超高效液相色谱-三重四极杆串联质谱法检测毛发中依托咪酯及其代谢物和美托咪酯  

Determination of etomidate,its metabolite and metomidate in hair by ultra-performance liquid chromatography-tandem mass spectrometry

作　　者：曹广生 徐巧 郑新勇 何宽 李剑 杨继伟 俞晓峰 CAO Guangsheng;XU Qiao;ZHENG Xinyong;HE Kuan;LI Jian;YANG Jiwei;YU Xiaofeng(Expec Technology Inc.,Hangzhou 311300,China;Institute of Criminal Science and Technology of Hefei Public Security Bureau,Hefei 230001,China)

机构地区：[1]杭州谱育科技发展有限公司,杭州311300 [2]合肥市公安局刑事科学技术研究所,合肥230001

出　　处：《分析试验室》2025年第4期592-596,共5页Chinese Journal of Analysis Laboratory

摘　　要：建立了超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)法快速检测毛发中依托咪酯及其代谢物依托咪酯酸和美托咪酯。毛发样品经冷冻湿法研磨提取和冷冻离心后,上清液经0.22μm有机滤膜过滤,UPLC-MS/MS法检测。经Acquity UPLC BEH C18色谱柱分离,以0.1%甲酸水溶液(含5 mmol/L甲酸铵)和乙腈为流动相进行梯度洗脱,正离子多反应监测模式(MRM)检测。依托咪酯、依托咪酯酸和美托咪酯的检出限在0.18~0.99 pg/mg之间,定量限在0.60~3.30 pg/mg之间;依托咪酯在1~100 pg/mg范围内,依托咪酯酸和美托咪酯在5~500 pg/mg范围内,线性关系良好,相关系数r均大于0.9992;低、中、高3种添加浓度的基质效应在105.8%~113.4%之间,提取回收率在88.1%~103.0%之间,日内和日间的相对标准差(RSD)分别在2.8%~4.3%和4.2%~5.6%之间。本方法适用于毛发中依托咪酯及其代谢物依托咪酯酸和美托咪酯的检测。A novel method was established for the rapid determination of etomidate,its metabolite of etomidate acid,and metomidate in hair with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The hair samples were extracted by wet grinding and centrifuged under freezing conditions,and the supernatant was filtered through 0.22μm organic filter membrane and detected by UPLC-MS/MS.The detection was conducted after separation by Acquity UPLC BEH C18 with gradient elution using 0.1%formic acid aqueous solution(containing 5 mmol/L ammonium formate)and acetonitrile as mobile phase,and positive ion mode multiple reaction monitoring mode(MRM)was used.The limits of detection(LODs)of etomidate,etomidate acid,and metomidate were in the range of 0.18-0.99 pg/mg,and the limits of quantification(LOQs)were in the range of 0.60-3.30 pg/mg.The results showed there were good linear relationships of etomidate in the range of 1-100 pg/mg,and etomidate acid and metomidate in the range of 5-500 pg/mg,the correlation coefficients(r)were all above 0.9992.Inlow,medium,and high spikedconcentrations,the matrix effects(ME)were 105.8%-113.4%,the recoveries were 88.1%-103.0%,and the intra-day and inter-day relative standard deviations(RSDs)were 2.8%-4.3%and 4.2%-5.6%,respectively.This method is suitable for the detection of etomidate,its metabolite and metomidate in hair.

关 键 词：依托咪酯 美托咪酯 依托咪酯酸 毛发 新型滥用药物 超高效液相色谱-三重四极杆串联质谱 

分 类 号：O657.7[理学—分析化学]