Differentiation of ring‐substituted regioisomers of amphetamine and methamphetamine by supercritical fluid chromatography

Abstract

Chromatographic differentiation of the ring-substituted regioisomers of amphetamine (AMP) and methamphetamine (MA) was performed by supercritical fluid chromatography (SFC). The behaviour of the retention against the changes of column temperature and co-solvent proportion was studied. The obtained information facilitated the optimization of the each regioisomer. As a result, 2-, 3-, and 4-ring-substituted analogues of AMP and MA with methyl, methoxy, fluoro, chloro, and bromo groups were separated, generally within 6 min. In addition, we found that the separation pattern of the examined regioisomers was classified into two, which depended on the electron donating/withdrawing effect of the substituent. Our results indicate that SFC could be used in forensic drug analysis for fast, reliable identification of structurally similar drugs of abuse. Copyright © 2016 John Wiley & Sons, Ltd.

Guilty by dissociation: Part B: evaluation of Supercritical Fluid Chromatography (SFC-UV) for the analysis of regioisomeric diphenidine-derived Novel Psychoactive Substances (NPS)

“…1) were prepared as their corresponding hydrochloride salts using the previously reported synthetic approach from prerequisite aromatic aldehydes as stable, colourless to off-white powders [7,10]. To ensure the authenticity of the materials utilized within this study, the 31 synthesized samples were structurally characterized by 1 H-NMR, 13 C{ 1 H}-NMR, GC-MS and ATR-FTIR and the purity of all samples was confirmed to be >99.5% (by NMR) in all cases. Selectivity in SFC can be controlled by changing the mobile phase composition, temperature and pressure [23][24][25], however, the stationary phase was reported to be the most influential parameter in affecting chromatographic selectivity [26][27][28].…”

“…The synthesis of the racemic target compounds was achieved using the previously reported method [7,10] and isolated as their corresponding hydrochloride salts. To ensure the authenticity of the materials utilized within this study, the 31 synthesized samples were structurally characterized by 1 H-NMR, 13 C{ 1 H}-NMR, GC-MS and ATR-FTIR and the purity of all samples was confirmed to be >99.5% (by NMR) in all cases. The analytical data for compounds 1 -31 has been previously reported [7,10].…”

Supercritical fluid chromatography – Mass spectrometry: Recent evolution and current trends

“…A second application area that is being under constant development is the implementation of SFC-MS in the forensic and anti-doping control analysis. Indeed, there has been an important number of papers recently released and focusing on several classes of compounds: amphetamines [45,69,70], stimulants and sympathomimetic drugs [51,71,72] or anabolic agents and steroids [44,54,73,74] (Fig. 4).…”

High-Throughput and Ultrafast Liquid Chromatography

“…A wide number of applications have been explored with ultrafast SFC separations, including pharmaceutical drugs, − dietary supplements, , steroid compounds, − forensic samples and drugs of abuse, − cosmetics, , and biofuels and coal tar, with MS detection becoming increasingly important in methods utilizing SFC. − Beyond these analytical-scale separations, SFC has also been applied for rapid preparative purifications, which is especially advantageous as a “greener” analytical technique with less solvent waste than a typical preparative-scale separation. , On the opposite column size regime, microfluidic SFC was reported for the first time, with both chiral and achiral separations achieved in under 30 s . Combined with a microfluidic board designed for flow control that is compatible with SFC mobile phases, there is significant potential for miniaturized SFC techniques to increase in use in coming years.…”