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)

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Field, Jennifer K. and Hinz, Christine and Titman, Christopher M. and Hulme, Matthew C. and Cowan, Rhona M. and Ainsworth-McMillan, Jack B. and Gilbert, Nicolas and Lee, Robert J. and Marron, Jack and Costello, Andrew and Mewis, Ryan E. and Euerby, Melvin R. and Sutcliffe, Oliver B. (2022) 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). Journal of Pharmaceutical and Biomedical Analysis, 216. 114798. ISSN 1873-264X (https://doi.org/10.1016/j.jpba.2022.114798)

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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 (t G = 10 min) protocol was applied to confirm the identity of the psychoactive components within four seized bulk samples provided by law enforcement.

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