Optimization of solid-phase microextraction (SPME) for the recovery of explosives from aqueous and post-explosion debris followed by gas and liquid chromatographic analysis
Furton, KG
Director, Graduate student, and associate director, respectively, International Forensic Research Institute, Department of Chemistry, Florida International University, University Park, FL 33199.

Wu, L
Director, Graduate student, and associate director, respectively, International Forensic Research Institute, Department of Chemistry, Florida International University, University Park, FL 33199.

Almirall, JR
Director, Graduate student, and associate director, respectively, International Forensic Research Institute, Department of Chemistry, Florida International University, University Park, FL 33199.


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 mg/kg to 40 mg/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:
chromatography explosives residue, criminalistics, explosives, forensic science, high-performance liquid chromatography interface, post-explosion debris, solid-phase microextraction

Paper ID: JFS4540857

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Author Mizuno, N Affiliation National Research Institute of Police Science, 6-3-1, Kashiwanoha Kashiwa,
Chiba 277-0082, Japan. Present address: Forensic Science Laboratory, Ishikawa
Prefectural Police Headquarters, Kanazawa, Japan. Author Ohmori, T Affiliation
National Research Institute of Police Science, 6-3-1, Kashiwanoha Kashiwa,
Chiba 277-0082, Japan. Present address: Forensic Science Laboratory, Ishikawa
Prefectural Police Headquarters, Kanazawa, Japan. Author Sekiguchi, K Affiliation National Research Institute of Police Science, 6-3-1, Kashiwanoha Kashiwa,
Chiba 277-0082, Japan. Present address: Forensic Science Laboratory, Ishikawa
Prefectural Police Headquarters, Kanazawa, Japan. Author Kato, T Affiliation Forensic Science Laboratory, Fukushima Prefectural Police Headquarters,
Fukushima, Japan. Author Fujii, K Affiliation Forensic Science Laboratory, Wakayama Prefectural Police Headquarters,
Wakayama, Japan. Author Shiraishi, T Affiliation National Research Institute of Police Science, 6-3-1, Kashiwanoha Kashiwa,
Chiba 277-0082, Japan. Present address: Forensic Science Laboratory, Ishikawa
Prefectural Police Headquarters, Kanazawa, Japan. Author Kasai, K Affiliation National Research Institute of Police Science, 6-3-1, Kashiwanoha Kashiwa,
Chiba 277-0082, Japan. Present address: Forensic Science Laboratory, Ishikawa
Prefectural Police Headquarters, Kanazawa, Japan. Author Sato, H Affiliation National Research Institute of Police Science, 6-3-1, Kashiwanoha Kashiwa,
Chiba 277-0082, Japan. Present address: Forensic Science Laboratory, Ishikawa
Prefectural Police Headquarters, Kanazawa, Japan. Author Fujii, T Affiliation National Research Institute of Police Science, 6-3-1, Kashiwanoha Kashiwa,
Chiba 277-0082, Japan. Present address: Forensic Science Laboratory, Ishikawa
Prefectural Police Headquarters, Kanazawa, Japan. Author Furton KG, Wu L, Almirall JR Title Optimization of solid-phase microextraction (SPME) for the recovery of explosives from aqueous and post-explosion debris followed by gas and liquid chromatographic analysis Symposium , Committee on