Trace Analysis of Peroxide Explosives by High Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization-Tandem Mass Spectrometry (HPLC-APCI-MS/MS) for Forensic Applications

Abstract

An HPLC-APCI-MS(/MS) method for the (trace) analysis of the most commonly encountered peroxide explosives, hexamethylenetriperoxidediamine (HMTD) and triacetonetriperoxide (TATP), has been developed. With this method, HMTD and TATP have been analyzed in the same run. (Pseudo-)molecular ions of these peroxides have been obtained as base peak under the same condition. A series of product ions was produced from these pseudo-molecular ions ([HMTD-1]+ and [TATP + NH4]+) in the MS/MS analysis. We also pioneeredin showing that TATP molecular ion [TATP-H]+ can be observed with HPLC-MS/MS. The limit of detection for HMTD and TATP was 0.26 and 3.3 ng, respectively, on column by HPLC-MS in the Full Scan mode and 0.08 and 0.8, respectively, by HPLC-APCI-MS/MS in Selected Reaction Monitoring (single ass unit) mode. The method presented has been applied successfully for the identification of peroxides in the bulk solid state (powder sample), as well as in post-blast extracts originating from a forensic case. For the post-blast extracts, the use of tandem MS has been shown clearly to be of crucial importance for the identification and detection of the peroxide explosives.

Detection of trace peroxide explosives in environmental samples using solid phase extraction and liquid chromatography mass spectrometry

“…The characteristic ions for the identification of TATP and HMTD are consistent with those stated in the published literature (Crowson and Beardah, 2001;Widmer et al, 2002;Xu et al, 2004); these are the ammonium adduct 240.1442 m/z for TATP, formed with ammonium from the buffer in the mobile phase, and the molecular ion plus hydrogen, [MCH] C (209.0761 m/z) for HMTD. Further optimization of the instrument conditions and implementation of a mobile phase gradient could further lower the limits of detection, as well as testing methods on different LC-MS systems, including an instrument with a triple quadrupole.…”

“…There is also limited published research regarding suitable methodologies for the extraction, detection, and quantification of peroxide explosives and their precursor chemicals (Crowson and Beardah, 2001;Widmer et al, 2002;Xu et al, 2004;Song-im et al, 2012). Recent advances include methods for the direct detection of peroxide explosives from ambient surfaces without the need for any sample preparation (Cotte-Rodr ıguez et al, 2008;Rowell et al, 2012;Cooks et al, 2006), which is a very useful technique for in situ trace analysis at airports, for example; however, these techniques would not be suitable for wastewater analysis purposes where a cleanup and preconcentration stage would be essential.…”

Assessing a novel contact heater as a new method of recovering explosives traces from porous surfaces

“…Due to its ease of synthesis and the ready availability of its precursors, it has been implicated in an increasing number of explosion incidents. [3][4][5][6][7][8][9] Ethylene glycol dinitrate (EGDN) is a well-recognised explosive compound which has had a high level of historical use. [10] It is relatively rare to find traces of explosives in an everyday environment.…”

A Fast Liquid Chromatography Tandem Mass Spectrometric Analysis of PETN (Pentaerythritol Tetranitrate), RDX (3,5-Trinitro-1,3,5-triazacyclohexane) and HMX (Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine) in Soil, Utilizing a Simple Ultrasonic-Assisted Extraction with Minimum Solvent

“…Various screening and/or quantitation methods with different sensitivity levels as ion mobility spectrometry, 1 colorimetric methods, presented here. 15,[17][18][19][20] Various extraction methods, such as SPE, 18,21-24 SPME, 25 SFE, 26,27 are used in the literature. A large volume and sample is required for some of these techniques and multi-step procedures lead to a loss of analyte.…”