高效液相色谱离子阱质谱联用法同时测定人血浆中曲马多和对乙酰氨基酚浓度  

Determination of Tramadol and Paracetamol in Human Plasma by Liquid Chromatography Ion Trap Mass Spectrum

作　　者：谭志荣[1] 欧阳冬生[1] 周淦[1] 王连生[1] 李智[1] 王丹[1] 陈国林[1] 黄松林[1] 刘英姿[1] 胡东莉[1] 周宏灏[1] 

机构地区：[1]中南大学临床药理研究所,长沙410078

出　　处：《药物分析杂志》2005年第7期795-798,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立快速、灵敏的液相色谱-电喷雾离子阱质谱法测定人血浆中曲马多和对乙酰氨基酚的浓度。方法:血浆样品经乙腈直接沉淀蛋白后,以乙腈-10 mmoL·L-1甲酸胺-0.1%甲酸(65:15:20)为流动相,采用Hypurity C18柱(150mm× 2·1 mm,5μm)分离,流速为0.2 mL·min-1,通过电喷雾离子化离子阱质谱,以二级质谱选择离子反应监测(SRM)方式进行检测。结果:曲马多和乙酰氨基酚的线性范围分别为5～1000及20-12800 ng·mL-1,最低检测浓度分别为1和10 ng· mL-1,平均相对回收率均为103.7%,日内和日间变异均<20%,每个样品测试时间仅为7.0 min。结论:本法简单、快速、灵敏、重现性好,是一种有效的检测人血浆中曲马多和对乙酰氨基酚浓度的方法。Objective:To develop a simple,quick and sensitive method of liquid chromatography - electrospray ion trap mass spectrometry to simultaneously determine tramadol and paracetamol in human plasma. Method:After precipitation with acetonitrile,plasma sample was separated on a Hypurity C18 column(150 mm×2.1 mm,5μm),with mobile phase acetonitrile - 10 mmol·L-1 formic amine - 0. 1 % formic acid (20:15:65),flow rate 0.2mL·min-1. The electrospray ion trap mass spectrum in the positive mode and selected reaction monitor (SRM) were adopted to detect the concentration of tramadol and paracetamol. Result:The response was linear over the ranges of 5-1000 and 20-12800 ng·mL-1 for tramadol and paracetamol respectively; the lower limits of assay were 1 and 10 ng·mL respectively. The relative recoveries of tramadol and paracetamol both were 103.7% , and it has a good precision with relative standard deviat2ion of both less than 20%. The analysis time for each sample was about 7 min. Conclusion:This method is simple, quick, sensitive and reproducible, and the results are reliable and accurate.

关 键 词：对乙酰氨基酚 曲马多 人血浆 高效液相色谱 液相色谱-电喷雾离子阱质谱法 同时测定 联用法 电喷雾离子化 沉淀蛋白 血浆样品 C18柱 选择离子 二级质谱 线性范围 检测浓度 测试时间 流动相 回收率 重现性 灵敏 乙腈 甲酸 

分 类 号：R971.1[医药卫生—药品] R614.42[医药卫生—药学]