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目的:建立液质联用法测定人全血中他克莫司的浓度。方法:采用HPLC-MS/MS法进行分析。血样处理:采用乙腈沉淀蛋白。色谱柱为Waters TDMC18(5μm,10mm×2.1mm)柱,柱温55℃,流动相A为10mmol·L-1醋酸铵-0.5%甲酸水溶液,流动相B为0.5%甲酸甲醇溶液,流速0.25mL.min-1,采用多反应监测进行定量,采用ESI正离子方式进行检测,用于定量分析的监测离子为m/z821.30→768.20(他克莫司)和m/z809.35→756.35(内标子囊霉素)。结果:本方法线性范围为1～30ng·mL-1(r=0.9996),相对回收率在80%～120%之间,日内、日间RSD均小于10%。结论:本方法经济、简便、灵敏,用于他克莫司血药浓度监测,并进行在肝移植早期患者的药代动力学研究。
Objective: To establish a method for the determination of tacrolimus in human whole blood by liquid chromatography-mass spectrometry. Methods: The HPLC-MS / MS method was used for the analysis. Blood sample processing: Precipitation of protein with acetonitrile. The column was Waters TDMC18 (5μm, 10mm × 2.1mm) with a column temperature of 55 ℃, mobile phase A was 10mmol·L -1 ammonium acetate-0.5% formic acid aqueous solution, mobile phase B was 0.5% formic acid methanol solution, .min-1, using multiple reaction monitoring for quantification, ESI positive ion detection, for the quantitative analysis of the monitoring ions m / z821.30 → 768.20 (tacrolimus) and m / z809.35 → 756.35 Internal standard ascomycin). Results: The linear range of this method was 1 ~ 30 ng · mL-1 (r = 0.9996). The relative recoveries ranged from 80% to 120%. The intra-day and inter-day RSD were less than 10%. Conclusion: The method is economical, simple and sensitive for the monitoring of tacrolimus plasma concentration and pharmacokinetics study in the early stage of liver transplantation.