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目的本文建立了HPLC-MS/MS法测定人血浆中卡马西平浓度。方法人血浆样本经乙腈沉淀蛋白后用ZORBAX Eclipse XDB-C18色谱柱,以0.1%甲酸水溶液、乙腈为流动相进行梯度洗脱。选用多重反应监测扫描方式进行质谱监测,监测离子反应分别为m/z 237.0→194.0(卡马西平),m/z 285.1→154.0(内标地西泮)。结果血浆中卡马西平的线性范围为4~4000 ng·ml~(-1),定量下限为4 ng·ml~(-1)。血浆日内、日间精密度分别为3.36%~6.88%,6.02%~12.97%。结论该方法快速、灵敏、专属性强、重复性好,适用于人血浆卡马西平浓度的测定。
Objective To establish a HPLC-MS / MS method for the determination of carbamazepine in human plasma. Methods Human plasma samples were precipitated with acetonitrile and eluted with a gradient of ZORBAX Eclipse XDB-C18 using 0.1% formic acid in water and acetonitrile as the mobile phase. Mass spectrometry monitoring was performed with multiplex reaction monitoring and scanning. The ionization responses were m / z 237.0 → 194.0 (carbamazepine) and m / z 285.1 → 154.0 (internal standard diazepam) respectively. Results The linear range of carbamazepine in plasma was 4 ~ 4000 ng · ml ~ (-1) and the lower limit of quantification was 4 ng · ml ~ (-1). The intra-day and inter-day plasma levels were 3.36% -6.88% and 6.02% -12.97%, respectively. Conclusion The method is rapid, sensitive, specific and reproducible. It is suitable for the determination of the concentration of carbamazepine in human plasma.