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目的建立HPLC-MS/MS法测定人血浆中米那普仑的质量浓度。方法用简单的蛋白沉淀法处理血浆,色谱柱:ZORBAX SB-Aq柱(2.1 mm×50 mm,3.5μm),流动相:甲醇-0.01%甲酸,梯度洗脱,流速:0.4 mL·min~(-1),柱温:20℃,用正离子扫描,多反应监测方式测定样品中药物的质量浓度。考察该方法的专属性、标准曲线与定量下限、精密度及回收率、基质效应和稳定性。结果血浆样品中,米那普仑在2.0~500.0 ng·mL~(-1)线性关系良好(r>0.999 8),定量下限为2.0 ng·mL~(-1)。血样日内与日间相对标准偏差(RSD)均小于15%,平均回收率>96%,且稳定性均较好。结论本方法简便快速、灵敏准确、特异性强,适用于测定人血浆中米那普仑的浓度。
Objective To establish a HPLC-MS / MS method for the determination of milnacipran in human plasma. Methods The plasma was treated with a simple protein precipitation method. The column was on a ZORBAX SB-Aq column (2.1 mm × 50 mm, 3.5 μm). The mobile phase consisted of methanol-0.01% formic acid and eluted with a gradient of 0.4 mL · min ~ -1), column temperature: 20 ℃, with positive ion scanning, multi-reaction monitoring method for the determination of the quality of the drug samples. Investigate the specificity of this method, the standard curve and lower limit of quantitation, precision and recovery, matrix effect and stability. Results The plasma concentration of milnacipran had good linearity (r> 0.999 8) at a concentration of 2.0-500.0 ng · mL -1, and the lower limit of quantification was 2.0 ng · mL -1. The relative standard deviations (RSDs) of intra-day and inter-day blood samples were less than 15%, and the average recovery was> 96%. The stability was good. Conclusion This method is simple, rapid, accurate, sensitive and specific. It is suitable for the determination of milnacipran in human plasma.