Development and validation of a GC–MS/MS method for the determination of 11 amphetamines and 34 synthetic cathinones in whole blood

Abstract

Purpose Psychoactive compounds that contain a phenylethylamine structure (such as amphetamine-type stimulants and synthetic cathinones) are one of the major classes of stimulants on the recreational drug market. Approximately 670 new psychoactive substances (NPS) are monitored only in Europe; however, new psychoactive compounds are being developed for illicit trade each year. In this context, the development of new analytical procedures for the determination of such compounds in biological specimens for forensic toxicology is of great importance. Methods Gas chromatography-tandem mass spectrometry (GC-MS/MS) technique was applied for analysis of amphetamines and synthetic cathinones. The volumes of 200 µL of each whole blood sample and 1 mL of liquid-liquid extraction solvent were used for extraction, followed by pentafluoropropionyl derivatization. Results A high-throughput, robust, rapid, and sensitive procedure involving a simple liquid-liquid extraction for the simultaneous determination of 45 amphetamine-type stimulants and synthetic cathinones in whole blood was developed. The assay was validated based on its recovery (83.2-106%), interday accuracy (89.0-108%), and interday precision (≤ 8.1%). In view of the low limits of detection (ranged between 0.02 and 0.72 ng/mL) and limits of quantification (1 and 2.5 ng/mL), the developed method can serve as a less expensive and more ecologically friendly alternative to the liquid chromatography-tandem mass spectrometric methods. Conclusions To the best of our knowledge, this is the first work presenting a GC-MS/MS method for the determination of NPS in blood samples. The presented procedure was applied to authentic samples from forensic cases, demonstrating its utility in the quantification of a wide number of psychoactive substances in routine toxicological analyses. The developed procedure can also be easily expanded to additional compounds. Keywords Amphetamine-type stimulants (ATSs) • Synthetic cathinones • Whole blood • GC-MS/MS Prof. Jacek Namieśnik passed away on 14 April 2019. He will always remain in our memory.

Stability of synthetic cathinones in clinical and forensic toxicological analysis—Where are we now?

“…In the case of SCs, the vast majority of these methods has been conducted by means of LC–MS, 1,12,31–35,37,38,40–46,48–50 with the exception of the method described by Busardò et al, 37 Alsenedi and Morrison, 39 and Woźniak et al, 51 in which SCs and related metabolites were analyzed by gas chromatography–MS (GC–MS).…”

“…In the literature, the experimental design for reporting the stability of SCs is highly variable. For example, whereas the majority of authors used two levels of concentration, 1,12,33,39,40,43,45,46,48–50 few authors used three 51 or four 35 . Although analyte stability is recommended to be assessed at two concentration levels as described before, a number of authors used only one concentration 31,32,34,36,37,41,43,44 .…”

New psychoactive substances: a review and updates

“…Synthetic cathinones are similar in structure to amphetamine type stimulants and are chemically referred to as β-ketone analogues because of the carbonyl (=O) group in β carbon. 38 , 39 The common pharmacophore group responsible for the psychoactive effect observed in synthetic stimulants is phenethylamine, 32 and its derivatives are reported to represent at least 37% of the NPS available on the illicit drug market. 40 …”

The influence of lateral flake size in graphene/graphite paste electrodes: an electroanalytical investigation

“…27 There is a need for the development of quick, accurate, simple and cost effective sensors for the detection and quantication of such abused drugs. Current methods utilised for the determination of cocaine and amphetamines include powerful but complex equipment and require experienced experimentalists; such as, chromatography-tandem mass spectrometry (LC-MS and GC-MS), [28][29][30][31] spectrouorimetry 32 and nuclear magnetic resonance spectroscopy (NMR). 33 Although these analytical techniques are sensitive, reliable and precise, they do however require expensive instrumentation, are labour intensive (extensive sample preparation) and thus are not available in all laboratories for routine analysis.…”