Thin-layer chromatographic method for urinary 4-hydroxy-3-methoxymandelic acid (vanilmandelic acid).
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Biomedical subjects
Publications and source records attributed to B H Gump.
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The low concentration of hydrocarbons anticipated in pollution baseline studies necessitates the development of analytical techniques sensitive at the sub-microgram per kilogram concentration level. The method of analysis developed in this laboratory involves dynamic headspace sampling for volatile hydrocarbon components of the sample, followed by coupled-column liquid chromatography for the non-volatile components. These techniques require minimal sample handling, reducing the risk of sample component loss and/or sample contamination. Volatile sample components are separated from the matrix in a closed system and concentrated on a TENAX-GC packed pre-column, free from large amounts of solvent and ready for GC/GC-MS analysis. Non-volatile compounds, such as the benzpyrenes, may be extracted from large volumes of water and concentrated on a Bondapak C18 packed pre-column for coupled-column liquid chromatographic separation and analysis. Results of the application of these techniques to the analysis of samples from sites of known low level hydrocarbon contamination are presented and discussed.
A method for the determination of total sulfite in shrimp, potatoes, dried pineapple, and white wine by flow injection analysis (FIA) was collaboratively studied by 8 laboratories. In the method, the sample solution is reacted with sodium hydroxide to liberate aldehyde-bound sulfite. The sample stream is acidified to produce SO2 gas, which diffuses across a Teflon membrane in the gas diffusion cell into a flowing stream of malachite green. The degree of discoloration of the malachite green is proportional to the amount of sulfite in the sample solution. Red wine was included in the study but interlaboratory precision for these samples was not satisfactory and correlation with Monier-Williams results was poor. The present method is not recommended for use with these samples. For shrimp, potatoes, dried pineapple, and white wine, average reproducibility (RSDR) of results was 25% for samples at 10 ppm SO2 and 10% for samples at greater than 50 ppm. Overall average reproducibility was 14%. Recoveries of sulfite added to samples averaged 80%. Comparison of FIA with the Monier-Williams method indicated comparable results by the 2 methods. The FIA method has been adopted official first action for determination of greater than or equal to 5 ppm total sulfite in shrimp, potatoes, dried pineapple, and white wine.
A method for the determination of free sulfite in wine by flow injection analysis (FIA) is described. The method involves liberation of sulfur dioxide from the wine at pH 2.2, with detection by decolorization of a malachite green solution. The method was collaboratively studied, and the results indicated an average reproducibility of 12% for white wine samples (average level 12.1 ppm SO2) and 26% for red wine samples (average level 3.1 ppm). When the FIA method was compared to an aeration/oxidation method, the results indicated a high degree of correlation between the 2 methods. The FIA method has been adopted by AOAC official first action.
Phosphorus in wine may be determined directly or indirectly by atomic absorption spectrometry. The direct method uses the carbon rod atomizer as the excitation source and a phosphorus hollow cathode lamp. In the indirect determination, one measures the amount of molybdenum that will complex with phosphorus in the wine. Both nitrous oxide-acetylene and air-acetylene flames are suitable as atomization sources in this indirect method. The resultant data have been compared with those from the AOAC colorimetric method (11.032-11.034). A 2-sample comparison test showed the results to be insignificantly different at the 95% confidence limits.