Gas-liquid chromatographic determination of monosodium glutamate in soups and soup bases.

A method is given for determining monosodium glutamate (MSG) in soups and soup bases by gas-liquid chromatography (GLC) of the trimethylsilyl ether derivative of glutamic acid. This method compared favorably with existing methods including GLC of the trifluoroacetate (TFA)/butyl ester derivative, and analysis on an amino acid analyzer. In addition, some samples were analyzed by GLC/mass spectrometry. The MSG content of various products ranged from approximately 0.2% in some condensed soups to 13.1% on bouillon cubes. The method, which can detect as little as 0.05%, requires only a 10 min single step derivatization at room temperature and is preferred to the TFA/butyl ester technique.     

Fast, short-column separation and fluorometric determination of monosodium glutamate in foods.

In a simple and fast procedure, monosodium glutamate in food products is first separated by a short ion exchange column and subsequently determined fluorometrically with fluorescamine. An average recovery of 90.8% with a standard deviation of plus or minus 6.67% was obtained for added monosodium glutamate in a series of 8 products. As little as 0.05% monosodium glutamate can be determined. The method is faster than the official method and saves 5 hr/determination.     

Simplified cleanup and gas chromatographic determination of organophosphorus pesticides in crops

A simple and efficient cleanup method for gas chromatographic determination of 23 organophosphorus pesticides in crops including onion is described. The sample was extracted with acetone. The extract was purified with coagulating solution, which contained ammonium chloride and phosphoric acid, and then filtered by suction. The filtrate was diluted with NaCl solution and reextracted with benzene. The organic layer was evaporated and injected into a gas chromatograph equipped with a flame photometric detector (FPD) and fused silica capillary columns (0.53 mm id) coated with silicone equivalent to OV-1701, OV-1, and SE-52. Onion extract, which contained FPD interferences, was cleaned up on a disposable silica cartridge. Recoveries of most organophosphorus pesticides from spiked crops: mandarin orange, tomato, spinach, sweet pepper, broccoli, lettuce, and onion at levels of 0.02-0.28 ppm, exceeded 80%, but the water-soluble pesticides dichlorvos and dimethoate gave poor recoveries in all crops; the nonpolar pesticides disulfoton, chlorpyrifos, fenthion, prothiophos, and leptophos were not recovered quantitatively in spinach, sweet pepper, broccoli, and lettuce. IBP, edifenphos, phosmet, and pyridaphenthion were not recovered from onion because of adsorption to the silica cartridge. The detection limits ranged from 1.25 to 17.5 ppb on a crop basis.     

Improved cleanup for gas chromatographic determination of propiconazole residues in soil, wheat grain, straw, and leaves

A simple and sensitive method is described for determination of propiconazole, a new type of broad-spectrum systemic fungicide, in soil, wheat grain, straw, and leaves. Pesticide residues in or on grain and green plant materials are extracted with methanol (or a mixture of methanol and water (4 + 1), for soil), partitioned into methylene chloride, and cleaned up on an alumina column for grain and soil or an activated charcoal column for green plant materials. The amount of residue is quantitatively measured by gas chromatography using an alkali flame ionization detector in the nitrogen-sensitive mode. Recoveries from soil, grain, and green plant materials fortified at 0.1-5 mg/kg are better than 80%. The practical detection limits of this method are 0.01 mg/kg in grain and soil and 0.02 mg/kg in green plant materials.     

Improved gas chromatographic method for determination of daminozide by alkaline hydrolysis and 2-nitrobenzaldehyde derivatization and survey results of daminozide in agricultural products

An improved method was developed for the quantitative determination of daminozide. This new method combines the alkaline hydrolysis and distillation steps of the PAM II method for daminozide with the derivatization, cleanup, and gas chromatographic determination steps of the Wright method for unsymmetrical dimethyl hydrazine (UDMH). The minimum detectable level is 0.05 ppm. Recoveries range from 85 to 110% when daminozide is added at 0.1 to 1.0 ppm, and are generally 40% at the 0.05 ppm level. A variety of domestic and imported products were analyzed by this improved method and daminozide was detected in 33 of the 98 samples analyzed. Levels detected ranged from a trace amount to 0.80 ppm. The identity of UDMH hydrazone was confirmed by mass spectrometry in many samples, thus confirming the presence of daminozide. Two samples containing daminozide were analyzed independently by a second laboratory and the findings were closely duplicated.     

Ion chromatographic determination of sulfites in foods

Ion chromatography (IC) is shown to be a promising technique for the determination of sulfites (SO2, SO2/3-) in foods. Results of a 10 min flash distillation and 10 min IC determination compare favorably with the results from the conventional Monier-Williams method for total sulfite in a variety of food matrices. The IC technique also provides a wealth of additional information, such as (1) sulfite and sulfate (oxidized sulfite) content of the spiking or treatment solution, (2) residual sulfite applied to the food after oxidation losses in the treatment process, (3) free sulfite in foods, and (4) total sulfite in foods. As a further check on the Monier-Williams method, the sulfate content of the trapping solution can be determined by IC. Because the IC technique traps the liberated SO2 in a non-oxidizing rather than an oxidizing medium, it is considered free from interfering sulfides and organic sulfur-containing groups which can give false positives in the Monier-Williams method. IC thus offers a high speed, more sensitive, and cost-effective alternative to conventional techniques for the determination of sulfite in foods.     

Gas chromatographic determination of glucono-delta-lactone in foods

A method is described for the gas chromatographic (GC) determination of glucono-delta-lactone in foods. A sample was homogenized with 60-70 degrees C water and filtered. The filtrate was buffered with NH4OH-NH4Cl pH 10 solution, and was passed through a QAE-Sephadex A25 column. The column was washed with water and glucono-delta-lactone was eluted with 0.1N HCl. An aliquot of the eluate was evaporated to dryness and derivatized with pyridine, N,O-bis(trimethylsilyl)trifluoroacetamide, and trimethylchlorosilane at room temperature. GC separation of glucono-delta-lactone as the TMS derivative was performed on a 2% OV-17 column at 180 degrees C. Recoveries from bread, jelly, soybean curd, and other foods fortified with 0.1% glucono-delta-lactone ranged from 92 to 106%, with standard deviations from 2.2 to 9.8%. The detection limit was approximately 0.025%.     

Ion-pair extraction cleanup for liquid chromatographic determination of bentazon in crops and soil

Bentazon was selectively extracted as an ion pair with tetrabutylammonium ion into dichloromethane. This technique was used to clean up crop and soil samples before determination of bentazon by reverse phase liquid chromatography and UV detection. Recoveries from potatoes, cucumbers, wheat grain, and clay soil were 77-103%, with a detection limit of 0.02 mg/kg.     

Gas chromatographic determination of total iodine in foods

A gas chromatographic (GC) method has been developed for determination of total iodine in foods, based on the reaction of iodine with 3-pentanone. Organic matter of a sample is destroyed by an alkaline ashing technique. Iodide in a water extract of the ash residues is oxidized to free iodine by adding dichromate in the presence of sulfuric acid. Liberated iodine is reacted with 3-pentanone to form 2-iodo-3-pentanone, extracted into n-hexane, and then determined by gas chromatography with an electron-capture detector. Recoveries of iodide from spiked food samples ranged from 91.4 to 99.6%. Detection limit for iodine is 0.05 micrograms/g.     

Gas chromatographic determination of oxalic acid in foods

A new quantitative gas chromatographic (GC) method has been developed for the determination of oxalic acid in foods. Solid sample is extracted with water (soluble oxalic acid) or 2N hydrochloric acid (total oxalic acid) at room temperature. An aliquot of sample extract is evaporated to dryness, and the oxalic acid in the residue is methylated with 7% hydrochloric acid-methanol. The reaction mixture is extracted with chloroform, and dimethyl oxalate is quantitated by GC. Recovery of oxalic acid added to liquid samples averaged 100.6%; recoveries from extracts of solid samples were 96.2-99.5 and 97.2-100.1% for water and hydrochloric acid extractions, respectively. Results are shown for determination of oxalic acid in spinach and beverages. The technique is simple, rapid, and accurate, and small samples may be used. The limit of determination is 20 micrograms.     

Simplified cleanup and liquid chromatographic determination of oxamyl residues in potato tubers

A simple and efficient method is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of oxamyl residues in potato tubers. Samples are extracted with methanol, partitioned into dichloromethane, and cleaned up using Sep-Pak Florisil cartridges. LC determination is performed using a Zorbax PSM 60 size exclusion column with an acetonitrile-water (1 + 9) mobile phase and UV detection at 254 nm. Recovery of oxamyl from spiked control tubers averaged 94.1 and 85.9% at fortification levels of 0.4 and 0.08 micrograms oxamyl/g tuber, respectively. The minimum detectable concentration of oxamyl by this method is 0.01 micrograms/g.     

Improved method for determination and identification of serotonin in foods

A previously described method to identify and quantitate serotonin in foods has been improved. The extraction and separation of serotonin from interfering substances has been improved, and the scope of material to which the method may be applied has been widened. The relative standard deviation (RSD) for repeated determinations of serotonin in canned fried tomato purée and the average recovery of serotonin added to the same sample was 6.25 and 89.9%, respectively. The method showed the presence of serotonin in apricots, cherries, and peaches.     

Gas chromatographic determination of electron capture sensitive volatile industrial chemical residues in foods, using AOAC pesticide multiresidue extraction and cleanup procedures

Electron capture (EC) gas chromatographic (GC) parameters have been developed for determining some of the more volatile industrial chemicals that can be determined by the AOAC multiresidue method for organochlorine and organophosphorus pesticides with modified GC operating conditions. Retention times relative to pentachlorobenzene are reported for 143 industrial chemicals, pesticides, and related compounds on OV-101 GC columns at 130 degrees C. Also reported for most of the compounds are recoveries from fortified samples carried through the AOAC extraction and cleanup procedures for fatty and/or nonfatty foods, Florisil elution characteristics, and GC relative retention times on mixed OV-101 + OV-210 columns at 130 degrees C. Our laboratory has used the modified EC/GC parameters with the AOAC multiresidue extraction/cleanup procedures to determine many volatile halogenated industrial chemical contaminants in foods, chiefly in samples of fresh-water fish. Other modifications of the AOAC method are described to improve the tentative identification and quantitative measurement of these volatile residues.     

Ion-pairing liquid chromatographic determination of benzimidazole fungicides in foods

A method is described for determining residues in foods of thiabendazole, thiophanate methyl, the di-oxygen analogue metabolite [dimethyl 4,4'-O-phenylene bis (allophanate)] that is the metabolite name of the latter, and methyl-2-benzimidazole carbamate, which is the major metabolite and fungitoxic principle common to both thiophanate methyl and benomyl. The residues are extracted from the product using methanol and are partitioned into dichloromethane after initial acidification and again after subsequent alkalinization of the extract. Residues are separated and quantified by reverse-phase liquid chromatography using an ion-pairing mobile phase with UV and fluorescence detectors in tandem. Recoveries from 7 different food crops fortified at 0.2-35 ppm levels ranged from 64 to 105%.     

Liquid chromatographic determination of vitamin B-6 in foods

Chromatographic analysis for vitamin B-6 in complex samples imposes certain requirements on the analyst, who must extract completely the bound, unstable vitamers without loss, remove interfering compounds, and provide clean extracts for analysis. The analyst also has to contend with the problems inherent in all methods, such as sample collection, storage, preparation, and homogenization. However, chromatography provides a means of identifying and quantitating all forms of the vitamin, and thus provides the possibility of addressing the problem of the bioavailability of specific vitamers. It also allows automation, which is absolutely essential in coping with the large numbers of samples that are generated in areas such as quality control. These factors are all addressed here, and chromatographic results for various meat and other food products are presented to illustrate the variations in vitamin content that occur from sample to sample, the agreement with microbiological results, and that liquid chromatography (LC) has come of age in dealing with complex biological samples, such as food and food products.     

Simplified cleanup and liquid chromatographic ultraviolet determination of linuron and three metabolites in potatoes

A simple and efficient method is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of linuron and 3 of its metabolites, 3-(3,4-dichlorophenyl)-1-methyl urea (DCPMU), 3-(3,4-dichlorophenyl) urea (DCPU), and 3,4-dichloroaniline (DCA), in potatoes. Samples are extracted with acetone, partitioned into dichloromethane-hexane (1 + 1), and cleaned up using disposable silica cartridges. LC determination is performed using a LiChrosorb NH2 5 microns column, with an isopropanol-isooctane gradient mobile phase and UV detection at 248 nm. Recoveries of linuron and 2 of the metabolites from untreated samples fortified at 0.02-2 micrograms/g ranged from 80 to 102%, while recoveries for the metabolite DCA ranged from 60 to 78%. The detection limit was 0.015 micrograms/g for linuron and each metabolite; the minimum quantitation level was 0.5 micrograms/g. The developed method was applied to potato samples from a field experiment.     

Reverse-phase liquid chromatographic determination of benzoic and sorbic acids in foods

An isocratic liquid chromatographic (LC) technique is described for the determination of benzoic acid and sorbic acid in foods such as beverages, fruits, seafood, vegetables, sauces, and dairy, bakery, and confectionery products. A C18 column is used with methanol-phosphate buffer (5 + 95) as mobile phase and 4-hydroxyacetanilide or 3,5-dinitrobenzoic acid as internal standard. Sample preparation is simple, rapid, and produces a sample extract that has a minimum effect on the column performance and life. Specificity of the method was checked against common food additives such as L-ascorbic acid, caffeine, artificial sweeteners (saccharin, cyclamate, aspartame), antioxidants (BHT, BHA) and artificial colors. Also described are 2 procedures for confirmation of the preservatives, using either redox reaction of sorbic acid with potassium permanganate or gas chromatography/mass spectrometry. Mean recoveries of 90-105% were obtained with a precision of 1-6% and a detection limit of 20 mg/kg for the 2 preservatives.