Abstract
SUMMARY Chloromethyldimethylsilyl ethers (CDMSE) of androsterone, aetiocholanolone and dehydroepiandrosterone were prepared by reacting the steroids with chloromethyldimethylchlorosilane and diethylamine in hexane. These derivatives gave more reproducible results than the corresponding trimethylsilyl ethers (TMSE) during gas chromatography on thin-film columns (e.g. 0·6% XE60). Interfering matter from urine extracts which can occur in the androsterone TMSE peak, was eliminated when CDMSE derivatives were used. The use of CDMSE derivatives in the routine analysis of urinary 11-deoxy-17-oxosteroids by gas-liquid chromatography, compared favourably with that of TMSE derivatives in terms of specificity, sensitivity, accuracy and precision.

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