高效液相色谱-质谱串联法同时测定人血清中拉莫三嗪及卡马西平的含量  被引量:8

Simultaneous Determination of Lamotrigine and Carbamazepine in Human Serum by LC-MS/MS

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作  者:陈凯云[1] 骆利平[2] 谢文毅[1] 成芳[1] 陈海芳[2] 

机构地区:[1]南昌大学第四附属医院药剂科,南昌330003 [2]江西中医学院教育部重点实验室,南昌330000

出  处:《中国医院用药评价与分析》2012年第12期1108-1110,共3页Evaluation and Analysis of Drug-use in Hospitals of China

基  金:2009年南昌大学科技基金资助项目(Z04848)

摘  要:目的:建立高效液相色谱-质谱串联(LC-MS/MS)法测定人血清中拉莫三嗪及卡马西平的含量。方法:取人血清经乙腈直接沉淀后进样分析,色谱柱为Diamonsil C18(150 mm×4.6 mm,5μm),流动相为甲醇∶0.2%甲酸水溶液,流速为0.4 mL.min-1;流动相采用梯度洗脱。质谱采用ESI离子源,正离子多反应监测扫描分析,拉莫三嗪离子对为m/z 256→145,卡马西平离子对为m/z 237→194。结果:卡马西平和拉莫三嗪血药浓度分别在5~500μg.L-1(r=0.998 9)和5~500μg.L-1(r=0.997 2)范围内线性关系良好,定量下限分别为5μg.L-1。日内、日间RSD均<7.0%;提取回收率均>85%。结论:本方法处理样品简便,适用于临床血药浓度监测及为联合用药的药动学研究奠定基础。OBJECTIVE:To develop LC-MS/MS method for determination of Lamotrigine(LTG) and Carbamazepine(CBZ) in human serum.METHODS: The human serum sample was precipitated by acetonitrile before separation on Diamonsil C18(150 mm×4.6 mm,5 μm) column with mobile phase consisted of methanol-0.2% formic acid solution and at flow rate of 0.4 mL·min-1.The elution program for the mobile phase was gradient elution.ESI ion source was adopted in mass spectrum.Protonated ion of samples was detected in positive ionization by Multiple Reaction Monitoring(MRM) mode.The ion pair was m/z 256→145 for Lamotrigine and m/z 237→194 for Carbamazepine.RESULTS: The linear calibration curve of Lamotrigine and Carbamazepine were obtained in the concentration range of 5-500 μg·L-1(r=0.998 9 and r=0.997 2).The lowest limit of quantitation was 5.0 μg·L-1.Both inter-day RSD and intra-day RSD were lower than 7.0%.The average extraction recovery rates of Lamotrigine and Carbamazepine were greater than 85%.CONCLUSION: The method is simple and suitable for blood concentration monitoring and it lays foundation for the pharmacokinetic study of Lamotrigine and Carbamazepine during drug combination.

关 键 词:拉莫三嗪 卡马西平 高效液相色谱-质谱串联法 药动学 

分 类 号:R965[医药卫生—药理学]

 

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