LC-MS/MS法测定人血浆中阿折地平的浓度

Determination of Content of Azelnidipine in Human Plasma by LC-MS/MS

目的：建立测定人血浆中阿折地平浓度的方法。方法：人血浆样本经乙腈沉淀蛋白后采用液相色谱-串联质谱（LC-MS/MS）法进样测定,色谱柱为Zorbax Eclipse XDB-C18,流动相为甲醇-10 mmol/L乙酸铵（含1%甲酸）（80∶20,V/V）。选用多重反应监测扫描方式进行质谱监测,监测离子反应分别为m/z 583.3→167.1（阿折地平）、m/z 285.1→154.0（内标地西泮）。结果：阿折地平的血药浓度在0.05~40 ng/ml范围内线性关系良好,定量下限为0.05 ng/ml。日内、日间RSD分别为3.01%~7.75%,0.99%~12.08%;平均提取回收率为110.20%~111.99%。结论：该方法简便、快速、灵敏、专属性强、重现性好,适用于人血浆中阿折地平浓度的测定。

OBJECTIVE：To establish a method for the content determination of azelnidipine. METHODS：Plasma samples were processed by protein precipitation and determined by LC-MS/MS. Chromatography was performed on a Zorbax Eclipse XDB-C18 column using mobile phases of methanol-10 mmol/L ammonium acetate（containing 1% formic acid）（80∶20,V/V）. The MS detection was used multiple reaction monitoring mode with MS/MS ion transitions at m/z 583.3→167.1（azelnidipine）and m/z285.1→154.0（internal standard diazepam）. RESULTS：There was a good relationship of blood concentration in the range of0.05-40 ng/ml in plasma with the lower limit of quantitation of 0.05 ng/ml. The RSD of intra- and inter-day was 3.01%-7.75%,0.99%-12.08%,respectively. The extraction recovery was 110.20%-111.99%. CONCLUSIONS：This is a rapid,sensitive,selective and reliable method for the determination of azelnidipine in human plasma.