液相色谱-串联质谱法测定人血清中苯磺酸氨氯地平的浓度

目的:建立测定体内苯磺酸氨氯地平的液相色谱-串联质谱(LC-MS/MS)方法。方法:血清样品中加入内标苯海拉明,直接沉淀蛋白法处理样品。色谱柱为Atlantis C_(18)(100 mm×2.1 mm,3μm),流动相为含0.1%甲酸的乙腈-0.1%甲酸水溶液(42:58,V:V),流速为0.25 mL·min~(-1)。MRM扫描分析,苯磺酸氨氯地平和内标苯海拉明的离子通道分别选择为m/z 409.1→238.1和256.3→167.0。结果:苯磺酸氨氯地平的线性范围为0.2～32μg·L~(-1),最低定量限为0.2μg·L~(-1),提取回收率均大于95%,日内、日间RSD均小于15%。结论:本方法灵敏、准确、专一、操作简便,适用于苯磺酸氨氯地平的体内药动学研究。

Determination of amlodipine besylate in human serum by LC-MS/MS method

AIM:To develop a LC-MS/MS method for determination of amlodipine besylate in human serum.METHODS:After addition of diphenhydramine(internal standard,IS),the analyte was isolated by protein precipitation.The chromatographic separation was performed on Atlantis C_(18)(100 mm×2.1 mm,3μm) column with a mobile phase of 0.1% formic acid acetonitrile-0.1% formic acid water(42:58,V:V)at a flow rate of 0.25 mL·min~(-1).The deprotonated ion of analyte was detected in negative ionization by multiple reaction monitoring mode(MRM).The mass transition pairs of m/z 409.1→238.1 and m/z 256.3→167.0 were used to detect amlodipine besylate and internal standard,respectively.RESULTS:The calibration curves were linear over the ranges of 0.2-32μg·L~(-1).The lower limit of quantification was 0.2μg·L~(-1).The extraction recovery was more than 95%.The intra-day RSD and inter-day RSD were less than 15%.CONCLUSION:The method is sensitive,accurate,convenient and suitable for the pharmacokinetic study of amlodipine besylate tablets.