论文部分内容阅读
目的:建立测定人血浆中左舒必利浓度的方法。方法:血浆样品经乙腈沉淀蛋白后,采用液相-串联质谱(LC-MS/MS)法测定血浆样品中左舒必利浓度,以吡格列酮为内标,以正离子多反应监测(MRM)扫描方式进行检测。用于定量的离子为m/z342.1→112.1(左舒必利)和m/z357.1→134.0(吡格列酮)。色谱柱为Capcell Pak CR(2.0mm×150 mm,5μm),流动相为乙腈-20 mmol·L-1醋酸铵(含0.3%甲酸)(65∶35)。结果:血浆中左舒必利的线性范围为3~4 000 ng·ml-1,定量限为3 ng·ml-1,批内RSD≤4.94%,批间RSD≤5.93%,准确度(RE)在-6.48%~3.42%之内,平均相对回收率在93.52%~103.42%之间。结论:该方法专属性强、灵敏度高、重复性好,符合血浆样品测定的要求,适用于人体血浆中左舒必利浓度的测定和药动学考察。
Objective: To establish a method for the determination of the concentration of zusulpride in human plasma. Methods: Plasma samples were pretreated with acetonitrile and analyzed by liquid chromatography-tandem mass spectrometry (LC-MS / MS). The concentration of plasma was determined by pioglitazone and positive ion MRM (scanning electron microscopy) Detection. The ions for quantitation were m / z 342.1-> 112.1 (levosulpiride) and m / z 357.1- 134.0 (pioglitazone). The column was Capcell Pak CR (2.0 mm × 150 mm, 5 μm). The mobile phase was acetonitrile-20 mmol·L-1 ammonium acetate (containing 0.3% formic acid) (65:35). Results: The linear range of plasma concentration was 3-4000 ng · ml-1, the limit of quantification was 3 ng · ml-1, the intra-assay RSD≤4.94%, the inter-assay RSD≤5.93% and the accuracy (RE) -6.48% ~ 3.42%, the average relative recovery was between 93.52% ~ 103.42%. Conclusion: This method is specific, sensitive and reproducible. It meets the requirements of plasma sample determination and is suitable for the determination of human plasma and its pharmacokinetic study.