Separation and Identification of Isomeric and Structurally Related Synthetic Cannabinoids Using 2D Liquid Chromatography and High Resolution Mass Spectrometry

• NCJ Number: 254239
• Journal: Journal of Analytical Toxicology Volume: 43 Issue: 3 Dated: 2019 Pages: 170-178
• Author(s): Melanie N. Eckberg; Luis E. Arroyo-Mora; Dwight R Stoll; Anthony P. DeCaprio
• Date Published: 2019
• Length: 9 pages
• Grant Number(s): 2014-R2-CX-K006
• Agencies: NIJ-Sponsored
• Publication Type: Research (Applied/Empirical); Report (Study/Research); Report (Grant Sponsored); Program/Project Description
• Award: Forensic Toxicological Screening/Confirmation of 500+ Designer Drugs by LC-QTOF-MS and LC-QqQ-MS Analysis

Annotation

Since 2D liquid chromatography (2D-LC) has demonstrated applicability in difficult separations of small molecules and compounds in complex mixtures, the current study tested the hypothesis that this technique could also be used to separate co-eluting isomeric and structurally related, non-isomeric NPS, including synthetic cannabinoids (SC).

Abstract

Novel psychoactive substances (NPS) are emerging drugs of abuse that are variations of existing compounds intended to cause a CNS psychotropic effect. Some NPS are so comparable in structure and physicochemical properties that they co-elute using traditional single column chromatographic techniques and therefore will not be detected as individual compounds. In the current research project, initial studies assessed several parameters, including column type, mobile phase, analysis time, gradient and flow rate, to optimize a 2D-LC method for separation and analysis of SC. The final comprehensive on-line 2D-LC method employed a Bonus-RP column in the first dimension (1D) coupled with UV detection and a biphenyl column in the second dimension (2D) coupled with QTOF-MS detection in full scan positive mode. To test the utility of the method, three SC mixes were created, each containing five compounds that were unresolvable in a traditional, 1D-LC separation, one mix with isomeric compounds and two with structurally related but non-isomeric compounds. Contour plots of UV absorbance in 1D and MS ion intensity in 2D demonstrated that all components in each mixture were successfully resolved using the 2D-LC separation method. This research serves as proof-of-concept for the application of 2D-LC to the separation of isomeric and structurally related SC. With further optimization and validation, 2D-LC may be a generally useful tool for separation of complex mixtures of NPS. (publisher abstract modified)