Mathieu Elie

An analysis of legal highs—do they contain what it says on the tin?

In recent years the availability of so-called legal highs over the Internet has hugely increased. Numerous online legal-high retailers market a broad variety of products which are advertised as research chemicals, bath salts, or plant food although clearly intended for human consumption as recreational drug replacements. No guidelines exist as to what is sold and in what purity. Consumers are led to believe that purchased goods are entirely legal. In this study, several legal-high products were purchased and analyzed for their content. The powdered products were screened with attenuated total reflectance-Fourier Transform Infrared (ATR-FTIR) followed by gas chromatography-mass spectrometry (GC-MS) analysis of methanol extracts. Spectra were compared to reference standards and the NIST library. Results showed that 6 out of 7 products did not contain the advertised active ingredient. Moreover, five samples contained the controlled substances benzylpiperazine and 1-[3-(trifluoromethyl)phenyl]piperazine combined with caffeine.

Enhancement of Microcrystalline Identification of γ-Hydroxybutyrate*

Abstract: An enhancement of the microcrystalline test for the detection of γ‐hydroxybutyrate (GHB) is described. The original test used a silver/copper reagent which consisted of 0.1 g of silver nitrate and 0.1 g of copper nitrate in 10 mL water. The enhanced test utilizes lanthanum nitrate in place of copper nitrate. A detection limit of 0.5 mg/mL was achieved and the visual discrimination was improved because of larger sized crystals. Transient crystals were observed between 0.1 and 0.4 mg/mL. Silver nitrate alone appeared to be suitable for GHB detection but was not specific as other hydroxyl acids, such as glycolic acid, produced a similar crystal pattern. Tests conducted on chemical precursors of GHB and substances with similar biological activity highlight the specificity of the enhanced test. The reagent is therefore selective and sensitive for GHB in aqueous solutions. However, in beverage testing, crystal formation appeared to be inhibited for some drinks. Citric acid was identified as a possible interference depending on its concentration relative to GHB.

E-cigarettes: controversies within the controversy

10 years have passed since e-cigarettes were first marketed in the UK. Since then, e-cigarettes have engendered substantial controversy in the realms of public health and respiratory medicine.

Reversing microcrystalline tests—An analytical approach to recycling of microcrystals from drugs of abuse

A combined analysis of microcrystalline tests followed by LC-MS or GC-MS analysis is described. Microcrystalline tests are shown to be non-destructive as addition products formed were easily dissociated after the application of an appropriate solvent. Subsequent analysis of the sample was done to quantify the recovery of the drug. Examples were performed using the date rape drug γ-hydroxybutyrate (GHB) and the synthetic opioid methadone.

E-cigarettes: further flavours of controversy within the controversy

Although some observers have alluded to an emerging public health consensus in the UK regarding the potential for e-cigarettes to reduce tobacco-related harms, controversy emerged when major UK public health organisations seemed to send out conflicting messages regarding the devices. The Royal College of Physicians (RCP) in February, 2016, advocated that it was important to promote e-cigarettes “as widely as possible as a substitute for smoking in the UK”. However, the National Institute for Health and Clinical Excellence, in draft guidance published in September, 2017, suggested clinicians should advise that, although some smokers have found e-cigarettes helpful to quit smoking, “there is currently little evidence on the long-term benefits or harms of these products”.

Preventing misidentification of 25I-NBOH as 2C-I on routine GC–MS analyses

Abstract25I-NBOH is a novel psychoactive substance (NPS) recently reported to have been found on blotter paper samples seized on the streets of Brazil, and used as a replacement for the NBOMes now scheduled in many countries. The presence of this NPS on the street market may go undetected, because the most widely and routinely utilised analytical technique for drug sample analyses is gas chromatography–mass spectrometry (GC–MS), which can misidentify 25I-NBOH (and indeed the other members of the NBOH series), because of its degradation into 2C-I (and corresponding 2C for the other members of the series) within the injector, unless a derivatization procedure is employed, which is often non-standard. While direct detection of 25I-NBOH under routine GC–MS conditions is still achieved, a slight adjustment in the standard GC–MS method, including shortening of the solvent delay window, was found to enable the detection of an additional peak due to 25I-NBOH degradation. Consequently, the presence of this secondary early chromatographic peak allowed for the distinction between 25I-NBOH and 2C-I using routine GC–MS without resorting to derivatization (or other analytical processes), thus preventing misidentification of 25I-NBOH as 2C-I.

The isolation and characterisation of the synthetic cannabinoid AM-2201 from commercial products using purification by HPLC-DAD

Abstract A total of six products containing legal highs were purchased via the internet from the UK- based retailers and screened for the presence of synthetic cannabinoids using a fast GC-MS method and identified, in the absence of reference materials, by comparing the mass spectra with the Scientific Working Group for the Analysis of Seized Drugs (SWGDRUG) mass spectral library. Four synthetic cannabinoids were detected: RCS-4, CP-47, 497, UR-144 and AM-2201. The active ingredient (1-(5-fluoropentyl)-3-(1-naphthoyl) indole), with the street name AM-2201, detected in the product named Doob was isolated and purified from the methanolic extract of the product using preparative HPLC with analytical column (column overloading method). The structure of the substance was confirmed using NMR. This approach used common analytical equipment found in forensic and other analytical laboratories (except for the NMR), therefore can be useful for the identification of unknown psychoactive substances in drugs of abuse.

Cleaning of metals contaminated with historic pesticide residues that are hazardous to health

AbstractThere is an increasing awareness of the risks that some collections can present, including the dangers posed by some historic household pesticides. Mr Straws House in Worksop, Nottinghamshire, is an Edwardian semi-detached home owned by the National Trust and contains everyday items from the 1900s to 1980s. Amongst the collections in the property were a number of gardening chemicals and containers with unidentified contents. It was recognised that some of these chemicals may pose a health risk to staff and visitors if unidentified and mishandled. In collaboration with the University of Lincolns Conservation Department, the contents of containers were identified where possible using Fourier transform infrared spectroscopy (FTIR), fast gas chromatography mass spectrometry (GCMS) and X-ray fluorescence (XRF), and the containers conserved following an agreed treatment protocol. This article discusses the hazards of removing pesticide materials and residues from containers (mainly metal), and the ext...

Investigation into the suitability of capillary tubes for microcrystalline testing

A comparison between microcrystalline tests performed on microscope slides and flat capillary tubes with inner diameters ranging from 0.1 to 0.7 mm was carried out to explore the appropriateness of tubes for rapid testing of suspected drugs of abuse in the laboratory as well as in the field. Tests for mephedrone, cocaine, and phencyclidine were chosen as examples to investigate the handling of the capillary tubes, the influence on crystal habit, size, and the effects on the limit of detection. Image stacking software was used to increase the depth of field of micrographs taken from developed microcrystals greatly enhancing the interpretability even months after carrying out the microcrystalline test. Additionally, the potential of seeding capillary tubes with a reagent was studied. Pre-treatment of tubes would allow microcrystalline tests to be carried out quicker and anywhere without the necessity of taking along expensive and hazardous reagents. The sealing of capillary tubes containing developed microcrystalline tests in order to preserve results for a long period of time was successfully done by applying paraffin wax to the open ends. Finally, it was concluded that capillary tubes are suitable vessels for performing microcrystalline tests. The increased portability of the improved set-up allows tests to be safely executed outside laboratories without impairing the quality of the result. Findings were applied to six legal high samples purchased online between May and August 2011. The active ingredients like MDAI as well as cutting agents like caffeine were successfully identified using the microcrystalline test technique in capillary tubes.