Systematic analysis of post-blast organic traces in soil, application of color tests, TLC, GC–MS, and ITMS

IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Journal of Chromatography A Pub Date : 2025-04-12 Epub Date: 2025-02-15 DOI:10.1016/j.chroma.2025.465776
Ahmed M.Bendary Salem , Mohamed Ismail , Bolaji Oladipo
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Abstract

The post-blast trace analysis of explosives is inherently complex, requiring the separation and identification of multiple unknown compounds within contaminated matrices. The study explores modified methods for the extraction, analysis, and detection of post-explosion residues, of the three main organic explosives groups, focusing on key explosives such as NC (Nitrocellulose), NG (Nitroglycerin), Tetryl, TNT, RDX, PETN, as well as sheet and plastic explosives. A comprehensive protocol was developed, involving sample extraction, filtration, and clean-up processes, followed by analysis using a range of analytical techniques. The study introduces an optimized spot test scheme and proposes novel TLC mobile phases for improved separation and characterization of explosives. In addition, a new GC/EI-MS method was developed for the selective detection of PETN, overcoming common thermal degradation issues.
The presented GC–MS findings of this study demonstrate the significant advancements made in overcoming these obstacles, providing a clearer understanding of the analytical improvements enabling its reliable detection. Ion Trap Mobility Spectrometry (ITMS) was employed for evaluating the concentration-time decay of explosive residues on hand swabs, revealing that NG exhibited higher persistence than TNT. The study determined the Minimum Detection Limits (MDL) to be 2 ng for TNT, 3 ng for RDX and NG, and 4 ng for PETN. The research underscores that the effectiveness of explosive detection methods depends on aligning techniques with the physical and chemical properties of the analytes. Results also emphasize the importance of using confirmatory techniques beyond TLC and spot tests, as these methods are presumptive analyses and insufficient for independent compound identification. The proposed TLC mobile phases achieved significant resolution of the studied explosives, achieving significantly improved Rf values for a wide range of explosives across different groups, confirming their suitability for forensic applications. This study establishes that GC/EI-MS with its basic set, can be used for PETN analysis, while ITMS offers a fast and reliable approach for field detection and persistence studies. Collectively, these findings contribute to the analytical protocols for forensic explosive residue analysis.
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爆炸后土壤中有机痕迹的系统分析,颜色测试,TLC, GC-MS和ITMS的应用
爆炸后爆炸物的痕量分析本质上是复杂的,需要在污染基质中分离和鉴定多种未知化合物。本研究探讨了三种主要有机炸药类的爆炸后残留物提取、分析和检测的改进方法,重点关注NC(硝化纤维素)、NG(硝化甘油)、Tetryl、TNT、RDX、PETN以及片状和塑料炸药等关键炸药。制定了一个全面的方案,包括样品提取、过滤和清理过程,然后使用一系列分析技术进行分析。该研究提出了一种优化的现场测试方案,并提出了一种新的TLC流动相,以改善爆炸物的分离和表征。此外,开发了一种新的GC/EI-MS方法用于选择性检测PETN,克服了常见的热降解问题。本研究的GC-MS结果显示了在克服这些障碍方面取得的重大进展,提供了对分析改进的更清晰的理解,使其能够可靠地检测。采用离子阱迁移率谱法(ITMS)评价了手拭子上炸药残留物的浓度-时间衰减,发现NG比TNT具有更高的持久性。该研究确定了TNT的最低检测限(MDL)为2 ng, RDX和ng为3 ng, PETN为4 ng。该研究强调,爆炸物检测方法的有效性取决于将技术与分析物的物理和化学性质相结合。结果还强调了使用TLC和现场测试之外的验证技术的重要性,因为这些方法是假定分析,不足以独立的化合物鉴定。所提出的TLC流动相获得了所研究爆炸物的显著分辨率,显著提高了不同类别爆炸物的Rf值,证实了其适用于法医应用。本研究建立了具有基本集的GC/EI-MS可用于PETN分析,而ITMS为现场检测和持久性研究提供了快速可靠的方法。总的来说,这些发现有助于法医爆炸残留物分析的分析规程。
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来源期刊
Journal of Chromatography A
Journal of Chromatography A 化学-分析化学
CiteScore
7.90
自引率
14.60%
发文量
742
审稿时长
45 days
期刊介绍: The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.
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