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目的建立测定人血浆中咪达普利拉浓度的固相萃取高效液相串联质谱电喷雾检测法(SPE-LC-ESI-MS/MS)。方法以美国Agilent Eclipse plus C18(4.6 mm×150 mm,3.5μm)为色谱柱,流动相为甲醇-水(含0.005 mol.L-1甲酸铵,含0.1%甲酸)(87∶13);流速:0.5 mL.min-1;柱温:40℃。样品用Agilent C8固相小柱净化。经电喷雾离子源正离子化后,通过三重四级杆串联质谱仪,采用选择反应监测(SRM)对咪达普利拉(m/z 378.2→206.2)和内标依那普利拉(m/z 349.1→206.1)进行测定。结果咪达普利拉的高(20μg.L-1)、中(10μg.L-1)、低(1μg.L-1。)3个质量浓度的方法回收率分别为102.44%,102.46%和105.69%,日内(n=5)、日间(n=3)RSD均小于15%;分析方法的最低定量限为0.5μg.L-1。线性范围为0.5～25μg.L-1,回归方程为y=0.480 7x+0.008 7×10-4,r=0.997 6(n=6)。结论该方法灵敏、准确、简单、快速,可用于临床血药浓度监测和药动学研究。
Objective To establish a SPE-LC-ESI-MS / MS method for the determination of imidapril in human plasma by high performance liquid chromatography-tandem mass spectrometry (ESI-MS / MS). Methods The mobile phase consisted of methanol-water (containing 0.005 mol·L-1 ammonium formate containing 0.1% formic acid) (87:13) with Agilent Eclipse plus C18 (4.6 mm × 150 mm, : 0.5 mL.min-1; column temperature: 40 ° C. The sample was purified with an Agilent C8 cartridge. Electrospray ionization (ESI) ionization was used to determine the effect of imidapril (m / z 378.2 → 206.2) and the internal standard enalaprilat (m / z 349.1 → 206.1). Results The recoveries of imidacloprid were 102.44% and 102.46% for the three concentrations of 20μg.L-1, 10μg.L-1 and 1μg.L-1, respectively 105.69%, intraday (n = 5), daytime (n = 3) RSD were less than 15%, and the lowest limit of quantitation was 0.5μg.L-1. The linear range was 0.5 ~ 25μg.L-1, the regression equation was y = 0.480 7x + 0.008 7 × 10-4, r = 0.997 6 (n = 6). Conclusion The method is sensitive, accurate, simple and rapid, which can be used for clinical blood drug concentration monitoring and pharmacokinetic studies.