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  

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

作　　者：顾洪安[1] 苗积康[1] 张曙华[1] 刘昀[1] 刘罡一[1] 陆川[1] 余琛[1] 

机构地区：[1]上海市徐汇区中心医院,上海200031

出　　处：《中国新药与临床杂志》2007年第10期737-740,共4页Chinese Journal of New Drugs and Clinical Remedies

摘　　要：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。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 C18 （100 mm × 2.1 mm, 3 μm） 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 0.2-32 μg. L^-1. The lower limit of quantification was 0.2 μg. 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.

关 键 词：氨氯地平 色谱法 高压液相 光谱法 质量 电喷雾电离 药动学 

分 类 号：R969.1[医药卫生—药理学] R972.4[医药卫生—药学]