HS-GC、LC-MS/MS同时检测血液中四种卤代羟基烷麻醉剂及其代谢物  

Simultaneous detection of four halogenated hydroxyalkane anesthetics and their metabolites in blood by HS-GC and HPLC-MS/MS

作　　者：吕惊晗 卫娟娜 李萌萌 辛国斌 商金磊 郭杰[2] 孟令宗[3] Lv Jinghan;Wei Juanna;Li Mengmeng;Xin Guobin;Shang Jinlei;Guo Jie;Meng Lingzong(Key Laboratory of Forensic Toxicology,Ministry of Public Security,Beijing 100192,China;Technology Section of Criminal Police Detachment of Qingdao Public Security Bureau,Qingdao 266001,Shandong,China;Linyi University,Linyi 276012,Shandong,China)

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

出　　处：《中国法医学杂志》2024年第5期577-583,共7页Chinese Journal of Forensic Medicine

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

摘　　要：目的 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-气相质谱(HS-GC)检验方法,并建立血液中恩氟烷、异氟烷、地氟烷共同代谢物三氟乙酸(TFA)的液相色谱-串联质谱(LC-MS/MS)检验方法。方法 取0.5 mL血样置于10 mL顶空瓶中,加1.0 mL超纯水混匀,再加入0.5 mL正丁醇内标溶液,密封后70℃加热20 min,取上层气体进HS-GC分析,以双柱保留时间定性,以内标标准曲线法定量;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)、负离子模式扫描,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。结果 恩氟烷、异氟烷、地氟烷、七氟烷、HFIP、TFA检出限(LOD)分别为0.05、0.2、0.5、0.05、0.5μg/mL和0.5 ng/mL,且在1~100μg/mL(TFA:1~100 ng/mL)范围内线性关系良好,相关系数均> 0.999,提取回收率在30%~80%之间,日内及日间精密度均<5%,准确度在85%~115%之间。结论 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。Objective To establish a HS-GC test method for the determination of enflurane,isoflurane,diflurane,sevoflurane and its metabolite hexafluoroisopropanol(HFIP)in blood,and to establish a LC-MS/MS method for the determination of trifluoroacetic acid(TFA),the co-metabolite of enflurane,isoflurane,and deflurane in blood.Methods Place 0.5 mL blood sample in a 10 mL headspace bottle,add 1.0 mL ultrapure water to mix,then add 0.5 mL n-butanol internal standard solution,sealed and heated at 70℃for 20 min,take the upper layer of gas for HS-GC analysis,qualitatived by dual-column retention time and quantified by the internal standard curve;Blood sample was acetonitrile precipitated protein,separated by liquid chromatography,scanned with electrospray ionization(ESI),negative ion mode,and examined in multiple reaction monitoring mode(MRM),qualitatived by retention time and characteristic ions,quantified by standard curve.Results The detection limits(LOD)of enflurane,isoflurane,desflurane,heptaflurane,HFIP and TFA are 0.05,0.2,0.5,0.05,0.5μg/mL and 0.5 ng/mL,and linear range as 1~100μg/mL(TFA:1~100 ng/mL),with correlation coefficients greater than 0.999.The extraction recovery rate is between 30%and 80%,and the intra-day and inter-day precision are less than 5%.The accuracy is between 85%and 115%.Conclusion This method is quick 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-气相色谱 液相色谱-串联质谱 

分 类 号：DF918.93[政治法律—国际法学]