液相色谱-串联质谱（LC-MS/MS）法测定他克莫司胶囊的含量___

摘要 目的：建立液相色谱-串联质谱（LC-MS/MS）法测定他克莫司胶囊中他克莫司的含量。方法:他克莫司胶囊内容物经乙腈超声提取，氮气吹干流动相复溶进样，色谱柱：Zorbax Extend-C18 柱（150 mm×4.6 mm，5 μm） 流动相：甲醇-乙腈-20 mmol•L-1醋酸铵溶液（80∶15∶5，v/v/v） 流速：0.4 mL•min-1。采用电喷雾离子化四极杆串联质谱，多反应检测方式测定样品的浓度。检测离子对分别为m/z 821.7→768.4和m/z 821.7 →786.5。结果：他克莫司浓度在0.437~280 ng•mL-1范围内，与峰面积线性关系良好（r=0.9999，n=5），平均回收率(n=15)为99.4%，日内精密度、日间精密度的RSD分别为4.0%和1.8% 3批样品中他克莫司的含量分别为95.6%，98.9%，97.4%。结论：本方法具有良好的灵敏度、准确度、精确度及专属性，结果准确，重现性好，易于操作，可用于制剂中他克莫司含量的测定。
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Abstract Objective:To develop an LC-MS/MS method for the content determination of tacrolimus capsules.Methods:The analysis was isolated from tacrolimus capsules by acetonitrile with ultrasound extraction.The supernatant was evaporated to dryness and reconstituted with the mobile phase,then 10 μL was injected for analysis.A Zorbax Extend-C18(150 mm×4.6 mm，5 μm ) was adopted with mobile phase of methanol-acetonitrile-20 mmol•L-1 ammonium acetate(80∶15∶5，v/v/v) at a flow rate of 0.4 mL•min-1.Electrospray ionization (ESI) sources was applied and operated in the position ion mode.Multiple reaction monitoring (MRM) mode with the transition of m/z 821.7→768.4 and m/z 821.7→786.5 were used to quantify tacrolimus.Results:The method was proved to be linear in the range of 0.437-280 ng•mL-1 with a regression coefficient of 0.9999 (n=5).The lower quantitative limit was 0.437 ng•mL-1.The average recovery rate was 99.4%(n=15).The RSDs of average contents of intra-day and inter-day were 4.0% and 1.8% respectively.Conclusion:This method is accurate,precise,sensitive and specific to be used in the content determination of tacrolimus capsules.