血液中依托咪酯及依托咪酯酸成分的HPLC-MS/MS检测
Determination of Etomidate and Etomidate Acid in Blood using HPLC-MS/MS
何天夫 1林贤文 1唐定睿 2田源源 1梁未未 1刘悦1
作者信息
- 1. 广州市刑事科学技术研究所,广东 广州 510030
- 2. 广东警官学院,广东 广州 510440
- 折叠
摘要
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.
Abstract
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.
关键词
法医毒物分析/HPLC-MS/MS/依托咪酯/依托咪酯酸/血液样品Key words
Analysis of forensic toxicology/HPLC-MS/MS/Etomidate/Etomidate acid/Blood引用本文复制引用
出版年
2024
NETL
NSTL
万方数据