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Trace detection of styphnate from pre- and post-blast samples by hydrophilic interaction chromatography with tandem
Sarah N Sipe1, Courtney A Cruse1, Christopher A Tipple2
1Federal Bureau of Investigation, Research and Support Unit, Visiting Scientist Program, Federal Bureau of Investigation Laboratory Division, Quantico, VA, USA.
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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