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.

A microcrystalline test for the detection of 4-methylmethcathinone (mephedrone), benzylpiperazine (BZP) and 5,6-methylenedioxy-2-aminoindane (MDAI) using aqueous solutions of mercury chloride is described. Each of the compounds investigated formed specific drug-reagent crystals within minutes. The uniqueness of the test was confirmed by comparison of the microcrystalline response to that of other psychoactive stimulants and a common cutting agent. The limit of detection and cut-off levels for reference standards were established to 3 g/L and 5 g/L for mephedrone, 0.5 g/L for MDAI and 0.2 g/L and 0.3 g/L for BZP, respectively. Various mixtures of standards of either mephedrone, BZP or MDAI combined with caffeine were investigated for their microcrystalline response. Results showed that simultaneous detection of drug and cutting agent was possible with the concentrations tested but were dependant on the ratio of drug to cutting agent. BZP could be detected alongside caffeine from as low as 20 % (v/v), MDAI from 40 % (v/v) and mephedrone from 50 % (v/v) and higher. Finally, seven samples of online purchased 'legal highs' were analysed using the developed test and the findings were compared to FTIR and GC-MS results. It was shown that 6 out of 7 samples did not contain the advertised active ingredient. Five samples consisted of BZP, caffeine and 1-[3-(Trifluoromethyl)phenyl]piperazine (3-TFMPP). The microcrystalline tests carried out on these samples showed positive results for both BZP and caffeine without interference from other substances present.

The continuous appearance of novel psychoactive substances (NPS) in legal high products presents a challenge for the routine analytical laboratory. A rapid screening method for NPS analysis using fast gas chromatography mass spectrometry (fast GC-MS) is presented. Twenty-three analytes, including 5-iodo-2-aminoindane (5-IAI), 1-(thiophen-2-yl)-2-methylaminopropane (MPA), 1-benzylpiperazine (BZP), 4-methylmethcathinone (mephedrone), 5,6-methylenedioxy-2-aminoindane (MDAI) and methoxetamine (MXE) were separated within 4 min. The method was used to analyze 35 Internet and head shop purchased 'legal high' products with the successful identification of their active ingredients. As previously observed, legal high products do not always contain their stated ingredients. Of the group of products purchased as 5-IAI not one contained 5-IAI with several containing mixtures of substances either already controlled in the UK or under consideration by the Advisory Council on Misuse of Drugs (ACMD). The low bleed and high inertness of the chromatography column used ensured clean high quality mass spectrometry data which when combined with the short run time resulted in an efficient tool for NPS screening, even when standards were unavailable. Electron impact and chemical ionization mass spectra used in combination for the identification of unknown NPS are presented.

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25I-NBOH is a novel psychoactive substance (NPS) recently reported to have been found on blotter paper samples seized on the streets of Brazil, 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 chromatographymass 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 conditions is still to be achieved, slight adjustments in standard GC methods, including shortening of the solvent delay window, enabled the detection of an additional peak containing 25I-NBOH degradation product's fragmentation ions. Consequently, 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. Keywords 25I-NBOH • 2C-I • NPS • Misidentification • Thermal degradation • GC-MS

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Drug detection in the forensic context requires numerous analytical techniques. Depending on locally adopted standard procedures, different techniques are used for screening solid samples for potential illicit substances (e.g. Fourier transform infrared spectroscopy (FTIR)). A sample suspected of containing prohibited material passes through another layer of techniques to confirm that the illegal substance is present and to identify it (e.g. liquid/gas chromatography). Finally, the drug is systematically quantified (e.g. mass spectrometry). Microcrystalline tests fall within the second step of this analytical process. They are low cost because of the minute amount of reagents used and the simplicity of the instrumentation and consumables required to perform the analysis. They offer all the features required by a good confirmation technique while being very fast to administer and interpret, although they do not offer quantification capabilities. Microcrystalline tests are chemical tests resulting in the formation of unique microcrystals for a given substance when combined with a specific reagent. Microcrystals are observed under a microscope and micrographs or microvideos constitute the results of the test. Thanks to the chemical mechanism by which microcrystals develop, microcrystalline tests can be applied to molecules of various sizes, shapes, charges, and with different functional groups, and can naturally distinguish between enantiomers.