论文部分内容阅读
目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)法测定人血浆中白消安血药浓度的方法。方法:采用卡马西平为内标和蛋白沉淀前处理的方法,采用色谱柱为ACQUITY UPLC BEH C_(18)(100 mm×2.1 mm,1.7μm),流动相为乙腈-0.05%甲酸水溶液(20∶80),流速为0.4 m L/min;采用正离子模式多反应监测(MRM)扫描分析,并考察其专属性、标准曲线、定量下限、精密度、回收率、基质效应和稳定性。结果:人血浆中白消安浓度的线性范围为0.1~10.0μg/m L(r=0.996),定量下限为0.1μg/m L,提取回收率范围为95.26%~98.22%,日内和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,可用于白消安的治疗药物浓度监测。
Objective: To establish a method for the determination of busulfan in human plasma by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods: Carbamazepine was used as an internal standard and pretreatment of protein precipitation. The column was ACQUITY UPLC BEH C 18 (100 mm × 2.1 mm, 1.7 μm) and the mobile phase was acetonitrile-0.05% formic acid solution (20 : 80) at a flow rate of 0.4 m L / min. Positive ion mode MRM was used to analyze the specificity, standard curve, lower limit of quantitation, precision, recovery, matrix effect and stability. Results: The linear range of the concentration of busulfan in human plasma was 0.1 ~ 10.0μg / m L (r = 0.996), the lower limit of quantification was 0.1μg / m L, and the recovery range was 95.26% ~ 98.22% The relative standard deviations of precision (RSD) were less than 15%. Conclusion: The method is simple, rapid, specific, sensitive and can be used to monitor the concentration of busulfan.