液相色谱-串联质谱法测定人血浆中卡维地洛的浓度  

Determination of carvedilol in human plasma by LC-MS/MS method

作　　者：张梦琪 周秀锦 陆川 陆晓佩 刘罡一 贾晶莹 刘昀 余琛 

机构地区：[1]徐汇区中心医院中心实验室,上海200031 [2]舟山出入境检验检疫局,浙江舟山316000 [3]上海医药临床研究中心分析化学部,上海200233

出　　处：《中国新药与临床杂志》2011年第7期533-536,共4页Chinese Journal of New Drugs and Clinical Remedies

基　　金：上海市科委科研计划项目(08411966700)

摘　　要：目的建立测定血浆中卡维地洛的液相色谱-串联质谱(LC-MS/MS)方法。方法血浆样品中加入内标氘3-卡维地洛,直接沉淀法处理样品。色谱柱为CAPCELL PACK C_(18)Ⅲ(100.0mm×2.0mm,5μm),流动相为含0.1%甲酸的水溶液-含0.1%甲酸的乙腈溶液(70:30,V/V),流速0.5mL·min^(-1),等度洗脱,进样体积8μL,正离子多离子反应监测(MRM)扫描分析,离子通道分别为m/z 407.3→100.1(卡维地洛),m/z 410.3→100.1(氘3-卡维地洛)。结果卡维地洛线性范围为0.2～200μg·L^(-1)(r>0.999),定量下限为0.2μg·L^(-1),提取回收率在92.27%～104.0%,日内、日间精密度RSD均小于8%。结论本方法操作简便,特异性强,灵敏度高,可适用于卡维地洛的药动学研究。AIM To establish a LC-MS/MS method for the determination of carvedilol in human plasma. METHODS After the addition of carvedilol-D3 （internal standards） , the plasma was processed by direct protein precipitation. The chromatographic separation was performed on a CAPCELL PACK C18Ⅲ column （（100.0mm×2.0mm,5μm） with a mobile phase of 0.1% formic acid solution- 0.1% formic acid acetonitrile （70 ： 30, V/V） at a flow rate of 0.5 mL·min^-1 in isocratic elution, and the injection volume was 8 μL. The protonated ions of analytes were detected in positive ionization in multiple reaction monitoring mode （MRM）. The mass transition pairs of m/z 407.3→100.1 and 410.3→100.1 were used to detect carvedilol and carvedilol-D3, respectively. RESULTS The calibration curve was linear over a concentration range of 0.2 to 200 μg·L^-1 （r 〉 0.999） and the low limit of quantitation was 0.2 μg·L^-1. The extraction recovery rates were ranged from 92.27% to 104.0%, within-day RSD and between-day RSD were less than 8%. CONCLUSION The method is simple and quick, with high specificity and sensitivity, and suitable for the research of carvedilol pharmacokinetics.

关 键 词：卡维地洛 血浆 色谱法 高压液相 串联质谱法 药动学 

分 类 号：R927.2[医药卫生—药学] R972.4