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目的建立超高效液相色谱-质谱(UPLC-MS/MS)法测定血浆中伊马替尼浓度的方法。方法以卡马西平为内标,用蛋白沉淀前处理方法。色谱柱为ACQUITY UPLC BEH C_(18)(100 mm×2.1 mm,1.7μm),流动相为乙腈-0.1%甲酸水溶液(25∶75),流速为0.4 m L·min~(-1),正离子模式多反应监测(MRM)扫描分析,并考察专属性、标准曲线与定量下限、精密度与回收率、基质效应和稳定性。结果血浆中伊马替尼线性范围为0.1~20.0μg·m L~(-1)(r=0.996),定量下限为0.1μg·m L~(-1),提取回收率在95.25%~98.21%,日内、日间精密度相对标准偏差(RSD)均小于15%。结论该法操作简便快速,特异性强,灵敏度高,可用于伊马替尼的治疗药物浓度监测。
Objective To establish a method for the determination of imatinib in plasma by ultra performance liquid chromatography-mass spectrometry (UPLC-MS / MS). Methods Carbamazepine was used as an internal standard and pretreated with protein. The column was ACQUITY UPLC BEH C 18 (100 mm × 2.1 mm, 1.7 μm). The mobile phase consisted of acetonitrile-0.1% formic acid (25:75) and the flow rate was 0.4 m L · min -1 Ion mode multiple reaction monitoring (MRM) scan analysis and investigated specificity, standard curves and lower limits of quantitation, precision and recovery, matrix effects and stability. Results The linear range of imatinib in plasma was 0.1 ~ 20.0μg · m L -1 (r = 0.996). The lower limit of quantitation was 0.1μg · m L -1 and the recovery was between 95.25% and 98.21 %, The relative standard deviations (RSDs) of intra-day and inter-day precision were less than 15%. Conclusion The method is simple, rapid, specific and sensitive and can be used to monitor the concentration of imatinib.