Rapid determination of etomidate and its structural analogues in e-liquid by probe electrospray ionization quadrupole time-of-flight mass spectrometry

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-01-13 DOI:10.1016/j.jpba.2025.116677

Meiting Lin , Zhen Zhang , Qun He , Hongyuan Hao , Ping Xiang , Junbo Zhao

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引用次数: 0

Abstract

Etomidate and its structural analogues, which have anesthetic effects, are classified as controlled psychotropic drugs. Electronic cigarettes (e-cigarettes) have become more and more popular. With the increase of adding etomidate and its analogues to electronic liquids (e-liquids), there is a trend of abuse, which is a tough problem urgently need to be solved. This seriously affects the health and security of the public and the development of society. A simple, rapid and effective screening method is very crucial for their identification. In this study, we applied a newly developed method, probe electrospray ionization quadrupole time-of-flight mass spectrometry (PESI-QTOF-MS) with DPiMS QT ion source to analyze etomidate and its analogues in e-liquids. It allowed identification in 0.3 min with lower sample usage. Isomers can be distinguished by ion abundance ratios at collision energy (CE) 15 eV, which provided possibility for distinguishing more isomers by in-situ mass spectrometry. Limit of detection (LOD) and limit of quantitation (LOQ) of four substances were 20 ng/mL and 50 ng/mL, respectively. Good linear relationships were obtained in the concentration range of 50–5000 ng/mL with little matrix effect. The accuracy, precision, dilution effect and carryover of the method were also validated. Positive specimens (n = 38) were analyzed by both PESI-QTOF-MS and gas chromatography-mass spectrometry (GC-MS). There were five impurities including nicotine, cooling agent and flavorings were investigated by PESI-QTOF-MS, which provided the possibility for tracing the origin of illegal e-liquids. This study will help solve the backlog of cases and improve work efficiency effectively by reducing analysis time. Furthermore, it meets the need of addressing current situation of drug control and can assist forensic laboratories in investigating cases. It also demonstrates the application prospects of rapid screening in new drugs.

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探针电喷雾电离四极杆飞行时间质谱法快速测定电子液体中依托咪酯及其结构类似物。

依托咪酯及其结构类似物具有麻醉作用，被列为管制精神药物。电子烟（e-cigarette）已经变得越来越流行。随着依托咪酯及其类似物在电子液体中添加量的增加，有滥用的趋势，这是一个亟待解决的棘手问题。这严重影响了公众的健康安全和社会的发展。一种简单、快速、有效的筛选方法对其鉴别至关重要。在这项研究中，我们采用了一种新的方法，探针电喷雾电离四极杆飞行时间质谱（PESI-QTOF-MS）与DPiMS QT离子源分析电子液体中的依托咪酯及其类似物。它可以在0.3 min内以较低的样本使用量进行鉴定。用碰撞能（CE） 15 eV的离子丰度比可以区分异构体，这为原位质谱法区分更多异构体提供了可能性。4种物质的检出限和定量限分别为20 ng/mL和50 ng/mL。在50 ~ 5000 ng/mL浓度范围内呈良好的线性关系，基质效应较小。验证了该方法的准确度、精密度、稀释效果和延展性。阳性标本（n = 38）采用PESI-QTOF-MS和气相色谱-质谱（GC-MS）分析。利用PESI-QTOF-MS分析了电子烟中尼古丁、冷却剂和调味剂等5种杂质，为非法电子烟的来源溯源提供了可能。通过减少分析时间，有助于解决积压的案例，有效提高工作效率。此外，它满足了解决药物管制现状的需要，并可协助法医实验室调查案件。同时也展示了快速筛选技术在新药中的应用前景。

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来源期刊

Journal of pharmaceutical and biomedical analysis 医学-分析化学

CiteScore

6.70

自引率

5.90%

发文量

588

审稿时长

37 days

期刊介绍： This journal is an international medium directed towards the needs of academic, clinical, government and industrial analysis by publishing original research reports and critical reviews on pharmaceutical and biomedical analysis. It covers the interdisciplinary aspects of analysis in the pharmaceutical, biomedical and clinical sciences, including developments in analytical methodology, instrumentation, computation and interpretation. Submissions on novel applications focusing on drug purity and stability studies, pharmacokinetics, therapeutic monitoring, metabolic profiling; drug-related aspects of analytical biochemistry and forensic toxicology; quality assurance in the pharmaceutical industry are also welcome. Studies from areas of well established and poorly selective methods, such as UV-VIS spectrophotometry (including derivative and multi-wavelength measurements), basic electroanalytical (potentiometric, polarographic and voltammetric) methods, fluorimetry, flow-injection analysis, etc. are accepted for publication in exceptional cases only, if a unique and substantial advantage over presently known systems is demonstrated. The same applies to the assay of simple drug formulations by any kind of methods and the determination of drugs in biological samples based merely on spiked samples. Drug purity/stability studies should contain information on the structure elucidation of the impurities/degradants.