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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