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Determination and excretion study of gestrinone in human urine by high performance liquid chromatography and gas chromatography/mass spectrometry
Author(s) -
Kim Yunje,
Lee Yongkwan,
Kim Myungsoo,
Yim YongHyeon,
Lee Won
Publication year - 2000
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/1097-0231(20000730)14:14<1293::aid-rcm28>3.0.co;2-0
Subject(s) - chemistry , chromatography , metabolite , urine , derivatization , mass spectrometry , high performance liquid chromatography , gas chromatography–mass spectrometry , gas chromatography , biochemistry
Gestrinone was studied by HPLC for screening and by GC/MS for confirmation. Three unknown peaks were found by HPLC which are probably the metabolites of gestrinone, and conjugated gestrinone in dosed human urine. The metabolites and gestrinone were excreted as the conjugated forms. The total amounts of metabolite 1 and conjugated gestrinone, recovered after 48 h, were 0.20 and 0.32 mg, respectively. When metabolite 1 was tested by LC/MS and LC/MS/MS, the parent ion was m/z 327, [MH] + , and fragment ions were seen at m/z 309 [MH − H 2 O] + , 291 [MH − 2H 2 O] + , 283, 263 and 239. The TMS‐enol‐TMS ether derivative of gestrinone has three peaks in the GC/MS chromatogram formed by tautomerism. The reproducibility of the derivatization method was stable and recoveries were over 87% when spiked into blank urine. Copyright © 2000 John Wiley & Sons, Ltd.