人血浆中氯吡格雷及其活性代谢物的LC-MS/MS法测定  

Determination of Clopidogrel and Its Active Metabolite in Human Plasma by LC-MS/MS

作　　者：田溪[1] 杨秀岭[1] 张志清[1] 王淑梅[1] 董维冲 

机构地区：[1]河北医科大学第二医院药学部,河北石家庄050000

出　　处：《中国医药工业杂志》2016年第2期202-206,共5页Chinese Journal of Pharmaceuticals

基　　金：河北省科技计划项目(14277767D)

摘　　要：建立了液相色谱-串联质谱法测定人血浆中的氯吡格雷（1）及其活性代谢物（2）。以2-溴-3＇-甲氧基苯乙酮（MPB）作为衍生化试剂,以噻氯匹定（3）为内标,使用Diamonsil C_（18）色谱柱,流动相为乙腈∶1 mmol/L乙酸铵水溶液（含0.01%甲酸）（80∶20）。使用电喷雾电离源（ESI）,正离子模式、多反应监测（MRM）监测离子对m/z 322.2→m/z 212.0（1）、m/z 504.4→m/z 354.1（2）和m/z 264.2→m/z 154.1（3）。血浆中的1和2衍生物在0.53~52.50 ng/ml和2~200 ng/ml范围内线性关系良好,最低定量限（LLOQ）为0.53和2.00 ng/ml,日内和日间RSD均小于10%。A LC-MS/MS method was established for the determination of clopidogrel（1） and its active metabolite（2） in human plasma. 2-Bromo-1-（3-methoxyphenyl）ethanone（MPB） was used as a derivation agent. A Diamonsil C_（18） column was used, with the mobile phase of acentonitrile∶1 mmol/L ammonium acetate solution containing 0.01% formic acid（80∶20）, with ticlopidine（3） as the internal standard. An ESI source was applied in the multiple reaction monitoring（MRM） and positive ion mode, with transitions of m/z 322.2→m/z 212.0（1）, m/z 504.4→m/z 354.1（2 derivative） and m/z 264.2→m/z 154.1（3）, respectively. It was linear for 1 and 2（derivative） in the ranges of 0.53 —52.50 ng/ml and 2 — 200 ng/ml. Their LLOQs were 0.53 and 2.00 ng/ml, and the intra- and inter-day RSDs were both less than 10%.

关 键 词：氯吡格雷 活性代谢产物 液相色谱-串联质谱 测定 

分 类 号：R969[医药卫生—药理学] O657.72[医药卫生—药学]