Gas chromatographic measurement of phenolic acids and alcohols in human urine

Abstract

Methylene unit values of trimethyl silyl ether/ester and of methyl ester/trimethyl silyl ether derivatives of some biologically important phenolic acids were determined gas chromatographically under isothermal conditions. The former were chromatographed on 4 non-polar stationary phases, methyl-, methyl phenyl-, methyl phenyl vinyl-silicone gums and silicone oil, and the latter on methyl phenyl silicone gum and silicone oil. Methyl ester/trimethyl silyl ether derivatives of a number of phenolic alcohols were also run on methyl phenyl silicone gum. From a detailed evaluation of these investigations using both authentic compounds and urine extracts, suitable conditions were defined for the quantitative analysis of a large number of urinary phenolic acids and alcohols, with particular reference to 4-hydroxy-3-methoxymandelic and homovanillic acids; the most satisfactory quantitative system involved chromatography of the methyl ester/trimethyl silyl ether derivative on a 7 ft. 10% methyl phenyl silicone gum column. The application of these procedures to the investigation of abnormal phenolic acid excretion in phenylketonuria, alkaptonuria, tyrosyluria of the newborn and catecholamine-secreting tumours is discussed.