Guilty by dissociation: Part A: Development of a rapid Ultra-High Performance Liquid Chromatography (UHPLC)-MS/MS methodology for the analysis of regioisomeric diphenidine-derived Novel Psychoactive Substances (NPS).
Jennifer K Field, Christine Hinz, Christopher M Titman, Matthew C Hulme, Rhona M Cowan, Jack B Ainsworth-Mcmillan, Nicolas Gilbert, Robert J Lee, Jack Marron, Andrew Costello, Ryan E Mewis, Melvin R Euerby, Oliver B Sutcliffe
Journal of pharmaceutical and biomedical analysis July 15, 2022 DOI: 10.1016/j.jpba.2022.114798 via PubMed
Summary
AI-generated from the abstractA rapid UHPLC-MS/MS method can detect and confirm 33 different diphenidine derivatives in solid drug samples. The method separates compounds based on the position and type of chemical substituents on the phenyl ring, and it works even when common adulterants are present. The 10-minute protocol was successfully used to identify psychoactive components in four seized drug samples from law enforcement.
Study at a glance
| Characteristics | Method development and validation Peer reviewed |
|---|---|
| Population | 33 substituted diphenidine derivatives synthesized in-house and four seized bulk drug samples |
| Keywords | Diphenidines Forensic Illicit drugs Novel psychoactive substances Regioisomers |
| Citations | 4 |
| Key finding | A rapid UHPLC-MS/MS method was developed to detect and confirm 33 substituted diphenidine derivatives, and it was applied to identify psychoactive components in four seized drug samples. |
Abstract
This study describes the first reported development of a rapid, generic gradient Ultra-High Performance Liquid Chromatography (UHPLC) methodology with targeted triple quadrupole MS/MS using electrospray positive ionisation to detect and unambiguously confirm the identity of 33 substituted 1, 2-diarylethamine (or diphenidine) derivatives in solid drug samples. The in-house synthesised library included a range of derivatives possessing either electron donating/withdrawing substituents, commonly included in combinatorial libraries, of varying size and lipophilicity on the phenyl ring. These test probes were used to investigate if their order of elution and that of their regioisomers were dependent on the position and type of the substituent on the phenyl ring. In addition, investigations into the retention mechanism of the diphenidines under reverse-phase UHPLC conditions were undertaken. Common adulterants found within seized bulk samples were assessed to prove that the methodology was specific, and the developed UHPLC-MS/MS (tG = 10 min) protocol was applied to confirm the identity of the psychoactive components within four seized bulk samples provided by law enforcement.