摘要
目的:建立一种检测人血浆中奥拉西坦的液相色谱-质谱联用(LC-ESI-MS)的方法。方法:加入吡拉西坦为内标,血浆中的药物用甲醇沉淀法去蛋白。采用Agilent Zorbax SB-C18(2.1 mm×100 mm,3.5μm)柱,流动相为甲醇-0.1%甲酸溶液(5:95,v/v)。采用电喷雾离子源(ESI),正离子检测,选择性离子监测(selected ion mon itoring,SIM)方式进行定量分析奥拉西坦,监测离子峰分别是m/z 158.5(奥拉西坦)和m/z 142.5(内标)。结果:血浆中奥拉西坦检测方法的线性范围为0.1-8μg/m l,最低定量限为0.1μg/m l,平均回收率在91.5%-96.4%之间,日内和日间精密度RSD都小于9%。结论:本方法简单、灵敏、快速,可用于药物动力学研究。
Objective:To develop a LC-ESI-MS method for determination of oxiracetam in human plasma.Methods:After addition of piracetam as internal standard,protein precipitation by methanol was used as sample preparation.Chromatographic separation was achieved on a Zorbax SB-C18(2.1 mm×100 mm,3.5 μm)column with(5:95,v/v) methanol-water containing 0.1% formic acid as mobile phase.Electrospray ionization(ESI) source was applied and operated in positive ion mode and selected ion monitoring(SIM) mode was used to quantify oxiracetam using target fragment ions m/z 158.5 for oxiracetam and m/z 142.5 for the IS.Results:Calibration plots were linear over the range of 0.1-8 μg/ml for oxiracetam in plasma.Lower limit of quantitation(LLOQ) for oxiracetam was 0.1 μg/ml.Mean recovery of oxiracetam from plasma was 91.5%-96.4%.RSD of intra-day and inter-day precision was less than 9%,respectively.Conclusion:This method is simple,sensitive and fast enough to be used in pharmacokinetic research for determination of oxiracetam in plasma.
出处
《中国卫生检验杂志》
CAS
2010年第1期79-80,共2页
Chinese Journal of Health Laboratory Technology