血液中七氟烷等四种卤代羟基烷麻醉剂及代谢物的检验方法研究  

Research on inspection methods for four halogenated hydroxylane anesthetics and metabolites in bloodpyrazole

作　　者：吕惊晗 李萌萌 卫娟娜 辛国斌 吴克宁 郭杰[2] 孟令宗[3] LU Jing-han;LI Meng-meng;WEI Juan-na;XIN Guo-bin;WU Ke-ning;CUO Jie;MENG Ling-zong(Key Laboratory of Forensic Toxicology,Ministry of Public Security,Bejing 100192,China;Qingdao Public Security Bureau,Qingdao 266001,China;Linyi University,Linyi 276012,China)

机构地区：[1]法庭毒物分析公安部重点实验室,北京100192 [2]青岛市公安局,山东青岛266001 [3]临沂大学,山东临沂276012

出　　处：《化学研究与应用》2025年第2期273-280,共8页Chemical Research and Application

基　　金：法庭毒物分析公安部重点实验室专项基金项目(2022FTDWFX06)资助。

摘　　要：建立血液中恩氟烷、异氟烷、地氟烷、七氟烷及其代谢物六氟异丙醇(HFIP)的顶空固相微萃取-气质联用(HS-SPME/GC-MS)检验方法,并建立了血液中恩氟烷、异氟烷、地氟烷共同代谢物三氟乙酸(TFA)的液相色谱-质谱(LC-MS/MS)检验方法,旨在开展对该类物质及代谢物整体系统的研究,可用于该类物质的滥用及麻醉犯罪案件中血液的检验。取0.5mL血样置于20mL顶空瓶中,加1.0mL超纯水混匀,密封后用80μm DVB/Carbon WR/PDMS SPME固相微萃取针70℃萃取20min,进GC-MS分析,采用HP-PLOT/Q(30m×0.32mm,20μm)色谱柱,SCAN质谱扫描模式;血样经乙腈沉淀蛋白,经液相色谱分离,采用电喷雾离子源(ESI)、正离子模式扫描,多反应监测模式(MRM)检验,以保留时间和特征离子定性,以标准曲线法定量。恩氟烷、异氟烷、地氟烷、七氟烷、HFIP、TFA检出限(LOD)分别为0.05、0.05、0.1、0.1、0.1μg·mL^(-1)和0.5 ng·mL^(-1),且在0.5~100μg·mL^(-1)(TFA:1~100ng·mL^(-1))范围内线性关系良好,相关系数均大于0.999,提取回收率均在85%~106%之间,日内及日间精密度均小于10%,准确度均在85%~115%之间。该方法快速、简便,可用于血中恩氟烷、异氟烷、地氟烷、七氟烷及其代谢物HFIP、TFA的定性定量检验。To establish HS-SPME/GC-MS method for the detection of enflurane,isoflurane,desflurane,heptaflurane,and their metabolite hexafluoroisopropanol(HFIP)in blood,and establish LC-MS/MS method for the detection of trifluoroacetic acid(TFA),a common metabolite of enflurane,isoflurane,and desflurane in blood.Put 0.5mL of blood sample in a 20mL headspace bottle.Add1.0mL water and mix well.Seal it and use 80μm DVB/Carbon WR/PDMS SPME solid-phase microextraction needle to extract at70℃for 20 minutes.Analyze it through GC-MS.Using HP-PLOT/Q(30m×0.32mm,20μm)Chromatographic column,SCAN mass spectrometry scanning mode,analyzed by GC-MS.The blood sample was precipitated by acetonitrile,separated by liquid chromatography,scanned by electrospray ion source(ESI),positive ion mode,and tested by MRM.It was characterized by retention time and characteristic ions,and quantified by standard curve.The detection limits(LOD)of enflurane,isoflurane,desflurane,heptaflurane,HFIP,and TFA are 0.05、0.05、0.1、0.1、0.1μg·mL^(-1)and 0.5 ng·mL^(-1),and linear range as 0.5~100μg·mL^(-1)(TFA:1-100ng·mL^(-1)),with correlation coefficients greater than 0.999.The extraction recovery rate is between 85%and 106%,and the intra day and inter day precision are less than 10%.The accuracy is between 85%and 115%.Conclusions This method is fast and simple,and can be used for qualitative and quantitative analysis of enflurane,isoflurane,desflurane,sevoflurane and their metabolites in blood.

关 键 词：法医毒物学 卤代羟基烷 顶空固相微萃取-气质联用 液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学]