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目的建立LC-MS/MS法同时测定人血浆中西酞普兰、米氮平、舍曲林和度洛西汀浓度。方法血浆样品用乙腈沉淀蛋白后,以替米沙坦为内标,选用Agilent Eclipse Plus-C_(18)(100 mm×2.1 mm,3.5μm)色谱柱,以乙腈-10 mmol·L~(-1)醋酸铵溶液(均含0.1%甲酸)为流动相梯度洗脱,梯度流速恒定为0.25 mL·min~(-1),柱温为30℃,进样量10μL,总分析时间为5 min,采用电喷雾离子化源,正离子方式,多反应监测(MRM)扫描方式进行监测。结果血浆中西酞普兰和米氮平的线性范围为0.50~100μg·L~(-1)(r>0.99),定量下限为0.50μg·L~(-1);舍曲林和度洛西汀的线性范围为0.20~50μg·L~(-1)(r>0.99),定量下限为0.20μg·L~(-1);方法回收率91.6%~109.2%;日内、日间RSD均<15%;提取回收率77.6%~92.6%,无明显基质效应。结论该方法快速、灵敏、准确,专属性强,重复性好,适用于临床测定血药浓度及药动学研究。
Objective To establish a LC-MS / MS method for the simultaneous determination of citalopram, mirtazapine, sertraline and duloxetine in human plasma. Methods Plasma samples were precipitated with acetonitrile and treated with telmisartan as an internal standard. The samples were separated on an Agilent Eclipse Plus-C_ (18) (100 mm × 2.1 mm, 3.5 μm) column with 10 mmol·L ~ 1) ammonium acetate solution (containing 0.1% formic acid) as the mobile phase. The gradient flow rate was constant at 0.25 mL · min -1, the column temperature was 30 ℃, and the injection volume was 10 μL. The total analysis time was 5 min , Using electrospray ionization source, positive ion mode, multiple reaction monitoring (MRM) scan mode for monitoring. Results The linear range of citalopram and mirtazapine in plasma was 0.50-100 μg · L -1 (r> 0.99) and the lower limit of quantitation was 0.50 μg · L -1. Sertraline and duloxetine The linear range was 0.20-50 μg · L -1 (r> 0.99). The lower limit of quantitation was 0.20 μg · L -1. The recovery rate was 91.6% -109.2%. The intra-day and interday RSD were all less than 15 %; Extraction recovery rate of 77.6% ~ 92.6%, no significant matrix effect. Conclusion The method is rapid, sensitive, accurate, specific and reproducible. It is suitable for the clinical determination of plasma concentration and pharmacokinetics.