Systematic analytical characterization of new psychoactive substances: A case study

Abstract

New psychoactive substances (NPS) are synthesized compounds that are not usually covered by European and/or international laws. With a slight alteration in the chemical structure of existing illegal substances registered in the European Union (EU), these NPS circumvent existing controls and are thus referred to as "legal highs". They are becoming increasingly available and can easily be purchased through both the internet and other means (smart shops). Thus, it is essential that the identification of NPS keeps up with this rapidly evolving market. In this case study, the Belgian Customs authorities apprehended a parcel, originating from China, containing two samples, declared as being "white pigments". For routine identification, the Belgian Customs Laboratory first analysed both samples by gas-chromatography mass-spectrometry and Fourier-Transform Infrared spectroscopy. The information obtained by these techniques is essential and can give an indication of the chemical structure of an unknown substance but not the complete identification of its structure. To bridge this gap, scientific and technical support is ensured by the Joint Research Centre (JRC) to the European Commission Directorate General for Taxation and Customs Unions (DG TAXUD) and the Customs Laboratory European Network (CLEN) through an Administrative Arrangement for fast recognition of NPS and identification of unknown chemicals. The samples were sent to the JRC for a complete characterization using advanced techniques and chemoinformatic tools. The aim of this study was also to encourage the development of a science-based policy driven approach on NPS. These samples were fully characterized and identified as 5F-AMB and PX-3 using (1)H and (13)C nuclear magnetic resonance (NMR), high-resolution tandem mass-spectrometry (HR-MS/MS) and Raman spectroscopy. A chemoinformatic platform was used to manage, unify analytical data from multiple techniques and instruments, and combine it with chemical and structural information.

Current applications of high-resolution mass spectrometry for the analysis of new psychoactive substances: a critical review

“…Furthermore, in silico fragmentation can be performed to assess whether the postulated structure's experimental and theoretical fragmentation correlate. This has been performed using software such as Mass Frontier™ (Thermo Fisher Scientific) [82,98] and Molecular Structure Correlator (MSC, Agilent Technologies) [47].…”

Identification and characterization of a putative new psychoactive substance, 2‐(2‐(4‐chlorophenyl)acetamido)‐3‐methylbutanamide, in Spain

“…This drug is widely used because of its fast onset, long duration of the narcotic effects and low toxicity. [5,9,10] In recent years, the potential for abuse and dependence of propofol has increasingly been reported in literature as it can provoke euphoria, relaxation, sexual hallucinations, and disinhibition; it is also used for suicidal purposes. [6][7][8] Self-injection of propofol without medical control is very dangerous and can have lethal consequences.…”

“…[7] Forensic laboratories, universities, research institutes, public health centres and law enforcement agencies play an important role in monitoring these types of substances, which are also encountered in customs seizures and medical emergencies. [4,[10][11][12] Moreover, HRMS allows screening analyses without reference standards being available (tentative identification). Gas chromatography coupled to mass spectrometry (GC-MS) using electron ionization (EI) is a fast and reliable technique for the identification of these compounds based on the use of spectral libraries.…”

“…[9] However, fragmentation spectra of novel NPS may not be available. [10] Nuclear magnetic resonance (NMR) spectroscopy has proved to be one of the most powerful techniques for the structural elucidation and characterization of organic molecules, and has been applied to the identification and characterization of synthetic cannabinoids [17] and synthetic cathinones. Liquid chromatography (LC) coupled to high-resolution MS (HRMS) has proven to be a powerful technique for the screening of NPS in legal highs samples.…”

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

“…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.…”