人血浆中白消安血药浓度的测定

Determination of Busulfan Concentration in Plasma by UPLC-MS-MS

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 C18（100mm×2．1mm，1．7μm），流动相为乙腈-0．05%甲酸水溶液（20：80），流速为0．4mL／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／mL（r=0．996），定量下限为0．1μg／mL，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 UPLC-MS/MS method for the determination ofbusulfan concentration in human plasma. Methods： The plasma procedure involveds a single-step protein precipitation by acetonitrile, and then chromatographed on a ACQUITY UPLC BEH C18 column （100 mm× 2.1 mm, 1.7 μm） using a mobile phase composed of acetonitrile-0.05% formic acid （20：80） at a flow rate of 0.4 μg/mL. The protonated ions of analytes were detected in positive ionization in multiple reaction monitoring mode （MRM）. The specificity, standard curve, lower limit of quantitation, precision, recovery rate and stability as well as the matrix effect were investigated. Results： The calibration curve was linear over a concentration range of 0.1 to 10 μg/mL （r= 0.996） and the low limit of quantitation was 0.1 μg/mL. The extraction recovery rates were ranged between 95.26% and 98.22%, with-day RSD and between-day RSD being all less than 15%. Conclusion： The method is simple and quick, with high specificity and sensitivity, and it can be used for therapeutic drug concentration monitoring of busulfan.