Development of gas chromatography–mass spectrometry (GC–MS) and other rapid screening methods for the analysis of 16 ‘legal high’ cathinone derivatives

Daéid, Niamh Nic; Savage, Katy; Ramsay, Donna L.; Holland, Ciara; Sutcliffe, Oliver B.

doi:10.1016/j.scijus.2013.08.004

Cited by 35 publications

(27 citation statements)

References 7 publications

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“…A range of chromatographic techniques including High Performance Liquid Chromatography (HPLC) and Gas Chromatography-Mass Spectrometry (GC-MS) have been applied to the detection of synthetic cathinones by many groups, 4,5,[8][9][10][11][12][13][14][15][16][17][18][19][20][21][22][23][24][25][26][27] however electrochemistry is advantageous as an analytical tool being sensitive, selective as well as low cost and having the potential to be scaled down to a portable device. [28][29][30][31][32][33][34] Previous work 2,34 has reported novel electroanalytical sensing protocols developed towards the electrochemical oxidation 34 in light of the scarcity of coins minted pre-1992.…”

Section: Introductionmentioning

confidence: 99%

Regal electrochemistry: sensing of the synthetic cathinone class of new psychoactive substances (NPSs)

et al. 2015

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In this paper the concept of 'Regal Electrochemistry' is expanded towards the electrochemical sensing of Novel Psychoactive Substances (NPSs) namely synthetic cathinone derivatives where British coinage is used as the electrochemical sensor. In this proof-of-concept approach, the electrochemical sensing of mephedrone (4-MMC) and 4'methyl-N-ethylcathinone (4-MEC) is shown to be possible using a British 1 pence coin for the first time. This novel electrochemical protocol is validated towards the detection of cathinone derivatives in a seized street sample that has been independently analysed via high performance liquid chromatography demonstrating its potential use as a novel electrochemical sensor for NPSs.

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Section: Introductionmentioning

confidence: 99%

Regal electrochemistry: sensing of the synthetic cathinone class of new psychoactive substances (NPSs)

et al. 2015

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“…Adamowicz et al measured the concentration of α‐PVP in 66 forensic specimens using LC/MS, which showed the levels ranging widely from 1.1 to 6200 ng mL −1 . Gas chromatography (GC)/MS is an alternative for confirming the presence of α‐PVP and its derivatives, since the mass spectra generated using electron ionization under specific conditions (70 eV) have high reproducibility . To compensate for the principal limitation of GC/MS, sample concentration to improve method sensitivity and derivatization to increase the thermal stability and volatility of the analytes are commonly coupled to GC/MS.…”

Section: Introductionmentioning

confidence: 99%

Determination of synthetic cathinone α‐pyrrolidinovalero‐phenone and its metabolite in urine using solid‐phase extraction and gas chromatography–mass spectrometry

Cheng

Hsieh

Chen

et al. 2020

Rapid Comm Mass Spectrometry

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Rationale The presence of α‐pyrrolidinovalerophenone (α‐PVP) and its metabolites in urine is evidence of the administration of α‐PVP. A toxicological challenge is that the metabolites of α‐PVP exhibit amphoteric properties, which make them unsuitable for detection using gas chromatography–mass spectrometry (GC/MS). In the study reported, proper derivatization and sample extraction were essential for improving the sensitivity for GC/MS analysis. Methods An automated solid‐phase extraction (SPE) method has been developed and optimized. The derivatization efficiency was tested using longer reaction time and the addition of polar pyridine into a mixture of N,O‐bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane. Method validation, including linearity, limit of detection, precision, accuracy, and recovery, was evaluated using automatic SPE and GC/MS. Results The results suggested that adding pyridine to BSTFA (1:1, v/v) significantly improved derivatization efficiency and precision. After optimization, the linear range was from 25 to 1000 ng mL−1 with R2 > 0.9950. The limit of detection was 5 ng mL−1 for α‐PVP and 25 ng mL−1 for OH‐α‐PVP. The recovery for SPE was over 88%. The inter‐day and intra‐day precisions were less than 15%. A forensic sample has been found containing α‐PVP (67.3 ng mL−1) and OH‐α‐PVP (560.2 ng mL−1). Conclusions This study is the first to validate an auto‐SPE‐GC/MS method for the quantification and qualification of α‐PVP and OH‐α‐PVP in urine. We have successfully improved the derivatization efficiency and developed a sensitive and semi‐automatic approach. This approach is desirable for the detection of synthetic cathinone at trace levels in biological samples.

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“…Favoured separation techniques are gas and liquid chromatography (GC and LC) which are typically hyphenated with MS . However, the hyphenation of chromatography techniques with non‐mass spectral detectors has been successfully investigated over the last years.…”

Section: Introductionmentioning

confidence: 99%

Microcrystalline testing used in combination with Raman micro‐spectroscopy for absolute identification of novel psychoactive substances

Elie

Cave

et al. 2016

J Raman Spectroscopy

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Two new psychoactive substances, namely 4-methylmethcathinone (mephedrone) and 5,6-methylenedioxy-2-aminoindane (MDAI) were analysed with a novel combination of microcrystalline tests followed by Raman micro-spectroscopy to facilitate their absolute identification. The discrimination power of the proposed combination was successfully demonstrated through the analysis of the positional isomers 2-and 3-methylmethcathinone. The addition of mercury dichloride as a microcrystalline test reagent produced specific microcrystals of each tested analyte. The robustness of the method was evaluated in the presence of common cutting agents (caffeine and benzocaine) as well as on street samples. The crystal lattice structures of mephedrone, 2-methylmethcathinone and MDAI mercury dichloride microcrystals were determined by single crystal X-ray diffraction. This confirmed the presence of both drug and reagent together in the lattice and accounts for the distinct habit of the observed microcrystals. Raman spectra of the formed microcrystals differed from those obtained from their standard salt form by loss and/or gain of some vibrational modes. Particularly important was the appearance of the mercury chloride link to each tested drug molecule which showed as strong bands at low wavenumbers. Its presence was corroborated by its detection in the crystal lattice. It was therefore concluded that microcrystalline testing followed by Raman micro-spectroscopy satisfies the technique combination requirement for psychoactive substances recommended by the Scientific Working Group for the Analysis of Seized Drugs (SWGDRUG) and provides a rapid and cheap analysis route. The proposed technique combination also aids the development of new microcrystalline tests as it allows for confirmation of the uniqueness of the developed microcrystals almost in-situ rather than growing single crystals for often long periods of time needed for single crystal X-ray diffraction analysis.2

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Development of gas chromatography–mass spectrometry (GC–MS) and other rapid screening methods for the analysis of 16 ‘legal high’ cathinone derivatives

Cited by 35 publications

References 7 publications

Regal electrochemistry: sensing of the synthetic cathinone class of new psychoactive substances (NPSs)

Regal electrochemistry: sensing of the synthetic cathinone class of new psychoactive substances (NPSs)

Determination of synthetic cathinone α‐pyrrolidinovalero‐phenone and its metabolite in urine using solid‐phase extraction and gas chromatography–mass spectrometry

Microcrystalline testing used in combination with Raman micro‐spectroscopy for absolute identification of novel psychoactive substances

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