摘要
目的:建立检测一种人血浆中阿米替林液相色谱-串联质谱(LC-MS/MS)的方法。方法:加入地西泮为内标,血浆中的药物用乙醚液-液萃取去蛋白。采用Agilent Zorbax SB-C18(2.1 mm×150 mm,5μm)柱,流动相为甲醇-0.1%甲酸溶液(70∶30,v/v)。采用电喷雾离子源(ESI),正离子检测,多反应监测(multiple reaction monitoring,MRM)方式进行定量分析阿米替林,监测碎片离子峰分别为m/z233,91(阿米替林)和m/z257,222(内标)。结果:血浆中阿米替林检测方法的线性范围为2.08～1040 ng.mL-1,最低检测限为0.52 ng.mL-1,平均萃取回收率在67.5%～75.5%之间,日内和日间精密度RSD都小于7%。结论:本方法简单、灵敏,可用于临床毒物分析和药物动力学研究。
Objective：To develop a LC-MS/MS method for determination of amitriptyline in human plasma. Methods： After addition of diazepam as internal standard, liquid-liquid extraction was used to produce a protein-free extract by using by using ehtyl ether. Chromatographic separation was achieved on a Zorbax SB-C18（2.1 mm×150 mm,5 μm）column with （70：30 ,v/v） methanol-water containing 0.1% formic acid as mobile phase. Electrospray ionization （ESI） source was applied and operated in positive ion mode, multiple reaction monitoring（MRM） mode was used to quantify amitriptyline using target fragment ions m/z 233, 91 for amitriptyline and m/z 257, 222 for the IS. Results： Calibration plots were linear over the range of 2.08- 1040 ng·mL^-1 for amitriptyline in plasma. Limit of detection （LOD） for amitriptyline was 0.52 ng·mL^-1. Mean extractive recovery of amitriptyline from plasma was in the range 67.5%- 75.5%. RSD of intra-day and inter-day precision were less than 7%, respectively. Conclusion： This method is simple and sensitive enough to be used in clinic toxicological analysis and pharmacokinetic research for determination of amitriptyline in human plasma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第11期1846-1849,共4页
Chinese Journal of Pharmaceutical Analysis
