Three methods for cleavage of 17-ketosteroid sulfates were evaluated for their acceptability in the preparation of urine extracts for gas chromatography. Recovery after hydrolysis with hot hydrochloric acid was unacceptably low, but solvolysis with ethyl acetate—sulfuric acid or tetrahydrofuran—perchloric acid was equally efficient and satisfactory. The results obtained by four techniques were intercompared: radioactivity measurement, Zimmermann- or Allen-chromogen development, and gas chromatography.
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