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目的:建立测定人血浆中美利曲辛浓度的高效液相串联质谱法(HPLC-MS/MS),用于氟哌噻吨美利曲辛片的生物等效性研究。方法:以Agilent ZORBAX Eclipse Plus C1(84.6mm×150mm,5μm)为色谱柱,流动相为乙腈(含1%甲酸):0.02mo·L-1甲酸铵水溶液(80:20,V:V),流速:0.8mL·min-1;柱温:40℃,以醋酸乙酯:二氯甲烷(4:1,V:V)为提取剂。样品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)对美利曲辛(m/z292.2→232.2)和阿米替林(m/z278.1→91.0)进行测定。结果:美利曲辛的高(50μg·L-1)、中(20μg·L-1)、低(0.5μg·L-1)3个浓度的平均回收率分别为97.53%、104.03%和106.87%,日内(n=5)、日间(n=3)RSD均小于15%;分析方法的最低定量限为0.2μg·L-1。线性范围为:0.2~60μg·L-1,回归方程为:F=1.8691ρ+0.0555,r=0.9986(n=9),权重为1/ρ2。结论:该方法灵敏、准确、简单、快速,可用于临床血浓监测和药动学研究。
OBJECTIVE: To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of the concentration of melitracen in human plasma for the bioequivalence study of flupenthixol and melitracen tablets. Methods: Agilent ZORBAX Eclipse Plus C1 (84.6 mm × 150 mm, 5 μm) was used as the mobile phase. The mobile phase consisted of acetonitrile (containing 1% formic acid): 0.02 mol·L-1 ammonium formate (80:20, V: V) Flow rate: 0.8mL · min-1; column temperature: 40 ℃, with ethyl acetate: dichloromethane (4: 1, V: V) as extractant. The sample was ionized by electrospray ionization (ESI) source and was analyzed by triple quadrupole mass spectrometry with selective reaction monitoring (SRM) for the presence of melitracen (m / z 292.2 → 232.2) and amitriptyline .1 → 91.0). Results: The average recoveries of the three concentrations of metyrapicin at the concentrations of 50μg · L-1, 20μg · L-1 and 0.5μg · L-1 were 97.53%, 104.03% and 106.87, respectively %, Day (n = 5), daytime (n = 3) RSD were less than 15%. The lowest limit of quantification was 0.2μg · L-1. The linear range was 0.2 ~ 60μg · L-1, the regression equation was: F = 1.8691ρ + 0.0555, r = 0.9986 (n = 9), weight was 1 / ρ2. Conclusion: The method is sensitive, accurate, simple and rapid and can be used in clinical blood concentration monitoring and pharmacokinetic studies.