HPLC-MS/MS法检测人血浆中卡马西平浓度

HPLC-MS / MS Assay for Quantification of Carbamazepine in Human Plasma

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 develop and validate an assay for carbamazepine in human plasma using LC-MS /MS. Methods Plasma samples were processed by protein precipitation. Chromatography was performed on a ZORBAX Eclipse XDB-C18 column with a binary mobile phase composed of acetonitrile 0. 1% formic acid in water. MS detection was used in a multiple reaction monitoring mode with MS / MS ion transitions at m / z 237. 0 →194. 0 for carbamazepine and m / z 285. 1→154. 0 for diazepam（ internal standard,IS）. Results The linearity ranged from 4 to4000 ng·ml^-1 in plasma with the lower limit of quantitation at 4 ng·ml^-1. The intra-and inter-day precisions of the concentration was 3. 36%- 6. 88% and 6. 02%- 12. 97%,respectively. Conclusion This is a quick,specific,selective and reliable method for determination of carbamazepine in human plasma.