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Updated: Jul 8, 2025

High-throughput and Comprehensive Drug Surveillance Using Multisegment Injection-Capillary Electrophoresis-Mass Spectrometry
Published on: April 23, 2019
Stereoselective separation of psychoactive substances: Multivariate optimization and validation of a capillary
Katerina A Ioannou1, Georgia D Ioannou1, Atalanti Christou1
1Department of Chemistry, University of Cyprus, 1678 Nicosia, Cyprus.
Abstract:
A comprehensive study was performed to determine an optimum enantioseparation method for fluorine-substituted amphetamine and cathinone derivatives (fluor-amphetamine and fluor-cathinone derivatives), using a binary system consisting of carboxymethyl-β-CD (CM-β-CD) and a deep eutectic solvent (DES), namely choline chloride-ethylene glycol (ChCl-EG). Under this framework, the optimization and modeling of the separation conditions in a binary system were performed with the objective of maximizing resolution and minimizing analysis time. This was achieved through the application of response surface methodology. In particular, the effect of chiral selector concentration and percentage of DES on resolution and analysis time were investigated and optimized using a complete experimental design. The optimum enantioseparation conditions were determined to be 13.84 mM CM-β-CD and 0.15% v/v ChCl-EG for fluorine-substituted amphetamine derivatives and 14.36 mM and 0.75% v/v ChCl-EG for fluorine-substituted cathinone derivatives, respectively. This combination resulted in a baseline separation for eight out of the nine analytes studied. Overall, the results demonstrated the synergistic effect of the CM-β-CD/DES dual system and highlighted the significance of DESs as additives in capillary electrophoresis.
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