PubMed · 5413223
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M D Vickers. 1970. Explosion hazards.. https://pubmed.ncbi.nlm.nih.gov/5413223/
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This study describes the development of a method for determining eleven sulphur compounds in wine, which takes into account that thiols are easily oxidizable. The equilibria of the analytes between air and aqueous ethanol were studied and optimised using static headspace gas chromatography in order to obtain the best sensitivities. The influences of parameters such as temperature, time, ionic strength, headspace volume and the volume of headspace injected were determined. A cryogenic trap was used to concentrate the headspace analytes and they were chromatographically analysed using GC temperature programming on a poly(ethylene glycol) capillary column with FPD detection at 394 nm. The power relationship was observed between the chromatography response and a concentration of sulphur compounds in the range 2-150 micrograms l(-1) in the sample. Recoveries were determined by the standard addition technique and were higher than 90% for sulphides and disulphides and close to 80% for thiols. The overall method was successfully used to determine the sulphur compounds in white and red wines.
At the end of a workweek 23 silkscreen printers gave a urine sample for capillary gas chromatographic analysis for 1,2-propanediol. The mean concentration was 2.52 (S.D. 2.01) mmol mol creatinine(-1) (median=1.76, n=23). The urinary excretion of 1,2-propanediol was linearly dependent on the preceding 1-methoxy-2-propanol exposure measured in the worker's breathing zone [y=0.99+0.28x, n=23, r=0.67, where y is the urinary 1,2-propanediol concentration, in mmol mol creatinine(-1) and x is the concentration, in cm3 m(-3), of 1-methoxy-2-propanol (90.2%), 1-ethoxy-2-propyl acetate (5.8%), 1-methoxy-2-propyl acetate (2.1%) and 1-ethoxy-2-propanol (1.9%) in the air].
Following deproteinization of plasma with organic solvents the supernatant was shaken with hexane and cation-exchange resin in an Eppendorf tube to remove fatty and amino acids and the medium was subjected to direct treatment with ethyl chloroformate under catalytic influence of pyridine. A subsequent extraction of the immediately formed ethyl esters with a drop of chloroform enabled us to subject the sample to gas chromatographic (GC) analysis. Since ketocarboxylic acids do not require a preliminary oximation the total time of sample workup and analysis takes only several minutes.