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目的:建立一种人血浆中三环类抗抑郁药的液相色谱-串联质谱方法。方法:血浆中的三环类抗抑郁药用醋酸乙酯提取,采用Zorbax SB-C18(2.1 mm×50 mm,3.5μm)柱,柱温35℃,流速0.3 mL.min-1,流动相为甲醇-0.1%甲酸。梯度洗脱,0min,10%甲醇;1 min,80%甲醇;5.5 min,80%甲醇;6 min,10%甲醇;8 min,运行完成,进样量5μL。ESI(电喷雾离子源),正离子检测,MRM模式,雾化气压力设为20 psi;干燥气(N2)流速设为6 L.min-1,干燥气温度设为350℃,采用多反应监测(multiple reaction monitoring,MRM)方式进行定量分析。结果:5种三环类抗抑郁药物的质量浓度在10～800 ng.mL-1范围内线性良好(r≥0.990 2),平均萃取回收率在60.4%以上,日内、日间精密度RSD≤12%。结论:该方法专属性强、灵敏及准确,可以适用于临床药物分析。
Objective: To establish a liquid chromatography tandem mass spectrometry method for tricyclic antidepressants in human plasma. Methods: Tricyclic antidepressants in plasma were extracted with ethyl acetate. The column was on a Zorbax SB-C18 (2.1 mm × 50 mm, 3.5 μm) column at 35 ℃ with a flow rate of 0.3 mL · min-1. The mobile phase was Methanol -0.1% Formic acid. Gradient elution, 0 min, 10% methanol; 1 min, 80% methanol; 5.5 min, 80% methanol; 6 min, 10% methanol; ESI (electrospray ionization), positive ion detection, MRM mode, atomizing gas pressure set to 20 psi; drying gas (N2) flow rate set to 6 L.min-1, drying gas temperature set to 350 ° C, Multiple reaction monitoring (MRM) was used for quantitative analysis. Results: The five tricyclic antidepressants had a good linearity (r ≥0.9902) in the range of 10 to 800 ng · mL-1 and the average extraction recovery was over 60.4%. The intra-day and inter-day precision RSD ≤ 12%. Conclusion: The method is specific, sensitive and accurate and can be applied to clinical drug analysis.