Lucangioli S E, Rodríguez V G, Fernández Otero G C, Carducci C N
Department of Analytical Chemistry and Physicochemistry, Faculty of Pharmacy and Biochemistry, University of Buenos Aires, Argentina.
J Capillary Electrophor. 1998 May-Aug;5(3-4):139-42.
A cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC) method has been developed and validated for purity determination of two bile acids, ursodeoxycholic acid (UDCA) and deoxycholic acid (DCA). Quantitation of related impurities such as lithocholic acid (LCA), chenodeoxycholic acid (CDCA), cholic acid (CA), and DCA in UDCA and CA in DCA was performed. A running buffer containing 20 mM borate-phosphate, 50 mM sodium dodecyl sulfate (SDS), 2.0 mM beta-cyclodextrin, and acetonitrile was used. Modifiers were added to improve resolution and selectivity. The applied voltage was 25 kV and detection was performed at 185 nm. Validation parameters such as selectivity, linearity, repeatability, intermediate precision, limit of detection, limit of quantitation, and robustness were evaluated. The method was simple and proved to be useful for the purity testing of bile acids in bulk drugs. Good results were obtained for related impurities at concentration levels from 0.05 to 1.5% with respect to the main component, according to international requirements.
已开发并验证了一种环糊精修饰的胶束电动色谱法（CD - MEKC），用于测定两种胆汁酸——熊去氧胆酸（UDCA）和脱氧胆酸（DCA）的纯度。对UDCA中的相关杂质如石胆酸（LCA）、鹅去氧胆酸（CDCA）、胆酸（CA）和DCA以及DCA中的CA进行了定量分析。使用了一种运行缓冲液，其包含20 mM硼酸盐 - 磷酸盐、50 mM十二烷基硫酸钠（SDS）、2.0 mMβ - 环糊精和乙腈。添加了改性剂以提高分离度和选择性。施加电压为25 kV，检测波长为185 nm。评估了选择性、线性、重复性、中间精密度、检测限、定量限和稳健性等验证参数。该方法简单，被证明可用于原料药中胆汁酸的纯度检测。根据国际要求，对于相对于主成分浓度在0.05%至1.5%水平的相关杂质，获得了良好的结果。
