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目的建立人体全血中五氟利多浓度的液相色谱-质谱联用法(LC-MS/MS)分析方法。方法全血中五氟利多和利培酮(内标)经正己烷液-液提取后,采用Capcell Pak C18色谱柱(250mm×2.0mm5,μm)进行分离,流动相为乙腈:20mmol/L乙酸胺和0.1%甲酸溶液(75∶25,V/V),流速为0.2mL/min,然后以MS/MS电喷雾正电离的多反应监测扫描方式(MRM)测定。用于定量分析的离子为m/z 524→109(五氟利多)和m/z 411→191(内标)。结果五氟利多的最低检测限为0.2ng/mL,在0.4～400ng/mL浓度范围内线性良好(r=0.9994),低、中、高浓度(1ng/mL、10ng/mL、100ng/mL)准确度分别为97%,108%和95%,日内和日间RSD均小于15%。结论该方法简便、快速、灵敏,适用于全血中五氟利多浓度的测定。
Objective To establish a liquid chromatography-mass spectrometry (LC-MS / MS) method for the determination of pentaflumidin in human whole blood. Methods The whole blood was treated with liquid-liquid extraction of pentafluidomide and risperidone (internal standard), and then separated on a Capcell Pak C18 column (250 mm × 2.0 mm 5, μm). The mobile phase consisted of acetonitrile: 20 mmol / L acetic acid Amine and 0.1% formic acid solution (75:25, V / V) at a flow rate of 0.2 mL / min and then by multiple reaction monitoring scan mode (MRM) using MS / MS electrospray positive ionization. The ions used for the quantitative analysis were m / z 524 → 109 (pentafluoride) and m / z 411 → 191 (internal standard). Results The detection limit of pentaflumidin was 0.2 ng / mL. The linearity was good (r = 0.9994), low, middle and high concentration (1 ng / mL, 10 ng / mL and 100 ng / mL) in the range of 0.4-400 ng / The accuracy was 97%, 108% and 95%, respectively, with intraday and daytime RSDs less than 15%. Conclusion The method is simple, rapid and sensitive and suitable for the determination of pentaflumidin in whole blood.