 91. 331 (1977). (68G) Orsi, F., €lelmiszervizsgalati Kozl., 22, 23 (1976): Chem. Abstr., 88. 41891k (1977). (69G) Otvos. L., Szep. I., ibid., p 142; Anal. Abstr., 34, 1F53 (1978). (70G) Pankar, D. S., Magar, N. G., J . Chromatogr., 144, 149 (1977). (71G) Parliment, T. H.. Scarpellino. R., J . Agric. FoodChem., 25, 97 (1977). (72G) Piergiovanni, L., Volonterio, G., Riv. Ita/. Sostanze Grasse, 53, 99 (1976); Anal. Abstr., 32, 2F31 (1977). (73G) Guijano-Rico, M., Bautista, R . E., Chaparro, B. F., Zamudio, G. V., Ortiz, P. A . , Von Helden, J., Adv. M a s s . Spectrom. Biochem. M e d 2, 207 (1977); Chem. Abstr., 86, 1 3 8 2 5 6 ~(1977). (74G) Ramos Palacio, J. J., J . Assoc. Off. Anal. C h e m . , 60, 970 (1977). (75G) Roedel, W.. Schroedter, R., Zoell, D., Steiniger, L., Nahrung, 21, 719 ( 1 977). (76G) Rhys Williams, A. T., Slavin, W., J . Agric. Food Chem., 25, 756 (1977). (77G) Schneyder, J., Pluhar, G.. Min. Hoeheren Bundeslehr Versuchsanst. Wein Obstbau, Klosterneuburg, 27, 14 (1977); Anal. Abstr.. 34, 1F49 (1978). Natarajan, C. (78G) Shankaranarayana, M. L., Raghavan, B., Abraham, K . O., P., J . 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(84G) Ibid., p 479. (85G) Strukova, V. E., Fal'kovich, Y. E., Tur'yan, Y. L., Grinfel'd, V. I., Lisetskaya. 2. A.. Izv. Vyssh. Uchebn. Zaved., Pishch. Teknol., 170 (1976): Anal. Abstr., 33, 1F43 (1977). (86G) Thomas, E. L., Reineccius, G. A., DeWaard, G. J., Siinkard, M. S., J . Dairv Sci.. 59. 1865 11976). (87G) fhomasow'. J.. Spienge;, U., Wollesen. C., Milchwissenschaft, 31, 334 (1976); Anal. Abstr., 32, 4F39 (1977). (88G) Todd, P. H., Jr., Bensinger, M. G.. Biftu, T., J . FoodSci., 42, 660 (1977). (89G) Tressl, R., Bahri, D., Holzer, M., Kossa, T., J . Agric. FoodChem., 25, 459 (1977). (90G) Tressl, R., Renner, R., Apetz, M., Z.Lebensm.-Unters.-Forsch., 162, 115 (1976). (91G) Tressl, R., Kossa, T., Renner. R., Koeppler, H., ibid., p 123. (92G) Waking, A. E., Zmachinski, H., J . A m . Oil Chem. SOC.,54, 454 (1977). (93G) Warner, J. S., Anal. Chem., 48, 578 (1976). (94G) Williams, P. J., Strauss, C. R., J . Inst. Brew., London, 83, 213 (1977): Anal. Abstr., 34, 2F51 (1978). (95G) Yamashita, I., Iino, K., Nemoto, Y., Yoshikawa. S..J. Agric. FoodChem., 25, 1165 (1977).

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132R


(8L) Castino, M., Di Stefano, R., Riv. Viticott. Enol.. 29, 290 (1976); Anal. Abstr., 33, 6F77 (1977). (9L) Ciha, A. J., Brenner, M. L., Brun, W. A., Plant Physiol., 59, 821 (1977); Anal. Abstr., 34, 3G12 (1978). (1OL) Donhauser, S.,Brauwissenschaft, 30, 325 (1977); Anal. Abstr., 34, 5F33 ( 1978). (11L) Drawert. F.. Lessing, V.. Leupold, G., Chromatographia, 9, 373 (1976); Anal. Abstr., 32, 2F48 (1977). (12L) Ibid., Chem. Mikrobiol. Technd. Lebensm., 5, 65 (1977); Anal. Abstr., 34, 5F37 (1978). (13L) Drawert, F., Leupold, G., Chromatograph&, 9, 397 (1976); Anal. Abstr., 32, 2F9 (1977). (14L) Ibid.. p 605; Anal. Abstr., 33, 1F40 (1977). (15L) Drawert, F., Leupoid, G., Lessing. V., Brauwissenschaft, 29, 345 (1976); Anal. Abstr., 32, 5F36 (1977). (16L) Ibid., 30, 13 (1977); Anal. Abstr., 33, 2F44 (1977). (17L) Duering, H., Experlentla, 33, 1666 (1977); Anal. Abstr., 34, 6F26 (1978). (18L) Durkee, A. B., J . Agric. Food Chem., 25, 286 (1977). (19L) Eskin, N. A. M., Hoehn, E., Frenkel, C., ibid., 26, 973 (1978). (20L) Esterbauer, H., Schauenstein, E., Z . Lebensm.-Unters.-Forsch., 164, 255 (1977). (21L) Farkas, J., Polonsky, J.. Kvasny Prum., 23, 16 (1977); Anal. Abstr., 34, 2F52 (1978). (22L) Felice. L. J., King, W. P.. Kissinger, P. T., J . Agric. Food Chem., 24, 380 (1976). (23L) Hanefeld, M., Herrmann, K., Msch. Lebensm.-Rundsch., 72, 383 (1976); Anal. Abstr., 32. 6F26 (1976). (24L) Harland, 8. F.. Oberleas, D., Cereal Chem., 54, 827 (1977). (25L) Hoff, J. E., Singleton, K. I . , J . Food Sci., 42, 1566 (1977). (26L) Kanbe, C., Ozawa, Y., Sakasai, T., Agric. Biol. Chem., 41, 863 (1977). (27L) Kasai, Y., Tanimura, T., Tamura. Z.,Ozawa, Y., Anal. Chem., 49, 655 (1977). (28L) Kenyhercz, T. M., Kissinger, P. T., J . Agric. FoodChem., 25, 959 (1977). (29L) Kieninger, H., Boeck, D., Brauwissenschaft, 30, 357 (1977); Anal. Abstr., 34, 6F36 (1978). (30L) List, D. M., Askar, A., Dtsch. Le6ensm.-Rundsch., 72, 389 (1976). (31L) Marsili, R. T., J . Food Sci., 42, 52 (1977). (32L) McCioskey, L. P.. J . Agric. Food Chem., 24, 523 (1976). (33L) Nakabayashi, T.. Mano, S., Nippon Shokuhin Kogyo Gakkaishi, 22, 545 (1975); Anal. Abstr., 32, 3F26 (1977). (34L) Nakajima, M.. Ozawa, Y., Tanimura. T., Tamura, Z.,J . Chromatogr., 123, 129 (1976). (35L) Nose, N., Hoshino, Y., Suzuki, T., Kikuchi, Y., Watanabe, A,, Shokuhin Eiseigaku Zasshi, 17, 290 (1976); Chem. Abstr., 86, 3639b (1977). (36L) Pease, H. L., Prince, J. L., Johnston, E. F., J . Agric. Food Chem.. 26, 331 (1978). (37L) Pilone, G. J., A m . J . Enol. Viticult., 28, 104 (1977); Anal. Abstr., 35, 2F43 (1978). (38L) Price, M. L.. Butler, L. G., J . Agric. Food Chem., 25, 1268 (1977). (39L) Roberts. E. J., Godshail. M. A., Int. Swar J . . 80, 10 (1978); Anal. Abstr., 35, 1F4 (1978). (40L) Sachse, J., 2 . Lebensm.-Unters.-Forsch., 166, 153 (1978). (41L) Siebert, K. J., J . Am. SOC.Brew. Chem., 34, 79 (1976); Anal. Abstr.. 32. 4F49 (1977). (42Lj'Siinkard, K., Singleton, V. L., Am. J . Enol. Viticult., 28, 49 (1977); Anal. Abstr.. 34, 4F41 (1978). (43L) Slotema, F. P., Verhagen, L. C.. Verzele. M., Brauwissenschaft. 30, 145 (1977); Anal. Abstr., 3 3 6F64 (1977). (44L) Suhren, G.. Heeschen, W., Tolle, A., Milchwissenschaft, 32, 709 (1977); Chem. Abstr., 88, 87725d (1978). (45L) Tanaka. A,. Tanabe, K., Kato, A., Muramatsu, J.. Yukagaku. 26, 119 (1977); Chem. Abstr., 86, 1380641 (1977). (46L) Terweij-Groen, C. P., Kraak, J. C., J . Chromatogr., 138, 245 (1977).

Nltrogen ( I M ) Adams, R. F., Schmidt, G., Slavin, W., Chromatogr. News/.,4, 10 (1976); Chem. Abstr., 87. 166119s (1977). (2M) Amaya-Farfan, J., Young, C. T., Chichester, C. O., J . Agric. FoodChem., 25, 139 (1977). (3M) Amico, V., Oriente, G., Tringaii, C., J . Chromatogr., 131, 233 (1977). (4M) Amorim, H. V., Basso, L. C., Crocomo, 0. J., Teixeira, A. A , , J . Agric. Food Chem., 25, 957 (1977). (5M) Anabsis Committee of the European Brewery Convention. Erauwissenschaft. 29, 231 (1976); Anal. Abstr., 32, 3F27 (1977). (6M) Asao, T., Anal. Biochem., 77, 321 (1977). (7M) Attina, M., Ciranni. G., Farmaco, Ed. Prat., 31, 650 (1976); Anal. Abstr., 33, 1F36 (1977). (EM) Basha, S. M. M., Roberts, R. M., Anal. Blochem., 77, 378 (1977). (9M) Beitz, D. C., Phillips, M. E., Eklund, S.H., J . Dairy Sci., 6 0 , 701 (1977). (10M) Bennett, M. C., J . Agric. Food Chem., 25, 219 (1977). (11M) Bosset, J. O., Blanc, 6.. Phttner, E., Mitt. Geb. Lebensminelunters. w g . , 67, 226 (1976); Anal. Abstr., 31, 5F10 (1976). (12M) Boudier, J. F., Luquet. F. M.. Vincent, M., Ind. Aliment. Agric., 94, 945 (1977); Chem. Abstr., 88, 49084m (1978). (13M) Burba, M., George, B., Z . Zuckerind.. 100, 667 (1975); Anal. Abstr., 32. 3G5 (1977). (14M) Calandra, F., Riv. Ital. Sostanze Grasse, 54, 161 (1977); Anal. Abstr., 33, 5G10 (1977). (15M) Catsimpoohs, N., FoodProteins, 106 (1977); Chem. Abstr., 87, 1660682 11977). (ISM) Chang, S. H., Gooding, K. M., Regnier, F. E., J . Chromatogr., 125, 103 (1976). (17M) Chang, S. H., Noel, R . , Regnier, F. E., Anal. Chem., 48, 1839 (1977). (18M) Creamer. L. K., Matheson, A. R., N . Z . J . DairySci. Techno/., 11, 211 (1976); Anal. Abstr., 33, 6D93 (1977). (19M) Cresser, M. S., Anal. Chim. Acta, 85, 253 (1976).

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(58M) Hunziker, H. R., Miserez, A.. Mitt. Geb. Lebensmiffelunters. Hyg., 68. 267 (1977); Anal. Abstr., 33, 6F63 (1977). (59M) Jozefowicz, M. L., O'Neill, I . K., Prosser, H. J., Anal. Chem., 49, 1140

,.

11n77i ,nu, I

(60M) Kaui, A. K., Sharma. T. R., Fresenius' Z . Anal. Chem.. 280, 133 (1976); Anal. Abstr., 31, 6G2 (1976). (61M) Kawabata, T., Ohshima, H.. Ishibashi, T., Matsui, M., Kitsuwa. T., J . Chromatogr., 140, 47 (1977). (62M) Khan. A. W., Cowen, D. C., J . Agric. Food Chem., 25, 236 (1977). (63M) Kidani, Y., Uno, S.,Inagaki, K.. BunsekiKagaku, 26, 158 (1977); Anal. Abstr., 33, 3D143 (1977). (64M) Kinoshita, T., Iinuma, P., Atsumi, K., Tsuji, A,, Anal. Biochem., 77, 471 (1977). (65M) de Koning, P. J., van Rooijen, P. J., Draaisma. J. T. M.. Milchwissenschaft, 31, 261 (1976); Anal. Abstr., 32, 2F24 (1977). (66M) Kreutzer, H., GITFachz. Lab., 21, 1163 (1977); Anal. Abstr., 34, 6C9 (1978). (67M) Krutzsch, H. C., Pisano. J. J., Biochem., 17, 2791 (1978). (68M) Kubadinow. N., Roesner, G., Sucr. Belge, 96, 9 (1977); Anal. Abstr., 34 1F20 (1978). (69M) Landman, A. D., Int. J . Vitamin Nutr. Res., 46, 310 (1976); Anal. Abstr., 33, 4E24 (1977). (70M) Lebedev, A. V., Neudachin. V. P., Zima. V. G., Ryadchikov, V. B., Sci. Tools, 23, 22 (1976); Anal. Abstr., 31, 6D112 (1976). (71M) Leske. B., Konrad, G., Nahrung, 21, 925 (1977); Anal. Abstr., 35, 2D129 (1978). (72M) Lipton, S. H., Bodweli, C. E., J . Agric. FoodChem., 25, 1214 (1977). (73M) Lund, E., Thomsen, J., Brunfeldt, K., J . Chromatogr., 130, 51 (1977). (74M) McCausiand, J., Wrigley, C. W.. J , Sci. Food Agr., 27, 1203 (1976). (75M) MacKenzie, S. L., J . Chromatogr.. 130, 399 (1977). (76M) Madarassy-Mersich, E., PetwTurza, M., Szarfold+Szaima, I., Acta Aliment., 7, 195 (1978). (77M) Madison, B. L., Kozarek, W. J., Danw, C. P., J . Assoc. Off. Anal. Chern., 59, 1258 (1976).

ANALYTICAL CHEMISTRY, VOL. 51, NO. 5, APRIL 1979 (78M) Makinde, M. A., Markley. R. A., Lachance, P. A,. Nutr. Rep. Inf., 15, 95 (1977); Anal. Abstr., 35, 1F7 (1978). (79M) Malingre, T. M., Batterman, S., Pharm. Weekbl., 112, 1305 (1977); Anal. Abstr.. 34. 6E19 (1978). f80MI~Manlev.C H..'J. Assoc. Pub. Anal.. 14. 29 (1976): Anal. Abstr.. 32. . 2Gl6 (1977) l R l M I Masters, R G., Leyden, D E., Anal. C h m . Acta, 98, 9 (1978) $2Mj Mattoo, B. N., Pai, P. P., Krishnamurthy. R , Indian J . Chem., Sect A . 15, 141 (1977); Anal. Abstr., 34, 2 E l l (1978). f83MI Medina, M. B... Klevn. D. H.. Swallow. W. H.. J . Am Oil Chem. SOC.. ' 53, 555 (1976). (84M) Miller, B. S., Pomeranz, Y., Thompson, W. O., Nolan, T. W., Hughes, J. W., Davis, G., Jackson, N. G., Fulk, D. W., CerealFoods World, 23, 198 (1978). (85M) Moeller, A. B., Andrews, A. T., Cheeseman, G. C., J . Dairy Res., 44, 277 (1977). (86M) Mrowetz, G., Kiostermeyer. H., Milschwlssenscha/t 32, 9 (1977); Chem. Abstr., 86, 87780b (1977). 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(4N) Defibaugh, P W.. Smith. J. S., Weeks, C. E., ibid., p 522. (5N) De Leenheer. A. P., Cruyl, A. A M., J. Chromatogr. Sci., 14, 434 (1976). (6N) Dennison, D. B., Kirk, J. R., J. Food Sci., 42, 1376 (1977). (7N) Egberg, D. C., Potter, R. H., Heroff, J. C., J. Assoc. O f f . Anal. Chem., 60, 126 (1977). (EN) Ibid.. 25, 1127 (1977). (9N) Fiedlerova. V., Davldek, J., Z.Lebensm.-Unters.-Forsch,, 166, 93 (1978). (10N) Frouin, A., Tacquet, A., Beerens, H., Roussin, D., Poncelet, F., Roll, N., Ann. Fakif. Expert. Chim., 68, 173 (1975); Cbem. Abstr., 86. 41875h (1977). (11N) Gebhardt, S. E., Elkins, E. R., Humphrey, J., J . Agric. FoodChem., 25, 629 (1977). (12N) Gmzalez Garcia-Gutierrez, A.. Ion(Madrid),38, 653 (1976); Anal. Absfr.. 34, 3E28 (1978). (13N) Gregory, J. F., 111. Kirk, J. R., J. Agric. Food Chem.. 26, 338 (1978). (14N) Gregory, J. F., Kirk, J. R., J. Food Sci., 42, 1073 (1977). (15N) Hammam, A. S., J . Appl. Chem. Biotechnol., 26, 611 (1976); Anal. Abstr., 32, 5F46 (1977). 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(7P) Dickes, G. J., Nicholas, P. V.. "Gas Chromatography in Food Analysis", Butterworths, London, 1976. (8P) Dols, T. J., Armbrecht. B. H., J. Assoc. Off. Anal. Chem., 59, 1204 (1976). (9P) F o b , A. K., Yeransian, J. A., Sloman, K. G., Anal. Chem.,49, 194R (1977). (1OP) Froede, W. D., Brauwissenschaft, 30, 52 (1977); Anal. Abstr., 33, 3F43 (1977). (1 1P) Gajzago, I., Vamos-Vigyazo, L., Proc. Hung. Annu. Meet. Biochem., 15, 67 (1975); Chem. Abstr., 88. 61184b (1978). (12P) Herrmann, K.. 2. Lebensrn.-Unters.-Forsch.,165, 87 (1977). (13P) Horwitz. W., J . Assoc. Off. Anal. C h e m . , 59, 1197 (1976). (14P) Kafka, K. J., Norris, K. H., Acta Aliment. Acad. Sci. Hung., 5, 267 (1976); Anal. Abstr., 34, 1F45 (1978). (15P) Karger, B. L.. J . Chromatogr. Sci., 45, 575 (1977). (16P) King, R. D., Ed., "Developments in Food Analysis Techniques-1", Applied Science Publishing Ltd., Essex, England, 1978. (17P) Lees, R., "Food Analysis: Analytical and Quality Control Methods For The Food Manufacturer and Buyer", 3rd ed., Leonard Hill Books, London, 1976.

(18P) Mendenhall, G. D., Angew. Chem., Int. Ed. Engl.. 16, 225 (1977): Anal. Abstr., 33, 4J76 (1977). (19P) Moll, M., Flayeux, R., Leheude, J.-M., Bios, France, 7 , 3 (1976); Anal. Abstr., 32, 6F35 (1976). (20P) Noble, A. C., Food Techno/., Chicago, 29, 56 (1975). (21P) Pearson, D., "The Chemical Analysis of Foods", 7th ed., Churchill Livingstone, Edinburgh, 1976. (22P) Pomeranz, Y., Meloan, C. E., "Food Analysis: Theory and Practice", rev. ed., AVI Publishing Company, Westport, Conn., 1978. (23P) "Proceedings of the Seventh International Colloquium on the Chemistry of Coffee, Hamburg, W. Germany, 1975", Association Scientifique Internationale du Cafe, Paris, 1976; Anal. Abstr.. 32, SA1 (1977). (24P) Ranganna, S., "Manual of Analysis of Fruit and Vegetable Products", Tata McGraw-Hill Publishing Co. Ltd., New Delhi, India, 1977. (25P) Ruzicka, J., Hansen, E. H., Anal. Chirn. Acta, 99, 37 (1978). (26P) Uriano, G. A., Gravatt, C. C., Crit. Rev. Anal. Chern., 6 , 361 (1977); Anal. Abstr.. 34, 5A6 (1978). (27P) Watson, C. A., Anal. C h e m . , 49, 835A (1977).

Food - Analytical Chemistry (ACS Publications)

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