Collaborative study of the determination of boric acid in caviar by emission spectroscopy.

Caviar samples were spiked at the 0.1 and 0.2% levels and digested with nitric acid in a closed Teflon-lined digestion vessel to prevent volatility losses. The boron was complexed with 2-ethyl-1,3-hexanediol and extracted into methylisobulty ketone. The emission of the boron oxide band was measured in a nitrous oxidehydrogen flame. The mean recoveries at the 0.1 and 0.2% levels for 6 collaborators were 95.7 and 97.1%, respectively.     

Colorimetric determination of mestranol in combination with ethynodiol diacetate.

Mestranol in combination with ethynodiol diacetate, an oral contraceptive formulation, is isolated from the sample on a partition chromatographic column prior to colorimetric determination. The color reaction which is specific for estrogens is formed by shaking an aliquot of the heptane eluate of mestranol with a 30% methanol-sulfuric acid solution. A collaborative study of the method gave results of 99.8% of added mestranol for the simulated mix and 100.7% of labelled mestranol for the commercial tablet. The method has been adopted as official first aciton.     

Colorimetric determination of uric acid in poultry excreta and in mixed feeds

Uric acid was determined in samples of poultry excreta and animal feeds to which poultry excreta were added. The rapid colorimetric method used by Van Handel was adapted for this purpose. The method is simple, accurate, and gives reproducible results.     

Colorimetric determination of poly(N-vinyl-2-pyrrolidone) in contact lens solutions.

A rapid colorimetric method is presented for the quantitative determination of poly(N-vinyl-2-pyrrolidone) in contact lens solutions. The method is simple, requires no sample pretreatment, and uses only a small volume of sample. The procedure is based on the measurement of the net absorbance of a poly(N-vinyl-2-pyrrolidone)- Congo red complex at 545 nm. An accuracy of greater than +/- 4% was obtained for the concetnration ranges usually found in contact lens solutions with a minimum detection level of 10 ppm. The method is useful as a screening procedure for solutions of unknown composition and as a quality assurance procedure for routine determinations.     

One-step extraction and cleanup procedure for determination of p,p'-DDT, p,p'-DDD, and p,p'-DDE in fish

A simplified method that combines extraction, partitioning, and cleanup in a single step for measuring p,p'-DDT and its metabolites in fish is described. Minced fish samples are emulsified with disodium hydrogen orthophosphate and trisodium citrate, ground with sodium sulfate, and eluted from a chromatographic column prepacked with alumina and silicic acid. The fats and fatty acids are solubilized and easily extracted from the tissues and retained by the column, while p,p'-DDT and its metabolites are quantitatively eluted with 40 mL n-hexane. The eluate is directly applied to a gas chromatographic column. Average recoveries of p,p'-DDT and its metabolites added to fish in vitro are 81%. The average coefficient of variation for recoveries of p,p'-DDT and its metabolites is less than 6.5% and the detection limit is 0.001 micrograms/g for p,p'-DDE, thus making this method very suitable for residue analysis.     

Gas-liquid chromatographic determination of residues of methanesulfonate of n-aminobenzoic acid ethyl ester in fish.

In this gas-liquid chromatographic procedure for determining residues of methanesulfonate of m-aminobenzoic acid ethyl ester (MS-222) in fish muscle, homogenized tissue is extracted with distilled water, and proteins are removed by coagulation with trichloroacetic acid, centrifugation, and filtration. After careful pH adjustment of the filtrate, MS-222 is partitioned into benzene-ethyl ether and measured by alkali flame ionization gas chromatography. Tissues with known additions of 1-19 microgram MS-222/g were analyzed, with recoveries of 84-95%.     

Distribution of bromophenols in species of marine polychaetes and bryozoans from eastern Australia and the role of such animals in the flavor of edible ocean fish and prawns (shrimp).

Sixteen species (44 samples) of marine polychaetes and 10 species (14 samples) of bryozoans from eastern Australia were analyzed by GC/MS for the key seafood flavor components 2- and 4-bromophenol, 2, 4- and 2,6-dibromophenol, and 2,4,6-tribromophenol. All five bromophenols were found in 91% of polychaetes and 64% of bryozoans. The remaining samples all contained at least three bromophenols. 2,4, 6-Tribromophenol was found in all polychaetes and bryozoans and, with few exceptions, was present in the highest concentrations. The total bromophenol content determined on a wet-weight basis varied widely between species: for polychaetes, from 58 ng/g for Australonuphis teres to 8.3 million ng/g for Barantolla lepte, and for bryozoans, from 36 ng/g for Cladostephus spongiosus to 1668 ng/g for Amathia wilsoni. Species of polychaetes with the highest concentrations of bromophenols were all collected from muddy environments. The possible effects that dietary polychaetes and bryozoans have on the ocean-, brine-, or iodine-like flavors of certain seafoods are discussed.     

Determination of total N-nitroso compounds and their precursors in frankfurters, fresh meat, dried salted fish, sauces, tobacco, and tobacco smoke particulates.

Total N-nitroso compounds (NOC) and NOC precursors (NOCP) were determined in extracts of food and tobacco products. Following Walters' method, NOC were decomposed to NO with refluxing HBr/HCl/HOAc/EtOAc and NO was measured by chemiluminescence. NOC were determined after sulfamic acid treatment to destroy nitrite, and NOCP were determined after treatment with 110 mM nitrite and then sulfamic acid. Analysis without HBr gave results < or =20% of those with HBr. This NOC method was efficient for nitrosamines but not nitrosoureas. The standard nitrosation for determining NOCP gave high yields for readily nitrosated amines, including 1-deoxy-1-fructosylvaline, but not for simple amines, dipeptides, and alkylureas. Mean NOC and NOCP results were (respectively, in micromol/kg of product) 5.5 and 2700 for frankfurters, 0.5 and 660 for fresh meat, 5.8 and 5800 for salted, dried fish, and 660 and 2900 for chewing tobacco (all for aqueous extracts) and 220 and 20000 nmol/cigarette for MeCN extracts of cigarette smoke filter pads.     

Colorimetric and spectrophotometric determination of total and non-phenolic alkaloids in ipeca and its formulations.

A simple method, requiring no chromatographic separation, is presented for the determination of the total and non-phenolic alkaloids in ipeca and its preparations. The complex formed between the alkaloid and methyl orange at pH 5.0 is extracted with chloroform and treated with 0.1N NaOH. The liberated dye, determined at 460 nm, is a measure of the total alkaloids. The chloroform phase remaining is treated with 0.1N H2SO4, and the acid extract is measured at 283 nm for the non-phenolic alkaloids, calculated as emetine. The proposed method was successfully applied to samples of ipeca powder, ipeca tincture, and 3 British Pharmaceutical Codex mixtures containing ipeca tincture, namely, ipecacuanha mixture, pediatric; ipecacuanha and ammonia mixture, pediatric; and belladonna and ipecacuanha mixture, pediatric. The proposed method compares favorably with the Egyptian Pharmacopoeia, British Pharmacopoeia, and USP methods and has a relative standard deviation of 1.54%. The present procedure is less time-consuming and requires about 45 and 90 min for the assay of ipeca tincture and powder, respectively. Only a small sample (0.2 mL tincture of 1.0 g powder) is required.     

Analysis of 2-alkylcyclobutanones with accelerated solvent extraction to detect irradiated meat and fish

A new analytical procedure has been developed to analyze 2-alkylcyclobutanones to detect gamma-ray-irradiated fat-containing foodstuffs. Samples were extracted with an accelerated solvent extraction system via hot and pressurized ethyl acetate in cells. A large amount of fat in the extract was precipitated and removed with filtration by standing at -20 degrees C after the addition of acetonitrile. The extract was further cleaned with a 1 g silica gel mini column, and the radiolytic compounds of 2-docecylcyclobutanone (2-DCB) and 2-tetradecylcyclobutanone (2-TCB) were determined with gas chromatography with mass spectrometry (GC/MS). Sample preparation time before GC/MS was 7-8 h. At first, the procedure was evaluated with a recovery test in eight samples spiked with 2-DCB and 2-TCB at 20 ng/g, resulting in 70-105% recoveries with mostly less than 10% relative standard deviations. The procedure was further evaluated with beef, pork, chicken, and salmon samples irradiated with gamma-rays from 0.7 to 7.0 kGy at -19 degrees C. Both 2-DCB and 2-TCB in most samples were detected with good dose-response relations at all doses, while salmon was detected more than 2 kGy irradiation. The amounts of 2-alkylcyclobutanones produced reflected precursor fatty acids levels in samples, especially for the combination of 2-TCB and stearic acid. The results indicated that the production rate of 2-TCB to stearic acid was more obvious than that of 2-DCB to palmitic acid in frozen samples with gamma-ray irradiation.     

Separation and determination of diesel contaminants in various fish products by capillary gas chromatography.

A semiquantitative capillary column gas chromatographic method is described for the determination of diesel fuel contamination in various canned seafood products. The diesel contaminants are separated from the fish sample by steam distillation, with little carry-over of interfering intrinsic materials such as fish oils. The diesel fuel is extracted from the condensate with n-hexane, and the extract is analyzed on an SPB-1 fused silica capillary column. The efficiency of recovery of diesel fuel added to canned seafood at levels of 40-400 ppt ranged from 72 to 102%. With the additional step of concentrating the hexane extract, the sensitivity of this procedure may be increased at least 10-fold. This procedure can detect the differences among diesel fuel grades No. 1, 2, and 5, and variations within diesel grade No. 2, and thus may be useful in determining the type of petroleum contaminants present in various canned fish products.     

Analysis of patulin in apple juice by diphasic dialysis extraction with in situ acylation and mass spectrometric determination.

A procedure combining diphasic dialysis extraction with in situ acylation and gas chromatography/mass spectrometry (GC/MS) determination was developed for detection and quantification of the mycotoxin patulin in apple juice. Apple juice samples spiked with 4-N,N-dimethylaminopyridine were dialyzed using methane chloride and acetic anhydride inside dialysis tubing. Patulin was derivatized into its acetate and collected in the tubing after diphasic dialysis and was directly determined using GC/MS with the selective ion monitoring mode without further concentration and cleanup steps. Quantification was carried out by a calibration curve with an internal standard of correlation. The appropriate parameters of both dialysis and derivatization were examined. The linear range of the calibration curve was found to be 10-250 microg/L for patulin, and the limit of quantification was 10 microg/L. Levels of patulin ranging from 0 to 107.2 microg/L with 77-109% recovery were found in 10 apple samples. The technique combining diphasic dialysis extraction and acylation was demonstrated and showed potential for other applications.     

Liquid chromatographic determination of L-ascorbate 2-polyphosphate in fish feeds by enzymatic release of L-ascorbate

An accurate method was devised to assay L-ascorbic 2-polyphosphate esters (AsPP) in fish feed by phosphatase digestion followed by determination of the released L-ascorbic acid (AsA). Compressed yeast and dithiothreitol are added to the phosphatase reaction mixture to give 95-100% recovery of AsA, which is quantitated by reverse-phase liquid chromatography (LC) with electrochemical detection. Chromatograms of all feed digests showed baseline resolution of AsA. In 3 feeds, to which 75-125 ppm AsA equivalents in the form of AsPP were added, the assay procedure gave 98-100% recovery of AsA.     

Colorimetric and gas-liquid chromatographic determination of atropine-hyoscyamine and hyoscine (scopolamine) in solanaceous plants.

Two colorimetric micromethods are described for the determination of atropine-hyoscyamine and hyoscine (scopolamine), using p-dimethylaminobenzaldehyde and citric acid-acetic anhydride as the color reagents. These methods are sensitive to 60-1200 and 10-360 mug alkaloid/10 ml. The colorimetric methods were also successfully applied after a preliminary thin layer chromatographic separation of the alkaloids. A gas-liquid chromatographic procedure was also developed, which yielded comparable results with the colorimetric methods.     

Liquid chromatographic determination of rotenone in fish, crayfish, mussels, and sediments

An analytical procedure is described for determining residues of rotenone in fish muscle, fish offal, crayfish, freshwater mussels, and bottom sediments. Tissue samples were extracted with ethyl ether and extracts were cleaned up by gel permeation chromatography and silica gel chromatography. Sediment samples were extracted with methanol, acidified, partitioned into hexane, and cleaned up on a silica gel column. Rotenone residues were quantitated by liquid chromatography, using ultraviolet (295 nm) detection. Recoveries from sediment samples fortified with rotenone at 0.3 microgram/g were 80.8%, whereas recoveries from tissue samples fortified with 0.1 microgram/g ranged from 87.7 to 96.8%. Samples fortified with 0.3 microgram/g and stored at -10 degrees C for 6 months before analysis had recoveries ranging from 83.2 to 90.5%. Limits of detection were 0.025 microgram/g for sediments and 0.005 microgram/g for tissue samples.