LC-MS/MS法测定人血浆中佐米曲普坦浓度  

LC-MS/MS determination of zolmitriptan in human plasma

作　　者：李鹏飞[1,2] 顾景凯[2] 潘志恒[1] 王静[1] 刘丽宏[1] 

机构地区：[1]第二炮兵总医院药剂科,北京100088 [2]吉林大学药物代谢研究中心,长春130023

出　　处：《药物分析杂志》2009年第7期1083-1087,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立高效液相色谱-质谱联用法测定人血浆中佐米曲普坦浓度。方法:选用Zorbax Extend-C18色谱柱(5μm,150mm×4.6mm),以甲醇-水-甲酸(80∶20∶1,v/v/v)为流动相,采用等度洗脱进行分离,样品用液-液萃取法处理后进样,流速:0.8mL·min-1,柱温:室温,进样量:20μL。选用API4000型三重四极杆串联质谱仪的多重反应监测(MRM)扫描方式进行检测。结果:佐米曲普坦的线性范围为0.10～40.0ng·mL-1,定量下限为0.10ng·mL-1。准确度与精密度结果显示方法日间、日内变异均小于15%,相对偏差-2.5%～3.3%,方法提取回收率大于45%,稳定性较好。结论:本研究所建立的方法快速、灵敏,专属性强、重现性好,可用于人体血浆中佐米曲普坦浓度的测定和药动学研究。Objective：To develop an LC - MS/MS method for the determination of zolmitriptan in human plasma. Methods ： Zolmitriptan and the internal standard were extracted from plasma with liquid - liquid extraction, and then separated on a Zorbax Extend - C18 column（5 μm, 150 mm × 4.6 mm）. The mobile phase consisted of methanol - water - formic acid（80： 20：1 ,v/v/v） maintained at room temperature. The flow rate was 0. 8 mL ·min^ -1 and 20 μL aliquot of residues were injected into the LC - MS/MS system. Detection was carried out by multiple reaction monitoring on an API 4000 LC -MS/MS system. Results：The assay was linear over the range 0. 10 -40. 0 ng · mL^-1 with a lower limit of quantitation of 0. 10 ng·mL^-1. Intra - and inter - day precision were both less than 15% ,respectively. The relative deviation was in the range - 2.5% - 3.3%. The recoveries of zolmitriptan were more than 45 % and stabilities were good. Conclusion：It is a rapid, sensitive, selective and reliable method for the determination of zolmitriptan in human plasma. The assay can be applied for the determination of zolmitriptan in human plasma and the study on pharmaeokineties.

关 键 词：高效液相色谱-质谱联用法 佐米曲普坦 

分 类 号：R917[医药卫生—药物分析学]