Method Development for the Analysis of Smokeless Powders and Organic Gunshot Residue by Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry

色谱法 残留物(化学) 化学 大气压化学电离 质谱法 电喷雾电离 串联质谱法 液相色谱-质谱法 高效液相色谱法 选择性反应监测 墨盒 分析化学(期刊) 电离 材料科学 化学电离 有机化学 冶金 离子
作者
Jennifer L. Thomas
标识
DOI:10.25148/etd.fi13121211
摘要

The goal of this project was to develop a rapid separation and detection method for analyzing organic compounds in smokeless powders and then test its applicability on gunshot residue (GSR) samples. In this project, a total of 20 common smokeless powder additives and their decomposition products were separated by ultra performance liquid chromatography (UPLC) and confirmed by tandem mass spectrometry (MS/MS) using multiple reaction monitoring mode (MRM). Some of the targeted compounds included diphenylamines, centralites, nitrotoluenes, nitroglycerin, and various phthalates. The compounds were ionized in the MS source using simultaneous positive and negative electrospray ionization (ESI) with negative atmospheric pressure chemical ionization (APCI) in order to detect all compounds in a single analysis. The developed UPLC/MS/MS method was applied to commercially available smokeless powders and gunshot residue samples recovered from the hands of shooters, spent cartridges, and smokeless powder retrieved from unfired cartridges. Distinct compositions were identified for smokeless powders from different manufacturers and from separate manufacturing lots. The procedure also produced specific chemical profiles when tested on gunshot residues from different manufacturers. Overall, this thesis represents the development of a rapid and reproducible procedure capable of simultaneously detecting the widest possible range of components present in organic gunshot residue.
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