A method for the determination of lead in fish by atomic absorption spectrophotometry and polarography is described. The samples were dry-ashed at 500°C and dissolved in IN HC1; lead was determined by either method. Good agreement between atomic absorption spectrophotometry and polarography was obtained at levels of 1.0 to 10.0 ppm. Over this range the recoveries averaged 96.1% for polarography and 93.8% for atomic absorption spectrophotometry. Twelve species of fresh and salt water fish were analyzed.
A method has been developed for the detection and quantitation of β-asarone in vermouths. Volatiles are isolated by steam distillation, and β-asarone is separated from interfering substances by solvent extraction and subjected to gas chromatographic analysis. Quantitation of samples containing 5–100 ppm β-asarone was achieved by direct chromatographic peak comparisons with standards prepared in 20% ethanol-water, which are treated the same as samples. Average recovery from light and dark vermouths spiked at 5, 15, 25, and 100 ppm was 98.8%.
GLC method has been developed for the quantitation of ammonium glycyrrhizinate as the aglycone, glycyrrhetic acid. The aglycone is freed from the sugar moiety in a dioxanewater mixture, using a well established acid hydrolysis procedure. The hydrolysate is extracted with chloroform, an aliquot is dried on a steam bath, and the residue is treated with pyridine - trimethylchlorosilane - N,0 - bis (trimethylsilyl)acetamide reagent. The reacted product and internal standard are then chromatographed on a column of 1.5% OV-1 on Gas Chrom Q. Recoveries from both water and sodas containing caramel averaged 87%.
Samples of 6 types of foods containing saccharin were subjected to a cleanup procedure, using lead acetate or alcohol precipitation. Saccharin was extracted with a combination of solvents and the extracts were treated with phenol and sulfuric acid and heated to form colored phenolsulfonphthalein derivatives. The color was measured spectrophotometrically at 558 nm. The method was applied to soft drinks, fruit juices, food sweetener tablets, concentrated liquid sweeteners, jellies, preserves, low calorie high protein powders, granulates, and liquids, and chocolate bars. Recoveries ranged from about 90.3 to 121.0% in spiked samples. Satisfactory recovery was obtained for levels as low as 5 mg/100 g sample (0.005%).
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