摘要
目的:建立大鼠脑微血管内皮细胞中卡马西平的LC-MS测定方法。方法:细胞悬液中加入内标盐酸非洛普,高速离心沉淀蛋白,取上清液进行LC-MS测定。色谱柱为ShimpackODSC18(5.0μm,150mm×2.0mmID),离子源为ESI,检测离子为[M+H]+:卡马西平(m/z):237;DDPH(m/z):344,流动相为2mmol/L醋酸铵缓冲液(pH=4)与乙腈(60∶40,v/v)。结果:本实验条件下卡马西平与内标盐酸非洛普可良好分离,保留时间分别为5.0min和3.6min左右;线性范围为0.39～50.00ng/mL;方法回收率为96%～104%;日内日间变异系数均小于13%;最低检测浓度为0.39ng/mL。结论:该方法符合生物样品测定要求,可用于细胞内卡马西平浓度的测定。
AIM:To develop an LC-MS method for the quantitative analysis of carbamazepine(CBZ) in the brain capillary endothelial cells of the rat.METHODS:Analysis was based on injection of carbamazepine in the cells into the ESI probe with a mobile phase consisting of acetonitrile and 2 mmol/L ammonium acetate with 0.2% acetic acid solution(pH=4.0) at a flow rate 0.2 mL/min.Analysis in the mass spectrometer was operated in the selected-ion monitoring model.The mass spectrometer was operated in SIM m/z 237.0 for carbamazepine and 344.0 for internal standard (DDPH).RESULTS:Under this situation the retention time of CBZ and DDPH was about 5.0 min and 3.6 min.The recorded chromatograms exhibited well-resolved peaks.The standard curve was linear in the range of 0.39～50.00 ng/mL.The instrumental detection limits were 0.39 ng/mL for the analytes.The recoveries of the analytes were 97% from untreated cell solution.The Intra-day and inter-day precision for cell ranged between 0% and (12 %.)CONCLUSION:This method is suitable for the determination of the concentration of carbamazepine in the cells.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2005年第3期241-244,共4页
Journal of China Pharmaceutical University
基金
国家高技术研究发展计划("八六三"计划)资助项目(No.2003AA2Z347A)
江苏省药物代谢动力学重点实验室资助项目(No.BM2001201)~~
