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Derivatization of estrogen conjugates for analysis by capillary gas chromatography
Authors:C H Shackleton
Institution:Dept. of Laboratory Medicine, University of California, San Francisco, CA 94143 and Biomedical Mass Spectrometry Resource, University of California, Berkeley, CA 94720 USA
Abstract:By using 20 meter wall-coated open tubular glass capillary columns of high stability, analysis of methyl ester, methyloxime trimethylsilyl ether derivatives of estrogen glucuronides had been achieved. Relative retention times of five glucuronide conjugates on OV-1 stationary phase are reported. Estrogen sulfates conjugated at the 3-position were shown to be quantitatively hydrolyzed and derivatized in a single trimethylsilylation step, and this method of direct derivatization was compared to two solvolysis methods. These analytical methods could be further developed to allow rapid and quantitative analysis of estrogens in biological fluids, and may prove particularly useful for analysis of labile compounds.
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