Musenga Alessandro, Mandrioli Roberto, Morganti Emanuele, Fanali Salvatore, Raggi Maria Augusta
Department of Pharmaceutical Sciences, University of Bologna, Via Belmeloro 6, 40126 Bologna, Italy.
J Pharm Biomed Anal. 2008 Apr 14;46(5):966-70. doi: 10.1016/j.jpba.2007.05.022. Epub 2007 May 25.
A capillary electrophoretic method has been developed for the enantioselective analysis of amisulpride in pharmaceutical formulations, using beta-cyclodextrin sulfate as the chiral selector. Several parameters, such as cyclodextrin type and concentration, buffer concentration and pH and capillary temperature were investigated for method optimisation. Baseline enantioseparation of the racemic compound was achieved in less than 10 min using a fused silica capillary (50 microm i.d. and 33.0, 8.5 cm, total and effective length, respectively), filled with a background electrolyte consisting of a 10mM citrate buffer at pH 3.5 supplemented with 0.22% (w/v) beta-cyclodextrin sulfate at 20 degrees C and applying a voltage of +15 kV. Formulation analysis was carried out after analyte extraction by methanol. The method was fully validated, with good results in terms of precision, selectivity, accuracy and amount of drug found with respect to the label claim. Thus, the method seems to be suitable for the enantiomeric analysis of amisulpride in pharmaceutical formulations.
已开发出一种毛细管电泳方法，以硫酸β-环糊精作为手性选择剂，用于对药物制剂中的阿立哌唑进行对映体选择性分析。研究了几个参数，如环糊精类型和浓度、缓冲液浓度和pH值以及毛细管温度，以优化该方法。使用内径为50微米、总长度和有效长度分别为33.0厘米和8.5厘米的熔融石英毛细管，在20℃下填充由pH值为3.5的10mM柠檬酸盐缓冲液组成的背景电解质，并施加+15 kV的电压，在不到10分钟内实现了外消旋化合物的基线对映体分离。通过甲醇萃取分析物后进行制剂分析。该方法经过全面验证，在精密度、选择性、准确性以及相对于标签声明所发现的药物量方面均取得了良好结果。因此，该方法似乎适用于药物制剂中阿立哌唑的对映体分析。
