Revealing novel ionic species and key forensic insights: comparative analysis of non-extracted seized tablets vs. corresponding extracts by DART-HRMS

IF 2.6 3区医学 Q2 CHEMISTRY, ANALYTICAL

Forensic Chemistry Pub Date : 2025-05-09 DOI:10.1016/j.forc.2025.100665

Alexandre Narcelli Pestana de Aguiar , Diego Rissi Carvalhosa , Francisco Radler de Aquino Neto , Gabriela Vanini

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引用次数: 0

Abstract

The modern drug market encompasses a wide variety of chemical structures present simultaneously in individual matrices, making it nearly impossible to efficiently extract all substances using a single, standardized extraction procedure. Nevertheless, many of these substances hold forensic value and can assist forensic authorities in their investigative efforts. Direct Analysis in Real Time (DART) is an ion source that has gained prominence due to its speed and ability to eliminate the need for sample extraction. However, unextracted solid analysis through DART can produce unknown ionic species, such as clusters and adducts, complicating result interpretation. This study qualitatively analyzed six seized tablets in both solid form and as extracts using direct analysis in real time high-resolution mass spectrometry (DART-HRMS), employing a non-targeted approach to highlight key differences. The comparative analysis revealed that several synthetic impurities, adulterants, and contaminants—such as fentanyl analogues, N-MEC, N-formyl-MDA, and N-formyl-MDMA—were exclusively detected through the direct analysis of unextracted tablets, with some present solely in a cluster form. Additionally, previously unreported ionic species were identified. Direct analysis of unextracted matrices provided valuable information that was lost during sample extraction, while the phenomenon of cluster formation proved beneficial by enhancing the detection of analytes. The identified synthetic impurities elucidated the synthetic route used in the manufacture of the seized tablets, whereas specific adulterants and contaminants shed light on drug manufacturing practices. The identification of these impurities, adulterants, and contaminants exclusively through the direct analysis of unextracted solids demonstrates DART-HRMS's ability to provide quicker and more comprehensive chemical profiling of seized drugs.

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揭示新的离子种类和关键的法医见解：用DART-HRMS对未提取的缉获片剂和相应的提取物进行比较分析

现代药品市场包含同时存在于单个基质中的多种化学结构，使得使用单一的标准化提取程序有效提取所有物质几乎是不可能的。然而，其中许多物质具有法医价值，可以协助法医当局进行调查工作。直接实时分析（DART）是一种离子源，由于其速度和消除样品提取需求的能力而获得突出地位。然而，通过DART进行未提取的固体分析可能会产生未知的离子种类，如簇和加合物，使结果解释复杂化。本研究采用实时高分辨率质谱（DART-HRMS）直接分析方法，对6种被查获的片剂进行了定性分析，包括固体形式和提取物，采用非靶向方法来突出关键差异。对比分析显示，几种合成杂质、掺假物和污染物，如芬太尼类似物、N-MEC、n -甲酰基mda和n -甲酰基mdma，通过对未提取片剂的直接分析可以完全检测到，其中一些仅以簇状形式存在。此外，还发现了以前未报道的离子种类。直接分析未提取的矩阵提供了在样品提取过程中丢失的有价值的信息，而簇形成现象通过增强分析物的检测被证明是有益的。鉴定出的合成杂质阐明了制造被查获药片所用的合成路线，而特定的掺杂物和污染物则阐明了药物生产实践。通过直接分析未提取的固体来识别这些杂质、掺假物和污染物，证明了DART-HRMS能够提供更快、更全面的缉获药物化学分析。

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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.