ISSN: 0022-1198
CODEN: JFSCA
Page Count: 8

Optimization of Solid-Phase Microextraction (SPME) for the Recovery of Explosives from Aqueous and Post-Explosion Debris Followed by Gas and Liquid Chromatographic Analysis
Almirall, JR
Director, graduate student, and associate director, Florida International University, FL

Furton, KG
Director, graduate student, and associate director, Florida International University, FL

Wu, L
Director, graduate student, and associate director, Florida International University, FL

(Received 25 March 1999; accepted 4 October 1999)

Abstract

Solid-phase microextraction (SPME) has been evaluated for the recovery of explosives residues from aqueous samples and real post-explosion solid debris samples and optimized using gas chromatography with an electron capture detector (GC-ECD) and high-performance liquid chromatography with ultraviolet detection (HPLC-UV). A modified SPME/HPLC interface utilizing dual six-port valves allowed for independent optimization of SPME desorption and injection variables that provided improved chromatographic resolution and sensitivity. A unique combination of cyano and octadecyl columns resulted in the complete separation of the 14 explosives in EPA method 8330 mixture using HPLC with good quantitative results. At the optimum SPME conditions, the limits of detection (LOD) were found to be of 5 ng/mL to 16 ng/mL of explosives in water and 10 μg/kg to 40 μg/kg of explosives from soil. The technique has been successfully applied to the analysis of real post-explosion debris and can be adapted for use in the field utilizing portable chromatographic instruments.

Keywords:
forensic science, criminalistics, explosives, post-explosion debris, solid-phase microextraction, high-performance liquid chromatography interface, chromatography explosives residue

Paper ID: JFS14784J
DOI: 10.1520/JFS14784J
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