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目的:建立一种快速灵敏测定人体血浆中度洛西汀浓度的高效液相色谱串联质谱法。方法:以AgilentC18(4.6mm×150mm,5μm)为色谱柱;流动相为甲醇-0.005mol.L-1甲酸铵水溶液(90:10);流速:0.8mL.min-1;柱温:30℃。采用选择反应监测(SRM)对度洛西汀(m/z297.9→156.7)和内标地西泮(m/z285.1→154.0)进行测定。结果:度洛西汀高、中、低(50,25,1μg.L-1)3个浓度的平均回收率RSD均小于15%;线性范围为:0.5～60μg.L-1,回归方程为F=0.0146C+9.4714×104,r=0.996(n=8),权重系数为1/C2,分析方法的最低定量限为0.5μg.L-1。结论:该方法灵敏、准确、简单、快速,可用于度洛西汀临床血药浓度监测和药动学研究。
Objective: To establish a rapid and sensitive HPLC method for the determination of duloxetine in human plasma by high performance liquid chromatography-tandem mass spectrometry. Method: The column was Agilent C18 (4.6 mm × 150 mm, 5 μm); the mobile phase was methanol-0.005 mol·L-1 ammonium formate (90:10); the flow rate was 0.8 mL.min-1; . Duloxetine (m / z 297.9 → 156.7) and internal standard diazepam (m / z 285.1 → 154.0) were measured using selective reaction monitoring (SRM). Results: The RSDs of duloxetine at high, medium and low concentrations (50,25 and 1μg.L-1) were less than 15% and the linear range was 0.5-60μg.L-1. The regression equation was F = 0.0146C + 9.4714 × 104, r = 0.996 (n = 8), the weight coefficient is 1 / C2, and the lowest limit of quantitation of the analytical method is 0.5μg.L-1. Conclusion: The method is sensitive, accurate, simple and rapid and can be used to monitor the clinical drug concentration and pharmacokinetics of duloxetine.