液相色谱-质谱法测定人血浆中的甲哌卡因

Determination of mepivacaine in human plasma by LC-MS/MS

目的建立灵敏、快速液相色谱-串联质谱法测定人血浆中甲哌卡因的浓度,并用于人体药动学研究。方法 200μL的血浆样品经甲基叔丁基醚提取处理后,以10 mmol.L-1醋酸铵(含0.5%甲酸)水溶液-乙腈(60∶40,v/v)为流动相,Inertsil CN柱分离,通过电喷雾离子源四极杆串联质谱,以多反应监测(MRM)的方式进行检测,选择离子反应为m/z 247.2→98.0(甲哌卡因)和m/z 235.2→86.0(利多卡因)。结果甲哌卡因在0.500～1 500 ng.mL-1线性关系良好,定量下限为0.500 ng.mL-1,日内、日间精密度(RSD)均≤10.1%,甲哌卡因和内标利多卡因的提取回收率分别为64.6%～67.4%和64.5%。结论该法选择性强、灵敏度高,适用于人血浆中甲哌卡因的浓度测定。

Objective To establish an LC-MS/MS method for the determination of mepivacaine in human plasma,and the pharmacokinetic study in human.Methods Plasma samples treated with methyl tert-butyl ether（MTBE）extraction were separated on the Inertsil CN column with a mobile phase of 10 mmol·L-1 ammonium acetate（containing 0.5 % formic acid）-acetonitrile（60 ：40,v/v）.The detection was carried out by electrospray ionization mass spectrometry in a positive ion mode.Multiple reaction monitoring mode was used with the transition of m/z 247.2→98.0 for mepivacaine and m/z 235.2→86.0 for the internal standard.Results The calibration curve of mepivacaine was linear at 0.500 0-1 500 ng ？ mL-1.The limit of quantification was 0.500 0 ng ？ mL-1.The extraction recovery of valsartan was 64.6%-67.4%,and that of the internal standard was 64.5%.The intra-and inter-day RSDs were less than 10.1%.Conclusion The method is simple,accurate,sensitive and specific for the determination of mepivacaine in human plasma.