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目的建立同时测定地西泮及其代谢产物质量浓度的HPLC-MS/MS方法。方法色谱柱:Kromasil C18,流动相:乙腈-2 mmol·L-1乙酸铵水溶液(70∶30),流速:0.3 m L·min-1,柱温:40℃,用正离子扫描,多反应监测方式测定样品中药物的质量浓度。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、基质效应及稳定性。结果肝微粒体孵育样品中,地西泮在20~1000ng·m L-1线性关系良好(r>0.99),定量下限为20 ng·m L-1。去甲地西泮、替马西泮和奥沙西泮在2~100 ng·m L-1线性关系良好(r>0.99),定量下限为2ng·m L-1。地西泮、去甲地西泮、替马西泮和奥沙西泮绝度回收率分别在55.47%~68.76%,64.84%~79.11%,68.32%~78.27%和72.66%~83.82%,日内与日间精密度均小于15%。结论本研究方法简便、快速、准确,适用于测定肝微粒体孵育样品中地西泮及其代谢产物的浓度。
Objective To establish a HPLC-MS / MS method for the simultaneous determination of diazepam and its metabolites. Methods Column: Kromasil C18, mobile phase: acetonitrile-2 mmol·L-1 ammonium acetate aqueous solution (70:30), flow rate: 0.3 m L · min-1, column temperature: 40 ℃, Monitoring methods determine the mass concentration of the drug in the sample. Investigate the specificity of this method, the standard curve and lower limit of quantitation, precision and recovery, matrix effects and stability. Results In the liver microsomal incubation samples, the linearity of diazepam was 20 ~ 1000 ng · m L-1 (r> 0.99), and the lower limit of quantitation was 20 ng · m L-1. There was a good linear relationship between niapazepam, temazepam and oxazepam at 2 ~ 100 ng · m L -1 (r> 0.99), and the lower limit of quantification was 2 ng · m L -1. The absolute recoveries of diazepam, noradazepam, temazepam and oxazepam were 55.47% -68.76%, 64.84% -79.11%, 68.32% -78.27% and 72.66% -83.82%, respectively. Days and days Between the precision of less than 15%. Conclusion The method is simple, rapid and accurate and is suitable for the determination of diazepam and its metabolites in liver microsomal samples.