Elbashir Abdalla A, Saad Bahruddin, Ali Abdussalam Salhin Mohamed, Saleh Muhammad Idiris, Aboul-Enein Hassan Y
School of Chemical Sciences, Universiti Sains Malaysia, Penang, Malaysia.
Biomed Chromatogr. 2009 May;23(5):464-71. doi: 10.1002/bmc.1137.
A capillary zone electrophoretic method has been developed and validated for the determination of the impurity quinocide (QC) in the antimalarial drug primaquine (PQ). Different buffer additives such as native cyclodextrins and crown ethers were evaluated. Promising results were obtained when either beta-cyclodextrin (beta-CD) or 18-crown-6 ether (18C6) were used. Their separation conditions such as type of buffer and its pH, buffer additive concentration, applied voltage capillary temperature and injection time were optimized. The use of 18C6 offers slight advantages over beta-CD such as faster elution times and improved resolution. Nevertheless, migration times of less than 5 min and resolution factors (R(s)) in the range of 2-4 were obtained when both additives were used. The method was validated with respect to selectivity, linearity, limits of detection and quantitation, analytical precision (intra- and inter-day variability) and repeatability. Concentrations of 2.12 and 2.71% (w/w) of QC were found in pharmaceutical preparations of PQ from two different manufacturers. A possible mechanism for the successful separation of the isomers is also discussed.
已开发并验证了一种毛细管区带电泳方法，用于测定抗疟药物伯氨喹（PQ）中的杂质喹诺酮（QC）。对不同的缓冲添加剂，如天然环糊精和冠醚进行了评估。当使用β-环糊精（β-CD）或18-冠-6醚（18C6）时，获得了有前景的结果。优化了它们的分离条件，如缓冲液类型及其pH值、缓冲添加剂浓度、施加电压、毛细管温度和进样时间。使用18C6比β-CD有一些轻微优势，如洗脱时间更快和分离度提高。然而，当使用这两种添加剂时，迁移时间均小于5分钟，分离度因子（R(s)）在2-4范围内。该方法在选择性、线性、检测限和定量限、分析精密度（日内和日间变异性）及重复性方面进行了验证。在来自两个不同制造商的PQ药物制剂中，发现QC的浓度分别为2.12%和2.71%（w/w）。还讨论了异构体成功分离的可能机制。
