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

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.