Design of experiments for capillary electrophoretic enantioresolution of salbutamol using dermatan sulfate

• Published in: Journal of Chromatography A 2000-04, Vol.875 (1), p.411-422
• Main Authors: Gotti, R., Furlanetto, S., Andrisano, V., Cavrini, V., Pinzauti, S.
• Format: Article
• Language: English
• Subjects: Adrenergic beta-Agonists - analysis; Adrenergic beta-Agonists - urine; Albuterol - analysis; Albuterol - urine; Dermatan sulfate; Dermatan Sulfate - chemistry; Electrophoresis, Capillary - methods; Humans; Hydrogen-Ion Concentration; Reproducibility of Results; Salbutamol; Stereoisomerism
• ISSN: 0021-9673
• DOI: 10.1016/S0021-9673(99)01303-5

Statistical experimental design was used for the optimization and for robustness evaluation of a capillary electrophoretic method developed for the enantioresolution of salbutamol. Dermatan sulfate was used as chiral selector. The goal of the study was to obtain an efficient and fast separation. An eight-run Plackett–Burman matrix was used during the optimization process for the screening of the factors and to adjust the experimental domain under study. Response surface methodology was adopted after the screening phase to obtain information about how the factors percentage of chiral selector, pH and voltage affected the considered responses resolution and analysis time. The Derringer desirability function, which makes it possible to combine results obtained for properties measured on different scales, was used to simultaneously optimize the two responses. Robustness testing was carried out using a Plackett–Burman matrix. The method was found robust as regards the response resolution while voltage and chiral selector were found to be critical factors for the robustness of analysis time response. The proposed CE method permitted the complete enantioseparation of racemic salbutamol and was applied to its chiral resolution in spiked urine samples.