为了快速、准确地检测人血浆中氨氯地平的浓度,建立了高效液相色谱-质谱联用检测方法.选用Eclipse XDB-C18色谱柱,以甲醇-1 mM乙酸铵溶液-0.1％甲酸溶液为流动相,采用梯度洗脱方法进行分离,样品经乙腈沉淀后进样,选用3200Q-trap型质谱仪的多重反应监测(MRM)扫描方式进行检测.氨氯地平线性范围为0.100～20.000μg/L,定量下限为0.100μg/L.准确度与精密度结果显示:方法日间、日内变异均小于15％,相对偏差为-3.85％～1.94％,低、中、高3个浓度提取回收率为94.90％～97.84％,稳定性好.该方法专属性强、样品处理简便、灵敏度高,可用于人体氨氯地平血药浓度的测定及其制剂的人体药代动力学研究.%LC-MS/MS method was established for determination of amlodipine in human plasma. After protein precipitation of acetonitrile, the plasma sample was separated on an Eclipse XDB-C18 column using methanol -1 mM ammonium acetate-0. 1 % formic acid as mobile phase by gradient elution. Detection was carried out by multiple reaction monitoring (MRM) on a 3200 Q-trap LC-MS/MS system. The assay was linear over the range 0.100— 20. 000 μg/L with a lower limit of quantitation of 0.100 μg/L. Intra-day and inter-day precision were less than 15%, respectively. The relative deviation was in the range —3. 85%— 1. 94%. The recovery of amlodipine was in the range 94. 90%—97. 84%. The method is a rapid, sensitive, selective and reliable method for the determination of amlodipine in human plasma. The assay can be applied for the determination of amlodipine in human plasma and the study on pharmacokinetics of its preparation.
展开▼
