UPLC-MS/MS法测定人血浆中卡马西平浓度

目的:建立UPLC-MS/MS法测定人血浆中卡马西平浓度并进行方法验证,应用于室间质评的样品测定。方法:采用UPLC-MS/MS法,以卡马西平-d8为内标,XSelect CSH C18柱(2.1 mm×75 mm,2.5μm)为分析柱,流动相A为含0.05%甲酸的水溶液,流动相B为含0.05%甲酸的乙腈溶液,流速为0.3 mL·min^-1,梯度洗脱;采用电喷雾离子源,以多反应监测(MRM)正离子模式进行检测,用于定量分析的离子对为m/z 237.1→194.1(卡马西平)、m/z 245.0→202.1(卡马西平-d8)。结果:卡马西平在5~1000 ng·mL^-1范围内线性关系良好(r≥0.9993),批内批间精密度和准确度、回收率和基质效应以及稳定性均符合生物样品测定要求。应用该方法测定的室间质评样品结果全部通过。结论:该方法准确、灵敏、选择性好、重现性高,适用于血浆中卡马西平浓度测定及室间质评。

Determination of carbamazepine in human plasma by UPLC-MS/MS

Objective:To established and validated a ultra performance liquid chromatography/tandem mass spectrometry(UPLC-MS/MS)method for concentration determination of carbamazepine in human plasma,and apply the method for external quality assessment.Methods:UPLC-MS/MS method was adopted.Carbamazepine-d8 was the internal standard(IS).The determination was performed on XSelect CSH C18 column(2.1 mm×75 mm,2.5μm)with a linear gradient.The flow rate was 0.3 mL·min^-1.The mobile phase A consisted of water and 0.05%formic acid.The mobile phase B consisted of acetonitrile and 0.05%formic acid.Carbamazepine was detected with multiple reaction monitoring(MRM)mode by positive electron spray ionization(ESI+).The ion pairs used for quantitative analysis were m/z 237.1→194.1(carbamazepine),m/z 245.0→202.1(carbamazepine-d8).Results:The liner range of carbamazepine were 5–1000 ng·m L^-1(r≥0.9993).The intra-day and inter-day accuracies and precisions,the recoveries,the matrix effects,and the sample stability all met the biological sample determination requirements.All samples determined by this method passed external quality assessment.Conclusion:The method was accurate,sensitive with good selectivity and reproducibility,which was suitable for the determination of carbamazepine in human plasma and external quality assessment.