分散液液微萃取-气相色谱串联质谱联用法测定生物样品中艾司西酞普兰  

Determination of Escitalopram in Biological Samples by Dispersive Liquid-Liquid Microextraction Combined with GC-MS/MS

作　　者：管青林 解文凯 吕晨曦 路晓君 尉志文[1] 郭相杰[1] 孙俊红[1] 贠克明[1] 崔海燕 GUAN Qing-lin;XIE Wen-kai;LÜ Chen-xi;LU Xiao-jun;WEI Zhi-wen;GUO Xiang-jie;SUN Junhong;YUN Ke-ming;CUI Hai-yan(School of Forensic Medicine,Shanxi Medical University,Jinzhong 030600,Shanxi Province,China)

机构地区：[1]山西医科大学法医学院,山西晋中030600

出　　处：《法医学杂志》2020年第4期519-524,共6页Journal of Forensic Medicine

基　　金：国家重点研发计划资助项目(2017YFC0803504);国家青年科学基金资助项目(81601647);国家博士后基金面上资助项目(2019M651086)。

摘　　要：目的建立超声辅助离子液体-分散液液微萃取-气相色谱串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)联用法测定生物样品中艾司西酞普兰的方法,为艾司西酞普兰相关案件的法医学鉴定提供依据。方法以1-己基-3-甲基咪唑六氟磷酸盐([C6MIM][PF6])离子液体为萃取剂处理生物样品,通过超声辅助萃取,GC-MS/MS法检测。结果血液和肝组织中艾司西酞普兰的线性范围分别为5.56~1111.10ng/mL和0.025~5.00mg/g,相关系数(r)均大于0.999,检出限分别为4.00ng/mL和2.00μg/g,定量限分别为14.00ng/mL和6.00μg/g,提取回收率均大于50%,日内和日间精密度均小于20%。采用本方法从实际中毒案件的血液和肝组织样品中均检出艾司西酞普兰成分,含量分别为1.26μg/mL和0.44 mg/g。结论超声辅助离子液体-分散液液微萃取-GC-MS/MS联用法检测生物样品中艾司西酞普兰,具有环境友好、快速、富集效果好、有机溶剂消耗小的优点,可应用于艾司西酞普兰相关案件的法医学鉴定。Objective To establish a method for determination of escitalopram in biological samples by ultrasound-assisted ionic liquid-dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)and provide evidences for forensic determination of cases related to escitalopram.Methods The 1-hexyl-3-methylimidazolium hexafluorophosphate([C6MIM][PF6])was selected as an extract solvent to process biological samples.Ultrasound-assisted extraction was used on the samples.Then the samples were detected by GC-MS/MS.Results The linear range of escitalopram in blood and liver were 5.56-1111.10 ng/mL and 0.025-5.00 mg/g,respectively.The correlation coefficient(r)were greater than 0.999,limit of detection(LOD)were 4.00 ng/mL and 2.00μg/g,limit of quantitation(LOQ)were 14.00 ng/mL and 6.00μg/g,respectively.The extraction recovery rates were all greater than 50%,the interday and intraday precision were less than 20%.Escitalopram was detected in blood and liver samples from the actual poisoning case by this method with a content of 1.26μg/mL and 0.44mg/g,respectively.Conclusion The ultrasound-assisted ionic liquid-dispersive liquidliquid microextraction combined with GC-MS/MS is environment friendly,rapid,has good enriching effect and consumes less organic solvent and can be used for forensic determination of escitalopram related cases.

关 键 词：法医毒理学 气相色谱-串联质谱法 艾司西酞普兰 超声辅助离子液体-分散液液微萃取 生物检材 

分 类 号：DF795.1[医药卫生—法医学]