液相色谱-串联质谱法测定人血浆中卡维地洛的浓度

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。

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

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 C_(18)Ⅲcolumn (100.0 mm×2.0 mm,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 8μL.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 200μg·L~(-1) (r>0.999) and the low limit of quantitation was 0.2μg·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.