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Detection of androst-4-ene-3,6,17-trione (6-OXO) and its metabolites in urine by gas chromatography-mass spectrometry in relation to doping analysis.

Van Thuyne W, Van Eenoo P, Mikulcíková P, Deventer K, Delbeke FT

Doping Control Laboratory, Department of Clinical Biology, Microbiology and Immunology, Ghent University-UGent, Technologiepark 30, B-9052 Zwijnaarde, Belgium.

The metabolism and excretion of androst-4-ene-3,6,17-trione after administration of the 'nutritional' supplement 6-OXO was investigated by gas chromatography-mass spectrometry (GC-MS) in full-scan mode. The parent drug androst-4-ene-3,6,17-trione and androst-4-ene-6alpha,17beta-diol-3-one and androst-4-ene-6alpha-ol-3,17-dione were detected in the post-administration urine samples. Because androst-4-ene-3,6,17-trione is an anabolic steroid and an aromatase inhibitor, this substance is regarded as a doping agent. Hence, a selective and sensitive GC-MS method in selected ion monitoring mode for the detection of the TMS-enol-TMS-ether derivatives of these substances was developed and validated for doping control purposes. The limit of detection (LOD) of the investigated compounds ranged from 5 to 10 ng/mL. Using this method, the detection time for androst-4-ene-3,6,17-trione and androst-4-ene-6alpha,17beta-diol-3-one was 24 h, while androst-4-ene-6alpha-ol-3,17-dione could be detected up to 37 h after administration of the dose recommended by the manufacturer.

Published 2 November 2005 in Biomed Chromatogr, 19(9): 689-95.
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