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제109회 대한화학회 학술발표회, 총회 및 기기전시회 안내 Comparison of GC/MS and LC/MS methods for the determination of propofol and its metabolites in human urine

2012년 2월 16일 14시 55분 15초
ANAL.P-584 이곳을 클릭하시면 발표코드에 대한 설명을 보실 수 있습니다.
4월 25일 (수요일) 18:00~21:00
저자 및
이선영, 박나현, 홍종기
경희대학교 약학과, Korea
Propofol and its phase I and II metabolites were determined by gas chromatography?mass spectrometry (GC/MS) and liquid chromatography?mass spectrometry (LC/MS) in human urine. Urine samples were collected at 0, 6, 12, 18, 24, and 48 hr after an intravenous injection. For GC/MS analysis, acidic hydrolysis, liquid-liquid extraction (LLE), and trimethylsilyl (TMS) derivatization procedure were subsequently applied. For LC-ESI-MS/MS analysis, a simple sample treatment based on centrifugation and dilution was applied. In case of GC/MS, overall amount of propofol and phase I metabolites obtained without hydrolysis were much lower than those after acidic hydrolysis. From this observation, most of these compounds might be presented as glucuronide or sulfate conjugated form in urine. Moreover, the detection sensitivity of propofol and its metabolites was improved after TMS derivatization. The linearity ranges by GC/MS scan mode was 1-2000 μg/mL for propofol TMS derivatizative. The limits of quantitation (LOQ) for propofol TMS derivatization was 325 ng/mL at S/N of 10. In case of LC-MS/MS, five conjugated metabolites were identified by the interpretation of their tandem mass spectral data and LC elution patterns. On the other hand, propofol and its unconjugated metabolites could not well observe due to its low MS detection sensitivity in both positive and negative ion modes. The linearity ranges by LC-ESI-MS-MRM mode was about 5-2000 ng/mL for propofol-glucuronide(PG). The limit of quantitation (LOQ) obtained by LC-MS-MRM mode for PG was 0.48 ng/mL. In addition, time profile of urinary excretion of propofol and its metabolites was presented using GC/MS and LC/MS. Based on this study, comprehensive assessment of propofol and its metabolites was compatible with GC/MS and LC-ESI-MS/MS.