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目的:建立人血浆中奎硫平测定的 HPLC-MS/MS 法。方法:血浆蛋白用乙腈直接沉淀。采用 Thermo Hypurity C_(18)(2.0mm×150 mm,5μm)分析柱,以乙腈(含1%甲酸)-1%甲酸水溶液(80:20)为流动相,流速为0.2 mL·min~(-1);采用 ESI~+MRM进行离子方式监测。质谱检测参数:源电压3.5 kV,源温度100℃,去溶剂化温度200℃,锥孔气流速50 L·h~(-1),去溶剂化气流速350 L·h~(-1)。结果:血浆中奎硫平检测方法的线性范围为1.764～1806 ng·mL~(-1),最低检测限为0.88 ng·mL~(-1)。方法回收率为94.1%～104.8%,提取回收率均值为68.0%～72.3%,日内 RSD 小于10%,日间 RSD 小于15%。结论:本方法灵敏、准确,可用于奎硫平的药代动力学研究。
Objective: To establish a HPLC-MS / MS method for the determination of quetiapine in human plasma. Methods: Plasma proteins were precipitated directly with acetonitrile. The mobile phase consisted of acetonitrile (containing 1% formic acid) and 1% formic acid (80:20) at a flow rate of 0.2 mL · min ~ (-1) using a Thermo Hypquis C 18 (2.0 mm × 150 mm, 1). The ion mode was monitored by ESI ~ + MRM. MS detection parameters: source voltage of 3.5 kV, source temperature of 100 ℃, desolvation temperature of 200 ℃, cone flow rate of 50 L · h ~ (-1) and desolvation flux of 350 L · h ~ (-1). Results: The calibration curve of quetiapine in plasma ranged from 1.764 to 1806 ng · mL -1 with the detection limit of 0.88 ng · mL -1. The method recoveries ranged from 94.1% to 104.8%. The mean recovery rates ranged from 68.0% to 72.3%. The intraday RSD was less than 10% and the intraday RSD was less than 15%. Conclusion: The method is sensitive and accurate and can be used to study the pharmacokinetics of quetiapine.