Investigating the capability of UA-DLLME and DART-HRMS in the analysis of benzodiazepines in whole human blood

IF 2.6 3区医学 Q2 CHEMISTRY, ANALYTICAL Forensic Chemistry Pub Date : 2024-04-27 DOI:10.1016/j.forc.2024.100580

Ananda da Silva Antonio , Cecília de Andrade Bhering , Gleicielle Tozzi Wurzler , Diego Rissi Carvalhosa , Antônio Celso Jardim , Marc Yves Chalom , Francisco Radler de Aquino Neto , Gabriela Vanini

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Abstract

Benzodiazepine (BZD) misuse has increased in the last decade, making its occurrence in criminal cases more commonplace. The detection of BZD in complex biological samples is challenging since they are usually found in small concentrations, requiring the development of sensitive and fast-to-execute methods. In this study, the application of direct analysis in real time – high-resolution mass spectrometry (DART-HRMS) was evaluated in the detection of 10 benzodiazepines (diazepam, oxazepam, chlordiazepoxide, temazepam, alprazolam, flunitrazepam, bromazepam, clonazepam, lorazepam, and midazolam) in ante and postmortem blood samples. Moreover, an ultrasound-assisted dispersive liquid–liquid microextraction (UA-DLLME) approach was developed by full factorial design as a clean-up step before the DART-HRMS analysis. DART-HRMS was capable of qualitative detection of all evaluated BZD in raw antemortem blood samples at concentrations as low as 10 µg mL⁻¹. The UA-DLLME DART-HRMS approach was linear for the 10 BZD in the range of 1 to 10 µg mL⁻¹, with recoveries ranging from 78.5 to 119.5 %, a precision lower than 36 % at 1 µg mL⁻¹, and limits of detection varying between 0.25 and 0.50 µg mL⁻¹. Moreover, the UA-DLLME DART-HRMS method was efficiently applied to postmortem blood samples from criminal cases, enabling the detection of BZD. The developed method facilitated the analysis of 10 BZD in ante and postmortem blood samples, offering a quick sample extraction that linked to the DART-HRMS can be used as a fast and reliable triage method for regulatory screening purposes and could be readily integrated into routine forensic analysis workflows in a high throughput manner.

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研究 UA-DLLME 和 DART-HRMS 分析全人类血液中苯并二氮杂卓的能力

苯二氮卓（BZD）的滥用在过去十年中有所增加，使其在刑事案件中的出现更为普遍。在复杂的生物样本中检测 BZD 具有挑战性，因为它们的浓度通常很低，因此需要开发灵敏、快速的方法。本研究评估了实时直接分析-高分辨质谱法（DART-HRMS）在检测死前和死后血液样本中 10 种苯二氮卓类药物（地西泮、奥沙西泮、氯氮卓、替马西泮、阿普唑仑、氟硝西泮、溴西泮、氯硝西泮、劳拉西泮和米达唑仑）中的应用。此外，还通过全因子设计开发了超声辅助分散液液微萃取（UA-DLLME）方法，作为 DART-HRMS 分析前的净化步骤。DART-HRMS 能够定性检测生前血液样本中所有被评估的 BZD，检测浓度低至 10 µg mL-1。UA-DLLME DART-HRMS 方法在 1 到 10 µg mL-1 的范围内对 10 种 BZD 具有良好的线性关系，回收率在 78.5% 到 119.5% 之间，1 µg mL-1 时的精确度低于 36%，检测限在 0.25 到 0.50 µg mL-1 之间。此外，UA-DLLME DART-HRMS 方法还有效地应用于刑事案件的死后血液样本，实现了对 BZD 的检测。所开发的方法有助于分析死前和死后血液样本中的 10 种 BZD，提供了一种快速的样本提取方法，与 DART-HRMS 相结合，可作为一种快速可靠的分流方法用于监管筛查目的，并能以高通量的方式随时纳入常规法医分析工作流程。

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来源期刊

Forensic Chemistry CHEMISTRY, ANALYTICAL-

CiteScore

5.70

自引率

14.80%

发文量

审稿时长

46 days

期刊介绍： Forensic Chemistry publishes high quality manuscripts focusing on the theory, research and application of any chemical science to forensic analysis. The scope of the journal includes fundamental advancements that result in a better understanding of the evidentiary significance derived from the physical and chemical analysis of materials. The scope of Forensic Chemistry will also include the application and or development of any molecular and atomic spectrochemical technique, electrochemical techniques, sensors, surface characterization techniques, mass spectrometry, nuclear magnetic resonance, chemometrics and statistics, and separation sciences (e.g. chromatography) that provide insight into the forensic analysis of materials. Evidential topics of interest to the journal include, but are not limited to, fingerprint analysis, drug analysis, ignitable liquid residue analysis, explosives detection and analysis, the characterization and comparison of trace evidence (glass, fibers, paints and polymers, tapes, soils and other materials), ink and paper analysis, gunshot residue analysis, synthetic pathways for drugs, toxicology and the analysis and chemistry associated with the components of fingermarks. The journal is particularly interested in receiving manuscripts that report advances in the forensic interpretation of chemical evidence. Technology Readiness Level: When submitting an article to Forensic Chemistry, all authors will be asked to self-assign a Technology Readiness Level (TRL) to their article. The purpose of the TRL system is to help readers understand the level of maturity of an idea or method, to help track the evolution of readiness of a given technique or method, and to help filter published articles by the expected ease of implementation in an operation setting within a crime lab.