Determination of the metabolites of gestrinone in human urine by high performance liquid chromatography, liquid chromatography/mass spectrometry and gas chromatography/mass spectrometry.
Gestrinone was studied by high performance liquid chromatography (HPLC) for screening and by gas chromatography/mass spectrometry (GC/MS) for confirmation. When the chromatograms of blank, spiked urine and dosed urine were compared by HPLC, two unknown metabolites were found and these were excreted as the conjugated forms. Metabolites 1 and 2 were tested by LC/MS and LC/MS/MS and both had parent ions at m/z 325. The fragment ion of metabolite 1 was at m/z 263 and ions for metabolite 2 were m/z 307 [MH - H(2)O](+), 289, 279 and 241. LC/MS/MS of m/z 263 as the parent ion of metabolite 1 gave fragment ions at m/z 245 and 217, which were assumed to be [263 - H(2)O](+) and [235 - H(2)O](+), respectively. The trimethylsilyl (TMS)-enol-TMS ether derivative of gestrinone displayed three peaks in its GC/MS chromatogram, formed by tautomerism.
Kim
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Y
Doping Control Center, Korea Institute of Science and Technology, P. O. Box 131, Cheongryang, Seoul, Korea. yjkim@kistmail.kist.re.kr
Lee
Y
Y
Kim
M
M
Yim
Y H
YH
Lee
W
W
D000328:Adult; D045930:Anabolic Agents / Q000493:pharmacokinetics / Q000652:urine*; D001711:Biotransformation; D002851:Chromatography, High Pressure Liquid; D003280:Contraceptives, Oral, Synthetic / Q000493:pharmacokinetics / Q000652:urine*; D008401:Gas Chromatography-Mass Spectrometry; D005867:Gestrinone / Q000493:pharmacokinetics / Q000652:urine*; D006801:Humans; D007202:Indicators and Reagents; D008297:Male; D013058:Mass Spectrometry
D045930:Anabolic Agents; D003280:Contraceptives, Oral, Synthetic; D007202:Indicators and Reagents; D005867:Gestrinone