A method for the longitudinal sectioning of single hair samples

A simple technique is presented for the longitudinal sectioning of hair samples without the need for any embedding medium. The technique applies to single hair samples that are placed in a groove of a particular depth and can either be scraped or cut to the desired level. Planar sections are obtained that reveal the internal structure of the sample and are ideal for the application of surface analytical techniques for the study of internal transverse and longitudinal distributions of xenobiotics.     

Application of solid-phase microextraction to the profiling of an illicit drug: manufacturing impurities in illicit 4-methoxyamphetamine

This article describes the application of solid-phase microextraction (SPME) to the recovery of manufacturing by-products and impurities from an illicit drug seizure. The preparation chosen for examination using this technique contained 4-methoxyamphetamine, an hallucinogenic amphetamine that has been encountered frequently in South Australia. Compounds found in the PMA preparation included 4-methoxyphenol, 4-methoxybenzaldehyde, 4-methoxyphenyl-2-propanone, 4-methoxyphenyl-2-propanol, 4-methoxyphenyl-propene, and (tentatively) 4-methyl-5-(4'-methoxyphenyl) pyrimidine. The presence of these compounds suggests that the active drug was prepared from 4-methoxybenzaldehyde via 4-methoxyphenyl-2-propanone using a Leuckardt reductive amination. In this instance, SPME was found to be a simple, rapid, and non-destructive recovery technique that gave results complementary to those provided by conventional liquid-liquid extraction. There is an indication that SPME might find application in profiling of illicit drugs.     

A review of impurity profiling and synthetic route of manufacture of methylamphetamine, 3,4-methylenedioxymethylamphetamine,amphetamine, dimethylamphetamine and p-methoxyamphetamine

Amphetamine-type substances (ATS), like other synthetically derived compounds, can be produced by a multitude of synthetic pathways using a variety of precursors and reagents, resulting in a large number of possible contaminants (by-products, intermediates and impurities). This review article describes the common contaminants found in preparations of methylamphetamine (MA), 3,4-methylenedioxymethylamphetamine (MDMA), amphetamine (AP), N,N-dimethylamphetamine (DMA) and p-methoxyamphetamine (PMA) synthesised via common synthetic pathways including reductive amination, Leuckart method, Nagai method, Emde method, Birch reduction, “Moscow” method, Wacker process, “Nitrostyrene” method and the Peracid oxidation method.Contaminants can facilitate identification of the synthetic route, origin of precursors and may suggest information as to the location of manufacture of these illicit drugs. Contaminant profiling can provide vital intelligence for investigations in which linking seizures or identifying the synthetic pathway is essential. This review article presents an accessible resource; a compilation of contaminants resulting from a variety of manufacturing methods used to synthesise the most common ATS. It is important for research in this field to continue as valuable information can be extracted from illicit drug samples, increasing discrimination amongst ATS, and in turn, leading to an increase in evidential value and forensic drug intelligence from forensic drug samples.     

Use of styryl 11 and STaR 11 for the luminescence enhancement of cyanoacrylate-developed fingermarks in the visible and near-infrared regions

In current casework, most post-cyanoacrylate stains rely on luminescence emission in the visible region (400-700 nm). While traditional stains such as rhodamine 6G work well under most circumstances, some surfaces may generate background luminescence under the same conditions. Detection in the near-infrared region (NIR > 700 nm) has shown to be effective in minimizing the interferences from such surfaces. The laser dye styryl 11 generated strongly luminescent fingermarks when applied after cyanoacrylate fuming on all surfaces tested. When compared to rhodamine 6G, the dye was superior only when viewed in the NIR. Styryl 11 was subsequently combined with rhodamine 6G, and the mixed stain formulation (named StaR 11 by the authors) induced stronger luminescence compared with styryl 11 alone with an ability to visualize in both the visible and NIR regions. Reliable and consistent results were obtained when using either styryl 11 alone or the STaR 11 mixture. The enhancement achieved did not otherwise vary depending on the source of the fingermark secretions. With visualization possible in both the visible and NIR regions, the styryl 11/rhodamine 6G mixture showed significant potential as a post-cyanoacrylate stain.     

Screening of gunshot residues using desorption electrospray ionisation-mass spectrometry (DESI-MS)

Several studies have indicated that there are potential environmental sources of particles resembling inorganic primer found in gunshot residues (GSR); as a consequence examiners are reluctant to unambiguously assign the origin of inorganic particles. If organic gunshot residues (OGSR) were found in combination with inorganic particles, the possibility of environmental sources could be potentially eliminated, thereby significantly enhancing the strength of the evidence. Methods have been previously described whereby GSR specimens can be analysed for the presence of OGSR or inorganic GRS (IGSR). However, no methods have been reported that allow the analysis of both OGSR and IGSR on the same specimen. Described in this article is a direct method using desorption electrospray ionisation-mass spectrometry (DESI-MS) for the detection of methyl centralite (MC), ethyl centralite (EC) and diphenylamine (DPA) on adhesive tape GSR stubs typically used for scanning electron microscopy-energy-dispersive X-ray (SEM-EDX) analysis. The optimisation of numerous parameters was conducted using an experimental design. The results indicate that direct analysis of these organic components of GSR is possible although some limitations were also identified. This initial investigation has also indicated that subjecting stubs to DESI analysis does not interfere with subsequent SEM-EDX analysis of primer residues; therefore the technique described herein allows a comprehensive examination of GSR that would be highly probative in the event that both OGSR and IGSR are detected in the same specimen.     

Rapid determination of carbohydrates in heroin drug seizures using capillary electrophoresis with short-end injection

A simple and rapid method for the analysis of carbohydrates in heroin samples by capillary electrophoresis utilizing a borate complexation method is described. Separations were performed using an uncoated fused silica capillary, 50 cm x 50 micro I.D. x 360 microm O.D. with an effective separation length of 9 cm. The system was run at 60 degrees C with an applied voltage of -8 kilovolts. Injection of each sample was for 1 sec at -50 mbar. UV detection was employed with the wavelength set at 195 nm. The background electrolyte consisted of 65 mM borate, pH 12.0. Samples and standards were prepared in the run buffer containing 2 mg/mL of mannose as an internal standard. Under these conditions a test mixture containing glucose, sucrose, lactose, mannitol and mannose as an internal standard was resolved within 5 min. The method was used to determine the concentration of carbohydrates in heroin seizure samples and synthetic heroin samples. The results were in good agreement with the reported values.     

An investigation on the secondary transfer of organic gunshot residues

Gunshot residues (GSR) are an important forensic trace in firearm-related events. Currently, routine GSR analyses focus on the detection and characterisation of the inorganic components (IGSR). The increasing prevalence of heavy metal-free ammunition challenges these current protocols and there is an increasing interest in how the organic components of GSR (OGSR) can provide complementary information. Similar to the situation with IGSR, OGSR compounds originally deposited on the shooter during the firing process may further be transferred onto another individual or surface. Hence, the aim of this study was to provide additional information regarding the risk of a secondary transfer of OGSR. Two scenarios were investigated, the first one related to the arrest process and the possibilities of a secondary transfer arising between a shooter onto a non-shooter (e.g. between a police officer and a person of interest (POI)). The second scenario concerned the transfer of OGSR onto the non-shooter after handling a firearm for few minutes without discharging it. One calibre was chosen, the .40 S&W calibre, used by several Australian State police forces. A secondary transfer was observed in all cases for the two scenarios investigated, for three compounds of interest: ethylcentralite (EC), diphenylamine (DPA), N-nitrosodiphenylamine (N-nDPA). The firearm handling scenario resulted in a larger secondary transfer to that of the arrest scenario. Overall, the amounts of OGSR detected on the non-shooter were generally lower than that detected on the shooter and controls after the arrest scenario. The results of this study provide complementary knowledge about OGSR, which can be further used to improve the current practice and the interpretation of OGSR evidence. In particular, it highlights that the secondary transfer proposition must be considered during the interpretation of forensic findings, especially when small amounts of OGSR target compounds are detected.     

Fatal respiration of liquefied petroleum gas.

We have found that an efficient method of providing evidence of lethal solvent abuse is to sample headspace above lung tissue and then perform cryogenically focused gas-liquid chromatography. In the case presented, the level of lethal agent in lung tissue was low, but the solvent was present in abundance in the pleural cavity. We conclude that the pleural cavity acts as an efficient trap for aspirated substances.