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目的建立高效液相色谱-质谱联用法测定人血浆中克唑替尼的质量浓度。方法用蛋白沉淀法处理血浆,色谱柱:Aglient ZORBAX XDB-C8柱,流动相:甲醇-0.1%甲酸+2 mmol·L~(-1)甲酸铵,梯度洗脱,流速:0.35 m L·min~(-1),柱温:室温,用正离子扫描,多反应监测方式测定样品中药物的质量浓度。考察该方法的专属性、标准曲线与定量下限、精密度与回收率、基质效应和稳定性。结果血浆样品中克唑替尼的回归方程为y=3.91×10-3x+1×10-3(r=0.999 4);克唑替尼在5～1000 ng·mL~(-1)内线性关系良好,最低定量下限为5 ng·mL~(-1)。血样日内与日间RSD均小于15%,平均回收率>95%,且稳定性较好。结论本方法简便快速、灵敏准确、特异性强,适用于人体克唑替尼血药浓度的测定。
Objective To establish a method for the determination of crizotinib in human plasma by high performance liquid chromatography-mass spectrometry. Methods The plasma was treated with protein precipitation method. The column was Aglient ZORBAX XDB-C8. The mobile phase consisted of methanol-0.1% formic acid and 2 mmol·L -1 ammonium formate with a gradient of 0.35 mL · min ~ (-1), column temperature: room temperature, with positive ion scan, multi-reaction monitoring method to determine the mass concentration of the drug samples. Investigate the specificity of this method, the standard curve and lower limit of quantitation, precision and recovery, matrix effect and stability. Results The regression equation of crizotinib in plasma samples was y = 3.91 × 10-3x + 1 × 10-3 (r = 0.999 4). The crizotinib was linear within 5-1000 ng · mL -1 The relationship was good, with the lowest limit of quantification being 5 ng · mL -1. The RSDs were less than 15% and the average recovery was> 95%. The stability was better. Conclusion This method is simple and rapid, sensitive and accurate, specific and suitable for the determination of human plasma concentration of crizotinib.