Polybasic organic acids in fruits are separated by precipitation as lead salts. Trimethylsilyl derivatives formed directly from these lead salts are separated and identified by gasliquid chromatographic procedures. Twentyseven types and varieties of fruits were analyzed and reported.
A rapid quantitative method for determining 8 antioxidants in various food products is described. Two procedures are employed. The first involves the use of a glass wool precolumn to separate 3(2)-tert-butyl-4-hydroxyanisole, 3,5-di -tert - butyl - 4 - hydroxytoluene, 4 - hydroxymethyl- 2,6-di-tert-butylphenol, and mono-tertbutylhydroquinone (TBHQ) from nonvolatile residues resulting from direct injection of diluted sample or sample extracts into the gasliquid chromatographic (GLC) column. In the second procedure, the antioxidants TBHQ, 3,3'- thiodipropionic acid, n-propyl gallate, 2,4,5- trihydroxybutyrophenone, and nordihydroguaiaretic acid are isolated from food products by extraction with 70% ethanol. The antioxidant residues are then converted to trimethylsilyl derivatives, and determined by GLC, using a flame ionization detector. Recoveries of all 8 antioxidants from 28 food samples fortified at either 10 or 100 ppm ranged from 70 to 105%.
A variety of food products containing nitrite were analyzed for 14 volatile N-nitrosamines by using a method demonstrated to be sensitive to 10 ppb. A total of 121 food samples were screened for volatile N-nitrosamine content. N-Nitrosopyrrolidine was confirmed in fried bacon at levels up to 139 ppb. N-Dimethylnitrosamine, N-nitrosopyrrolidine, and N-nitrosopiperidine were also confirmed in spice-cure mixtures at levels ranging from 50 to 2000 ppb.
A gas-liquid chromatographic (GLC)-mass spectral (MS) method for the determination and confirmation of urethane in wines has been developed. Analyses of domestic and imported wines indicated urethane to be present at levels ranging from 1 to 20 μg/L. Recoveries of urethane from wines fortified at 10 ppb (μg/L) ranged from 50 to 100% with an average value of 71%. GLC-MS was used to confirm the identity of urethane in wine extracts in which GLC indicated the presence of urethane.
V method utilizing gas-liquid chromatography and the Sorensen formol titration procedure has been devised for the qualitative and quantitative analysis of amino acids in fruits. Korty-four samples representing 22 varieties of fruits were analyzed for 15 free amino acids. The amino acids were determined as N-trifluoroacetyl n-butyl esters. In a majority of the fruits, aspartic acid was the major component, while hvdroxvproline was the minor component when present. All fruits were found to have different quantitative profiles as well as a distinct qualitative distribution of the free amino acids.
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