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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2005年第7期795-798,共4页
Chinese Journal of Pharmaceutical Analysis
