HPLC-MS/MS法测定人血浆中奎硫平浓度的方法学研究

HPLC-MS/MS determination of quetiapine in human plasma

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 develop an HPLC MS/MS method for determination of quetiapine in human plasma. Methods：The plasma proteins were precipitated by acetonitrile directly. The separation was performed on a Thermo Hypurity C18（2. 0 mm × 150 mm,5 μm）analytical column using acetonitrile（0. 1% formic acid） -0. 1% formic acid（80： 20）as the mobile phase at a flow rate of 0. 2 mL · min^-1. The analyses were detected by the electronic - spray ionization（ESI） -multiple reaction monitoring （MRM）mode. The MS detection parameters were as follows： the capillary voltage was 3.5 kV, source temperature was 100℃ , desolation temperature was 200℃ ,cone gas flow was 50 L · h^-1 and desolation flow was 350 L · h^-1. Results：The linear range of the plasma concentration of quetiapine was 1. 764 - 1806 ng · mL^-1 and limit of detection was 0. 88 ng · mL^-1. The method recovery was 94. 1% - 104. 8%. The extractive recovery of quetiapine was 68.0% - 72. 3%. The RSDs of intra - day and inter - day were less than 10% and 15 %, respectively. Conclusion：The method has high sensitivity and good selectivity,it can be used for the pharmacokinetic research of quetiapine.