LC-MS/MS法测定人血浆中阿立哌唑及其代谢物脱氢阿立哌唑浓度

目的: 建立液相色谱串联质谱法测定人血浆中阿立哌唑和脱氢阿立哌唑浓度。 方法: 血浆样品中加入适量内标和饱和碳酸氢钠,以乙醚萃取后采用API 3000 LC-MS/MS进行分析。色谱柱采用Chembond ODS-W柱(2.1 mm×150 mm,3.5 μm),柱温30 ℃,流动相由乙腈-0.1%醋酸水溶液(60∶ 40,v/v)组成,流速0.2 mL·min^-1。质谱采用多反应离子监测(MRM)的扫描模式,以电喷雾离子源(ESI)在正离子电离模式下进行测定。 结果: 本方法的线性范围是0.1~100 ng·mL^-1,最低定量限为0.1 ng·mL^-1,日内、日间精密度均小于15%,准确度在85%~115%之间,萃取回收率约70%~80%,稳定性考察结果良好。 结论: 本方法快速、灵敏,专属性强,适用于阿立哌唑的人体药代动力学研究。

Objective: To develop an LC-MS/MS method for the determination of aripiprazole and dehydroaripirazole in human plasma. Methods: The plasma samples were extracted with ether after addition of internal standard and sodium bicarbonate,and then analyzed with API 3000 LC-MS/MS system.The analytical column was Chembond ODS-W(2.1 mm×150 mm,3.5 μm) and the column temperature was set at 30 ℃.The mobile phase was composed of acetonitrile-0.1% acetic acid in water(60∶ 40,v/v) and the flow rate was 0.2 mL·min^-1.Detection was performed with multiple reactions monitoring(MRM) using positive electrospray ionization(ESI). Results: The calibration curve was linear over the concentration range of 0.1-100 ng·mL^-1.The lower limit of quantification was 0.1 ng·mL^-1.Inter-and intra-day precision were less than 15% and accuracy was within 85%-115%.Extraction recoveries were around 70%-80% and the analytes were proved to be stable. Conclusion: This method is rapid,sensitive and specific,and applicable to the pharmacokinetic study of aripiprazole in humans.