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Determination of ibuprofen and its metabolites in human urine by GC-MS

GC-MS에 의한 소변 중 Ibuprofen의 대사체 규명 및 대사 연구

  • 유대형 (경희대학교 약학대학 약학과) ;
  • 조정흠 (경희대학교 약학대학 약학과) ;
  • 홍종기 (경희대학교 약학대학 약학과)
  • Received : 2010.03.10
  • Accepted : 2010.04.01
  • Published : 2010.04.25

Abstract

The oxidative metabolism of ibuprofen in healthy male urine collected at 3, 6, 9, 12 and 15 h after oral administration of ibuprofen was studied by GC/MS assay. To detect conjugated metabolites of ibuprofen, urine sample was acid-hydrolyzed with 6 M HCl at $100^{\circ}C$ for 30 min. To effectively extract ibuprofen and its metabolites, liquid-liquid extraction (LLE) was conducted at pH 3, 5, and 7, respectively. As a result, LLE at pH 3 was shown to be the best extraction condition. For the determination of trace amounts of ibuprofen and its metabolites in extract, trimethylsilylation (TMS) with BSTFA was applied and followed by GC/MS analysis. In this study, main 5 metabolites including parent drug were detected and these metabolites were assigned as three hydroxylated forms and one carboxylated form. Each metabolite was tentatively identified by both interpretation of mass spectrum and comparison with previously reported results. In addition, time profile of urinary excretion rate for parent drugs and metabolites was studied. Finally, the metabolic pathways of ibuprofen were suggested on the basis of the structural elucidation of its metabolites and excretion profiles.

Keywords

ibuprofen;urine;metabolites;TMS;GC/MS;mass spectrum

Acknowledgement

Grant : 유해물질 인체 모니터링

Supported by : 식품의약품안전청

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