Guilty by dissociation—development of gas chromatography–mass spectrometry (GC-MS) and other rapid screening methods for the analysis of 13 diphenidine-derived new psychoactive substances (NPSs)

Abstract

The prevalence of new psychoactive substances (NPSs) in forensic casework has increased prominently in recent years. This has given rise to significant legal and analytical challenges in the identification of these substances. The requirement for validated, robust and rapid testing methodologies for these compounds is obvious. This study details the analysis of 13 synthesised diphenidine derivatives encountered in casework using presumptive testing, thin layer chromatography and gas chromatography-mass spectrometry (GC-MS). Specifically, the validated GC-MS method provides, for the first time, both a general screening method and quantification of the active components for seized solid samples, both in their pure form and in the presence of common adulterants. Graphical Abstract Chemical synthesis and forensic analysis of 13 diphenidine-derived new psychoactive substance(s).

Syntheses and analytical characterizations of the research chemical 1‐[1‐(2‐fluorophenyl)‐2‐phenylethyl]pyrrolidine (fluorolintane) and five of its isomers

“…The reactions generally utilize convenient low‐cost reagents to produce final compounds in moderate to excellent yields. This method was utilized previously to prepare other 1,2‐diarylethylamines such as 2‐MXP and 2‐Cl‐DPP and a range of other diphenidine analogs . Finally, during final preparation of HCl salts, it was noticed via NMR that these crystals can form solvate co‐crystals with methanol, ethanol, and isopropanol to differing degrees which led to the decision to employ acetone as the recrystallization solvent.…”

Chromatographic retention behaviour, modelling and optimization of a UHPLC-UV separation of the regioisomers of the Novel Psychoactive Substance (NPS) methoxphenidine (MXP)

“…Geyer et al has recently published a validated GC-(EI)-MS protocol for the qualitative and quantitative analysis of thirteen diarylethylamine derivatives (including 2-MXP and its isomers) in seized powder sampleshowever, the published method has significant limitations in terms of overall analysis time (circa. 45 mins) [11]. This HPLC method provides, for the first time, both a general screening method and quantification of the active components for seized solid samples of methoxphenidine, which is significantly superior to the previously reported GC-MS [11] and HPLC [6,10] methods in terms of overall run time (7 mins) and resolution of the regioisomers.…”

“…45 mins) [11]. This HPLC method provides, for the first time, both a general screening method and quantification of the active components for seized solid samples of methoxphenidine, which is significantly superior to the previously reported GC-MS [11] and HPLC [6,10] methods in terms of overall run time (7 mins) and resolution of the regioisomers.…”

Detection of newly emerging psychoactive substances using Raman spectroscopy and chemometrics

“…In the last decade there has been an increasingly large and rapid appearance of newly emerging drugs, with more than 700 currently monitored. [1][2][3] In most cases, this can be attributed to efforts by suppliers to evade their detection and circumvent existing legislation. 1,4 This rapid appearance, poor detectability, increased potency and availability of newly emerging drugs is oen accompanied by an increase in reported health harms, emergency department visits and even fatalities, making NPS a major public health concern.…”