Danel Cécile, Chaminade Pierre, Odou Pascal, Bartélémy Christine, Azarzar Dalila, Bonte Jean-Paul, Vaccher Claude
Laboratoire de Chimie Analytique, Faculté des Sciences Pharmaceutiques et Biologiques, Université de Lille, Lille, France.
Electrophoresis. 2007 Aug;28(15):2683-92. doi: 10.1002/elps.200600837.
An analytical method for the enantioseparation of the 9-hydroxyrisperidone, main metabolite of the antipsychotic risperidone (Risp), was developed by CD-EKC in the dual CDs mode using anionic and neutral CDs at acidic pH 2.5. Preliminary experiments allowed us to select the more suitable couple of CDs composed of sulfated-alpha-CD and hydroxypropylated-beta-CD. The optimization of the main experimental parameters (concentrations of both CDs and concentration of the phosphate buffer) was based on a central composite design through the response surface methodology. Then, the influence of the voltage and the temperature on the enantioseparation was studied using the classical univariate approach. The final method permits to resolve the enantiomers of the 9-hydroxyrisperidone with a resolution of 3.13 and an analysis time of about 13 min. Finally, this method was successfully applied for the simultaneous determination of Risp and the enantiomers of 9-hydroxyrisperidone (9-OHRisp).
采用毛细管电泳手性拆分法，在酸性pH 2.5条件下，以阴离子型环糊精和中性环糊精组成的双环糊精模式，建立了抗精神病药物利培酮（Risp）的主要代谢产物9-羟基利培酮对映体的分析方法。通过初步实验，我们选择了由硫酸化α-环糊精和羟丙基化β-环糊精组成的更合适的环糊精对。主要实验参数（两种环糊精的浓度和磷酸盐缓冲液的浓度）的优化基于响应面法的中心复合设计。然后，采用经典单变量方法研究了电压和温度对映体拆分的影响。最终方法能够以3.13的分辨率和大约13分钟的分析时间拆分9-羟基利培酮对映体。最后，该方法成功应用于同时测定利培酮和9-羟基利培酮（9-OHRisp）对映体。
