【摘要】 目的:建立测定人血浆中伏立康唑浓度的液相色谱-串联质谱联用法。方法:待测血浆0.5 mL经乙醚-二氯甲烷萃取,以甲醇-10 mmo.lL-1醋酸铵水溶液(80∶20)为流动相,流速为1.0 mL.min-1,液相色谱-串联质谱联用法多反应离子检测,正离子模式,用于定量分析的离子分别是伏立康唑m/z351.0→127.0[M+H+]和地西泮m/z285.8→193.3[M+H+]。结果:血浆中无干扰测定的内源性物质,每个样品分析时间小于5 min,线性范围为20.0~4 000 ng.mL-1,定量下限为20.0 ng.mL-1,批内、批间精密度均小于10%,提取回收率大于85%。结论:该法操作快速、简单、准确、灵敏度高,适用于临床药动学研究。更多还原

【Abstract】 Objective: To develop a sensitive and specific LC-MS-MS method for determination of voriconazole in human plasma.Methods: Voriconazole was extracted by diethyl ether and dichloromethane from human plasma,then separated on a C 18-column.The mobile phase consisted of methanol and 10 mmol ·L-1 ammonium acetate solution(80 ∶20) and the flow rate was 1.0 mL ·min-1.A mass spectrometer equipped with electrospray ionization source was used as detector and operated in the positive ion mode.In multiple reaction monitoring(MRM) mode,the ion combinations of m/z 351.0→127.0 and m/z 285.8→193.3 were used to qualify voriconazole and an internal standard(diazapam),respectively.Results: Chromatograms showed no endogenous interfering peaks in the respective blank human plasma samples.Each analysis was completed within 5 min.The calibration was linear in the concentration range within 20.0~4 000 ng ·mL-1,and quantitative limit was 20.0 ng ·mL-1.The intra-batch and inter-batch RSDs were less than 10%.The recovery of the extraction was more than 85%.Conclusion: The method is proved to be suitable for clinical investigation of voriconazole pharmacokinetics,which offers advantages of specificity,quickness and higher sensitivity over the previously reported methods.更多还原