Scientific article
English

Experimental design for enantioselective separation of celiprolol by capillary electrophoresis using sulfated beta-cyclodextrin

Published inElectrophoresis, vol. 20, no. 17, p. 3424-3431
Publication date1999
Abstract

A capillary zone electrophoresis method was developed for the enantioseparation of celiprolol enantiomers, using a sulfated beta-cyclodextrin (beta-CD) as a chiral selector. The use of a coated capillary was necessary to achieve stable and reproducible enantioseparations. A central composite design was applied to optimize the method and four parameters were selected for this study: the buffer pH, the buffer concentration, the sulfated beta-CD concentration and the temperature. Resolution between celiprolol enantiomers as well as analysis time and generated current were established as responses. For each response, a model was obtained by a second-degree mathematical expression. From the models, the most favorable conditions were determined by optimizing the resolution between celiprolol enantiomers and by setting the two other responses at threshold values. Response surfaces were also used to assess the robustness of the analytical method around the optimal region. Successful results were obtained with a 52 mM acetate buffer at pH 4.0 in the presence of 3.0 mM sulfated beta-CD at a temperature of 19.5 degrees C. Under these optimized conditions, baseline separation of the celiprolol enantiomers was achieved in less than 10 min. The method showed good validation data in terms of precision, accuracy and linearity, and was found to be suitable in determining celiprolol enantiomers in pharmaceutical preparations and in biological fluids.

Keywords
  • Adrenergic beta-Antagonists/isolation & purification/urine
  • Celiprolol/isolation & purification/urine
  • Cyclodextrins/chemistry
  • Electrophoresis, Capillary/methods
  • Humans
  • Reproducibility of Results
  • Stereoisomerism
  • Sulfates/chemistry
  • Tablets/chemistry
  • Beta-Cyclodextrins
Citation (ISO format)
DAALI, Youssef et al. Experimental design for enantioselective separation of celiprolol by capillary electrophoresis using sulfated beta-cyclodextrin. In: Electrophoresis, 1999, vol. 20, n° 17, p. 3424–3431. doi: 10.1002/(SICI)1522-2683(19991101)20:17<3424::AID-ELPS3424>3.0.CO;2-Z
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Journal ISSN0173-0835
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