A study on the derivatization technique for tamoxifen metabolites in human urine by gas chromatography/mass spectrometry

기체크로마토그래피/질량분석기를 이용한 인체 내 뇨시료에서의 Tamoxifen 대사체 검출을 위한 유도체화 연구

  • Kim, Yunje (Doping Control Center, Korea Institute of Science and Technology) ;
  • Lee, Yoonjung (Doping Control Center, Korea Institute of Science and Technology)
  • 김연제 (한국과학기술연구원 도핑콘트롤센터) ;
  • 이윤정 (한국과학기술연구원 도핑콘트롤센터)
  • Received : 2004.06.16
  • Accepted : 2004.07.06
  • Published : 2004.08.25

Abstract

The improved derivatization technique of tamoxifen metabolite in human urine is described for the acylation method that they are substituted by derivatization reagent like acyl anhydride for use of gas chromatography/mass spectrometry. The hydroxyl group of tamoxifen metabolite was derivatized by trifluoroacetic anhydride (TFAA), pentafluoroacetic anhydride (PFPA) and heptaflorobutylic anhydride (HFBA). It was investigated to the gas chromatography/mass spectrometry (GC/MS) technique use negative ion chemical ionization (NCI), positive ion chemical ionization (PCI) and electron impact (EI). In acylation of the metabolites of tamoxifen, the effective reaction temperature and time were shown to be at $50^{\circ}C$ for 30 min. The 4-hydroxytamoxifen, which is known to major metabolite of tamoxifen, was not detected in human urine, whileas the hydroxymethoxytamoxifen was detected. We thought that this result was from the single dose of tamoxifen.

Keywords

Tamoxifen;metabolite;gas chromatography/mass spectrometry;acylation;derivatization;electron impact;chemical ionization

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