液相色谱-串联质谱(LCMSMS)方法 - 岛津中国.pdf

液相色谱-串联质谱（LC/MS/MS）法测定癫痫患者血清中 卡马西平的浓度 ∗ 谢 华 ，王 荣，贾正平 ， 徐丽婷 （兰州军区兰州总医院临床药理基地，兰州 730050） 摘要 目的：本文建立了液相色谱- 串联质谱（LC/MS/MS ）法测定患者血清中的卡马西平浓度的方法。 方法：色谱柱：Zorbax Extend-C18 柱（150×4.6 mm I.D，5μm ）；流动相：甲醇-0.01mmol·L-1 乙酸 胺溶液（80:20，v/v ）；流速：0.3 mL·min-1 。结果：卡马西平浓度在 2～40 ng·mL-1范围内，峰面积 与浓度线性关系良好，平均回收率为 101.1%，日内精密度、日间精密度的RSD分别为 3.39%和 4.11% 。 并测定了 10 名患者血清中卡马西平的浓度。结论：本方法具有良好的灵敏度、准确度、精确度及专 属性，结果准确，重现性好，易于操作，可用于患者血清中卡马西平浓度的测定。 关键词 卡马西平；LC/MS/MS ；血清 Content Determination of Carbamazepine in epileptic patient serum by Liquid Chromatographic Tandem Mass Spectrometry XIE Hua, JIA Zheng-ping*, WANG Rong, XU Li-ting (Base of Clinic Pharmacology, Lanzhou General Hospital, Lanzhou Command, Lanzhou 730050, China) ABSTRACT OBJECTIVE: An analytical method based on Liquid Chromatography with tandem Mass Spectrometry (LC-MS/MS) detection was developed for the content determination of carbamazepine in epileptic patient serum. METHODS: The method included that the column was Zorbax Extend-C18(150×4.6 mm I.D. ，5μm ); mobile phase was methanol-0.01mmol·L-1amine acetic acid (80:20 ，v/v) at a flow rate of 0.3 mL·min-1. RESULTS: The method was proved to be linear in the range of 2~40ng·mL-1 with a regression confficient of 0.9976. The average recovery rate was 101.1%(n=5). The RSD of average contents of intra-day and inter-day was 3.39% and 4.11% respectively. The carbamazepine concentrations of ten epileptic patient’s serums were detected. CONCLUSION: This method is accurate, precise, sensitive and specific to be used in the content determination of carbamazepine serum. KEY WORDS Carbamazepine; LC/MS/MS; Serum ∗基金项目：国家科技部重大项目（2008ZX