Determination of the metabolites of gestrinone in human urine by high performance liquid chromatography, liquid chromatography/mass spectrometry and gas chromatography/mass spectrometry

被引:0
作者
Kim, Y
Lee, Y
Kim, M
Yim, YH
Lee, W
机构
[1] Korea Inst Sci & Technol, Doping Control Ctr, Seoul, South Korea
[2] LG Chem Ltd, Taejon, South Korea
[3] Kyung Hee Univ, Res Inst Basic Sci, Seoul, South Korea
[4] Kyung Hee Univ, Dept Chem, Seoul, South Korea
关键词
Ether derivatives - Fragment ions - Gaschromatography-mass spectrometry - High-performance liquid chromatography - Human urine - LC-MS-MS - Liquid chromatography - mass spectrometries - Parent ions - Trimethylsilyl - Trimethylsilyl ethers;
D O I
10.1002/1097-0231(20000930)14:18<1717::AID-RCM65>3.0.CO;2-2
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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 - H2O](+), 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 - H2O](+) and [235 - H2O](+), respectively. The trimethylsilyl (TMS)-enol-TMS ether derivative of gestrinone displayed three peaks in its GC/MS chromatogram, formed by tautomerism. Copyright (C) 2000 John Wiley gr Sons, Ltd.
引用
收藏
页码:1717 / 1726
页数:10
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