No abstract

Desorption electrospray ionization - mass spectrometry (DESI-MS) is a useful technique for the qualitative analysis of compounds found in seized drug material. In this study, DESI-MS was utilized in the screening analysis of illicit cocaine samples. The technique was also applied to the geographical origin determination of these samples. The limit of detection was determined to be 24.3 µg (or 3.47 µg/mm(2) ) and the analysis time was less than 1 minute per sample. The intra-day and inter-day precision for the detection of cocaine was 11 % and 42 %, respectively; therefore the quantitative data provided by DESI-MS was limited in its use for accurate determination of cocaine concentration in a sample. Using the quadrupole time-of-flight (QTOF) mass spectrometer, the presence of cocaine and impurities detected were confirmed by accurate tandem MS data. The qualitative chemical profiles obtained using DESI-MS were compared to two popular analysis techniques, GC-MS and LC-MS. The effects of a range of adulterants including caffeine, procaine, levamisole, lignocaine, paracetamol, and atropine on the detectability of cocaine were also investigated. It was found that the addition of these adulterants in a cocaine sample did not prevent the detection of the analyte itself (there was slight enhancement in some samples), which was useful in drug detection. The detection of truxillines in the seized samples by DESI-MS aided in the preliminary determination of geographical origin, i.e., Bolivian, Peruvian or Colombian leaf origin. The application of DESI-MS to the qualitative analysis and screening of seized cocaine samples demonstrates the potential and applicability of the technique to the fast chemical profiling of illicit samples.

No abstract

This work has demonstrated the applicability of DESI-MS in the screening and profiling of MDMA, PMMA, BZP, TFMPP, mCPP, MeOPP as well as other complex mixtures.

PAPER Fu et al. Development and validation of a presumptive colour spot test method for the detection of piperazine analogues in seized illicit materials Development and validation of a presumptive colour spot test method for the detection of piperazine analogues in seized illicit materials

4-Methylmethcathione (4-MMC or mephedrone) is a prevalent drug of abuse globally. 4-MMC is often marketed as 'bath salts' and is readily available over the internet. The need for a rapid universal technique capable of detecting an extensive range of drug compounds has become increasingly important with the continued emergence of novel drug analogues. Desorption electrospray ionisation -mass spectrometry (DESI-MS) is a mass spectrometry technique that allows for the analysis of compounds directly from ambient surfaces, reducing or eliminating the need for sample preparation. Although 4-MMC has gained significant attention in recent years, the application of the DESI-MS technique to the fast presumptive detection and chemical analysis of this analogue has not been presented. In the present study, DESI-MS was applied to the rapid qualitative analysis of 4-MMC. A particularly suitable surface, semi-porous polytetrafluoroethylene (PTFE, Teflon) was utilised, as it generated the least variable signal and reproducibility compared to other surfaces (polymethyl-methacrylate (PMMA) and polyvinyl chloride (PVC)). Selectivity of the technique to the detection of 4-MMC was evaluated by analysing a range of adulterated samples including mixtures containing caffeine, methylamphetamine, cathinone and paracetamol. Specificity based on tandem MS (MS/MS) was also demonstrated by analysing substances with the same molecular formula as 4-MMC. Accuracy (% RE) and precision (% RSD) of the method were found to be within 13% and 38%, respectively; and therefore the quantitative data provided by the DESI-MS method is limited compared to gas chromatography-mass spectrometry (GC-MS; accuracy < 13% and precision < 12%). The results suggest that DESI-MS can greatly aid in the rapid presumptive identification of 4-MMC and other similar novel drug analogues.

In further work investigating the intriguing application of diacetylene copolymers in fingermark detection, methods were developed to control (inhibit or enhance) the diacetylene polymerization reaction in fingermarks treated with a mixture of the monomers 2,4-hexadiyne-1,6-bis-(phenylurethane) (HDDPU) and 2,4-hexadiyne-1,6-bis(p-chlorophenylurethane) (HDDCPU) in acetone solution. These methods included the use of a humidity chamber to reduce the amount of background development while promoting development on the fingermark, subjecting developed fingermarks to freezing temperatures and using a solvent to remove unreacted monomer in order to inhibit the polymerization reaction. Developed fingermarks were enhanced by conventional lighting (white light, filtered light) and fast Raman mapping, which was shown to be advantageous over FTIR imaging. This study also demonstrated the applicability of diacetylene copolymer solutions in the covert detection of fingermarks on difficult surfaces. Furthermore, fingermarks were successfully developed with good ridge detail on pig skin (used as a model for human skin, a notoriously difficult surface on which to develop fingermarks).

No abstract