Detection of Etomidate and Etomidate Acid in Urine Using HPLC-MS/MS Method
10.12116/j.issn.1004-5619.2023.330702
- VernacularTitle:HPLC-MS/MS法检测尿液中依托咪酯及依托咪酯酸
- Author:
Tian-Fu HE
1
;
Huan-Hui ZHU
;
Yuan-Yuan TIAN
;
Yin-Shuang JIN
;
Xian-Wen LIN
;
Song-Cai WANG
Author Information
1. 广州市刑事科学技术研究所,广东 广州 510442
- Keywords:
forensic medicine;
toxicological analysis;
etomidate;
etomidate acid;
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS);
urine
- From:
Journal of Forensic Medicine
2024;40(5):454-460
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the detection of etomidate and etomidate acid in urine samples.Methods Protein in the urine samples was precipitated by adding acetonitrile,and the supernatant was obtained after centrifugation and filtered.The supernatant was separated on a C18 column with a mobile phase consisting of 0.1%formic acid solution and acetonitrile at a flow rate of 0.4 mL/min.The detection was performed in positive electrospray ionization(ESI)and multiple reaction monitoring(MRM)modes.The method was validated for selectivity,linearity and limit of detection(LOD),and applied to a case of etomidate poisoning death.Results The LOD of etomidate and etomidate acid were 0.2 and 0.5 ng/mL,respectively,and the limit of quantitation(LOQ)were 0.5 and 1.0 ng/mL,respectively.Good linear relationship was observed within the linear range(r>0.995 0).At three concentration levels(0.5,5,50 ng/mL for etomidate and 1,10,100 ng/mL for etomidate acid),the matrix effect was within the range of 5.42%to 18.47%,the extraction recovery rate was greater than 84.25%and the stability was greater than 88.23%.The accuracy,precision and dilution reliability all met the experimen-tal requirements.Etomidate and etomidate acid were successfully detected with the concentrations of 8.82 and 27.88 μg/mL in the urine of a deceased individual who had consumed excessive etomidate.Conclusion The method has simple pretreatment,high sensitivity and wide linear range,which can be applied to the detection of etomidate and etomidate acid in urine samples in forensic science.
