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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(150mm×4.6mm,5μm);流动相:甲醇-乙腈-20mmol·L-1醋酸铵溶液(80∶15∶5,v/v/v);流速:0.4mL贾正平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/z821.7→768.4和m/z821.7→786.5。结果:他克莫司浓度在0.437～280ng·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。
Objective: To establish a method for the determination of tacrolimus in tacrolimus capsules by liquid chromatography-tandem mass spectrometry (LC-MS / MS). METHODS: The contents of tacrolimus capsule were extracted by acetonitrile and dried under nitrogen. The mobile phase consisted of Zorbax Extend-C18 column (150mm × 4.6mm, 5μm) L-1 ammonium acetate solution (80:15:5, v / v / v); flow rate: 0.4 mL Jia Zhengping min-1. Electrospray ionization quadrupole tandem mass spectrometry was used to determine the concentration of the sample. The detected ion pairs were m / z 821.7 → 768.4 and m / z 821.7 → 786.5, respectively. Results: The tacrolimus concentration ranged from 0.437 to 280 ng · mL-1 and had a good linear relationship with the peak area (r = 0.9999, n = 5). The average recovery was 99.4% (n = 15) The RSDs of daytime precision were 4.0% and 1.8%, respectively. The contents of tacrolimus in three batches were 95.6%, 98.9% and 97.4% respectively. Conclusion: The method has good sensitivity, accuracy, precision and specificity, accurate results, good reproducibility, easy to operate, can be used for the determination of the content of tacrolimus in the preparation.