Trace detection of styphnate from pre- and post-blast samples by hydrophilic interaction chromatography with tandem mass spectrometry

IF 1.8 3区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Rapid Communications in Mass Spectrometry Pub Date : 2024-08-08 DOI:10.1002/rcm.9882

Sarah N. Sipe, Courtney A. Cruse, Christopher A. Tipple, Mark L. Miller

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引用次数: 0

Abstract

Rationale

Although ubiquitous in explosives and ammunition, few trace methods for detection of heavy metal-containing primary explosives from forensic samples are currently in practice.

Methods

Extracts of cotton swabs or direct sampling of items were cleaned up using solid-phase extraction to remove heavy metal contaminants (i.e., lead) while retaining the organic styphnate component. The styphnate was chromatographically separated using hydrophilic interaction chromatography (HILIC) and detected via high-resolution tandem mass spectrometry (MS/MS) using a sensitive, targeted approach in five minutes or less.

Results

A mass spectrometric method for the detection of styphnate, including limit of detection (LOD), sample stability, and interferences was developed. We present a validated method for the extraction, separation, and detection of styphnate from lead(II) styphnate with an estimated LOD of 257 ppt (pg/mL).

Conclusions

We detail an improved LOD relative to previous reports for trace detection of styphnate and, for the first time to our knowledge, the post-blast analysis of styphnate.

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亲水作用色谱-串联质谱法痕量检测爆炸前和爆炸后样本中的苯乙烯酸盐。

理由：尽管在爆炸物和弹药中无处不在，但目前从法医样本中检测含重金属的初级爆炸物的痕量方法却很少：方法：使用固相萃取法对棉签提取物或直接取样的物品进行清理，以去除重金属污染物（如铅），同时保留有机苯乙烯酸盐成分。使用亲水作用色谱法 (HILIC) 对苯乙烯酸盐进行色谱分离，并通过高分辨率串联质谱法 (MS/MS) 在五分钟或更短时间内进行灵敏、有针对性的检测：结果：我们开发了一种检测苯乙烯酸盐的质谱方法，包括检测限（LOD）、样品稳定性和干扰因素。我们提出了一种从苯乙烯酸铅（II）中提取、分离和检测苯乙烯酸盐的有效方法，估计 LOD 为 257 ppt（皮克/毫升）：我们详细介绍了在痕量检测苯乙烯酸铅方面比以前报告的 LOD 值更高的方法，据我们所知，这是第一次对苯乙烯酸铅进行爆炸后分析。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Rapid Communications in Mass Spectrometry 化学-分析化学

CiteScore

4.10

自引率

5.00%

发文量

219

审稿时长

2.6 months

期刊介绍： Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.