LC-MS法测定人血浆中氯雷他定浓度

目的:建立以液-质联用法测定人血浆中氯雷他定的方法。方法:血浆样品中加入内标地西泮,用液相萃取法处理后测定,色谱柱为AgilentTC-C18,流动相为乙腈(含1%甲酸)-0.02mol·L-1甲酸铵水溶液(90∶10),流速为0.8mL·min-1,柱温为40℃。通过电喷雾电离源(ESI),质谱在正离子多反应监测模式(MRM)下行特征母-子离子对信号采集,以m/z383.2→337.0(氯雷他定)和m/z285.1→154.0(地西泮)进行定量分析。结果:氯雷他定检测浓度在0.5~100μg·L-1范围内线性关系良好(r=0.9960),定量下限为0.5μg·L-1;提取回收率在61.15%~67.11%之间,日内、日间RSD均≤16.54%。结论:本方法简便、灵敏,适用于人体内氯雷他定血药浓度测定及临床药动学研究。

Determination of Loratadine in Human Plasma by LC-MS

OBJECTIVE： To establish an LC- MS method for the determination of loratadine in human plasma. METHODS： The plasma sample was treated by liquid phase extraction, with diazepam as the internal standard, The separation of sample was performed on an Aglient TC - C18 column with a column temperature of 40℃. The mobile phase consisted of acetonitrile （including 1% methanoic acid） -0.02 mol·L^-1 ammonium formate aq sol （90 ： 10） at a flow rate of 0.8 mL ·min^-1. Loratadine was detected by LC - MS under positive electrospray ionization MRM mode. The quantification was performed based on the peak intensity of fragment ion m/z 383.2→337.0 （loratadine） and m/z 285.1→154.0 （diazepam） . RESULTS： The linear regression curve was obtained in the range of 0.5-100 μg · L^-1 for loratadine（ r = 0.996 0） . The lower quantification limit was 0.5 μg · L^-1. The extraction recovery rate stood at 61.15% -67.11%. Both intra- day RSD and inter-day RSD were no more than 16.54% （n = 5）. CONCLUSION： This method is simple, sensitive and suitable for the determination of and clinical pharmacokinetic study of loratadine.