title: Effect of the nature of the single-isomer anionic CD and the BGE composition on the enantiomeric separation of beta-blockers in NACE.
abstract: The separation of ten beta-blockers has been investigated in NACE systems using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-CD (HDMS-beta-CD) and heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-CD (HDAS-beta-CD). The influence on enantioresolution, mobility difference and selectivity of the nature of both anionic CD and BGE anion as well as their concentrations were studied by means of a multivariate approach. A D-optimal design with 25 experimental points was applied. For all studied analytes, the enantiomeric resolution was shown to be significantly influenced by both CD nature and concentration. Except for two compounds, HDAS-beta-CD was found to give higher enantioresolution values than HDMS-beta-CD. The best enantioseparation for all compounds was achieved in the presence of a high chiral selector concentration and for most of them at a low BGE anion concentration. For each investigated compound, operating conditions leading to the best enantiomeric resolution were deduced. A generic NACE system was then recommended, namely 10 mM ammonium acetate and 40 mM HDAS-beta-CD in methanol acidified with 0.75 M formic acid. This generic system was able to completely resolve the enantiomers of all beta-blockers, with a R(s) value of at least 4. Finally, the optimal conditions obtained modelling resolution, mobility difference and selectivity were compared.
authors: Department of Analytical Pharmaceutical Chemistry, Institute of Pharmacy, University of Liège, Liège, Belgium.
authors: Anne
authors: A
authors: Rousseau
authors: Patrice
authors: P
authors: Chiap
authors: Radu
authors: R
authors: Oprean
authors: Jacques
authors: J
authors: Crommen
authors: Marianne
authors: M
authors: Fillet
authors: Anne-Catherine
authors: AC
authors: Servais
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000302:isolation & purification*; D004573:Electrolytes / Q000737:chemistry; D019075:Electrophoresis, Capillary / Q000379:methods*; D008956:Models, Chemical; D015203:Reproducibility of Results; D013015:Sotalol / Q000302:isolation & purification; D013999:Timolol / Q000302:isolation & purification; D047392:beta-Cyclodextrins / Q000737:chemistry*
chemical_list: D000319:Adrenergic beta-Antagonists; D004573:Electrolytes; D047392:beta-Cyclodextrins; C400661:heptakis(2,3-dimethyl-6-sulfato)cyclodextrin; D013999:Timolol; D013015:Sotalol