节点文献
SPE-GC/MS法测定人全血中的9种新型抗抑郁药及2种代谢产物
Determination of nine antidepressants and their metabolites in human blood using SPE-GC/MS
【作者】 陈秀娟; 宋林; 梁晨; 柴逸峰; 张润生; 洪战英;
【Author】 Song Lin;Liang Chen;Chai Yifeng;Zhang Runsheng;Hong Zhanying;School of Pharmacy,Second Military Medical University,Shanghai Key Laboratory for Pharmaceutical Metabolites Research;Fujian University of Traditional Chinese Medicine;Shanghai Institute of Forensic Science,Shanghai Key Laboratory of Crime Scene Evidence;
【机构】 中国人民解放军第二军医大学药学院上海市药物代谢产物研究重点实验室; 福建中医药大学药学院; 上海市公安局物证鉴定中心上海市现场物证重点实验室;
【摘要】 目的:采用SPE-GC/MS法测定人全血中的9种新型抗抑郁药及2种代谢产物——吗氯贝胺、马普替林、舍曲林、米安舍林、文拉法辛、帕罗西汀、美利曲辛、氟西汀、西酞普兰、N-去甲西酞普兰、O-去甲文拉法辛。方法:通过对比不同类型填料(C18、CX等)的萃取效果,最终采用C18固相萃取小柱进行萃取,操作简便。GC/MS测定采用气相色谱柱DB-5ms(0.25 mm×30 m×0.25μm),不分流进样,进样口280℃;程序升温:100℃(1 min)20℃/min200℃(10 min)8℃/min300℃(5 min)。MS采用EI电子轰击源,离子源温度230℃,接口温度300℃,选择离子扫描模式(SIM)对各物质进行定量。结果:各物质在50~1000 ng/mL(或100~2000ng/mL)范围内线性良好。除氟西汀外,各物质的提取回收率均大于50%;各物质相对回收率均在85~115%范围内;除O-去甲文拉法辛外其他物质的日内、日间精密度均在15%以内。结论:该方法快速简便,可用于不同种类新型抗抑郁药物的检测,作为法医毒物分析的技术储备。
【Abstract】 Objective:A SPE-GC/MS method has been developed to determine the concentrations of nine new antidepressants and two metabolites in human blood, i.e., moclobemide, maprotiline, sertraline, mianserin, venlafaxine, paroxetine, melitracen, fluoxetine, citalopram, N-desmethylcitalopram, and O-desmethylvenlafaxine. Methods:By comparing the extraction efficiency of different column packings such as C18 and CX, the C18 cartridge was finally chosen to extract the target objects in SPE. Temperature programming was adopted for the GC column, and the interface temperature was 300℃. Results:Under the optimized conditions, all the compounds were linear in the range of 50~1000 ng/mL or 100~2000 ng/mL, and the extraction recoveries were greater than 50% except fluoxetine. The relative recoveries were between 85~115%. The precision in RSD were less than 15% except O-desmethylvenlafaxine. Conclusion : The developed method was demonstrated to detect various kinds of new antidepressants in human blood.
【Key words】 GC/MS; solid-phase extraction; new antidepressants; metabolites; human blood;
- 【会议录名称】 2016年中国药学大会暨第十六届中国药师周论文集
- 【会议名称】2016年中国药学大会暨第十六届中国药师周
- 【会议时间】2016-12-08
- 【会议地点】中国北京
- 【分类号】D919.1
- 【主办单位】中国药学会