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血液中依托咪酯及依托咪酯酸成分的HPLC-MS/MS检测

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目的 建立HPLC-MS/MS法检测血液样品中依托咪酯和依托咪酯酸成分.方法 待测样品加入乙腈沉淀蛋白,经振荡、超声后离心取上清液过 0.22 μm滤膜,采用Poroshell 120 EC-C18(150 mm×3.0 mm,2.7 μm)色谱柱分离,流动相A为含0.1%甲酸水,流动相B为乙腈,流速0.8 mL/min梯度洗脱.质谱仪采用电喷雾离子源、正离子模式、多反应监测模式检测.结果 血液样品中依托咪酯和依托咪酯酸在相应范围内线性关系良好,相关系数(r)均>0.998 8,检出限分别为 19.94 和 40.25 ng/mL,定量限分别为 50 和 100 ng/mL.基质效应在 1.47%~10.34%范围内,提取回收率在82.81%~90.07%范围内.采用本方法从阳性检材中检出依托咪酯和依托咪酯酸成分的含量分别为1 138.89和3 126.41 ng/mL.结论 该方法前处理简单、样品用量少、线性范围宽,可应用于依托咪酯相关的法医学检测工作.
Determination of Etomidate and Etomidate Acid in Blood using HPLC-MS/MS
Objective This study was to develop a HPLC-MS/MS method for determination of etomidate and etomidate acid in blood samples.Methods The blood samples were deproteinized with acetonitrile and supernatant was achieved by shake,sonication,centrifuge and filtration using 0.22 μm membrane.Then,supernatant was performed on an analytical column Poroshell 120 EC-C18(150 mm×3.0 mm,2.7 μm)and flowed with 0.1%formic acid(mobile phase A)and acetonitrile(mobile phase B).The gradient elution at a flow rate of 0.8 mL/min was determined using an electrospray ionization source in positive ion mode and multiple reaction monitoring mode.Results The linearities of etomidate and etomidate acid in blood samples were good within the corresponding range and the correlation coefficients(r)were over 0.9988.The limit of detection(LOD)of etomidate and etomidate acid were 19.94 and 40.25 ng/mL,and the limit of quantitation(LOQ)of them were 50 and 100 ng/mL,respectively.Moreover,matrix effects were ranged from 1.47%to 10.34%and recoveries ranged from 82.81%to 90.07%.The detection of a positive case using our method was successfully determined to be 1 138.89 and 3 126.41 ng/mL for the contents of etomidate and etomidate acid,respectively.Conclusion Our study has further confirmed that this method with simple pretreatment,little sample usage and wide linear range,can be successfully applied to the detection of forensic sciences on etomidate and etomidate acid.

Analysis of forensic toxicologyHPLC-MS/MSEtomidateEtomidate acidBlood

何天夫、林贤文、唐定睿、田源源、梁未未、刘悦

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广州市刑事科学技术研究所,广东 广州 510030

广东警官学院,广东 广州 510440

法医毒物分析 HPLC-MS/MS 依托咪酯 依托咪酯酸 血液样品

2024

中国法医学杂志
中国法医学会

中国法医学杂志

CSTPCD
影响因子:0.352
ISSN:1001-5728
年,卷(期):2024.39(4)