HPLC-MS/MS法检测尿液中依托咪酯和依托咪酯酸。

Q3 Medicine
Tian-Fu He, Huan-Hui Zhu, Yuan-Yuan Tian, Yin-Shuang Jin, Xian-Wen Lin, Song-Cai Wang
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引用次数: 0

摘要

目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)检测尿液中依托咪酯和依托咪酯酸的方法。方法:用乙腈沉淀尿液中的蛋白质,离心过滤后得到上清。上清液在C18柱上分离,流动相为0.1%甲酸溶液和乙腈,流速为0.4 mL/min。采用正电喷雾电离(ESI)和多重反应监测(MRM)模式进行检测。对该方法的选择性、线性度和检出限进行了验证,并应用于一起依托咪酯中毒死亡病例。结果:依托咪酯和依托咪酯酸的检出限分别为0.2、0.5 ng/mL,定量限分别为0.5、1.0 ng/mL。在线性范围内呈良好的线性关系(r为0 ~ 0.995 0),在0.5、5、50 ng/mL依托咪酯和1、10、100 ng/mL依托咪酯酸3个浓度水平下,基质效应在5.42% ~ 18.47%范围内,提取回收率大于84.25%,稳定性大于88.23%。准确度、精密度和稀释度均满足实验要求。在过量服用依托咪酯的死者尿液中成功检测到依托咪酯和依托咪酯酸的浓度分别为8.82和27.88 μg/mL。结论:该方法预处理简单、灵敏度高、线性范围宽,可用于法医学中尿液样品中依托咪酯及依托咪酯酸的检测。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Detection of Etomidate and Etomidate Acid in Urine Using HPLC-MS/MS Method.

Objectives: 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 experimental 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.

Conclusions: 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.

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来源期刊
法医学杂志
法医学杂志 Medicine-Pathology and Forensic Medicine
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1.50
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