Klockow-Beck A, Nick A, Geisshuesler S, Schaufelberger D
The R.W. Johnson Pharmaceutical Research Institute, a Division of Cilag AG, Analytical Development, Schaffhausen, Switzerland.
J Chromatogr B Biomed Sci Appl. 1998 Dec 11;720(1-2):141-51. doi: 10.1016/s0378-4347(98)00365-x.
A capillary electrophoresis (CE) method has been developed as an alternative method for the determination of the inorganic degradation products sulfate and sulfamate in topiramate drug product and drug substance, currently performed by ion chromatography. The anions are separated in a background electrolyte containing potassium chromate and boric acid, followed by indirect UV detection. By adding tetradecyltrimethylammonium bromide to the electrolyte, analysis is performed under co-electroosmotic flow conditions. Variations in injection volumes and migration times are compensated for by use of an internal standard. The validation of the method, which was performed according to ICH guidelines (International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use) [1], comprises specificity, accuracy, linearity, precision, sensitivity and robustness. In addition, the results of an actual tablet sample analysis obtained by this CE method are statistically shown to be in close agreement with those obtained by an ion chromatographic method.
已开发出一种毛细管电泳（CE）方法，作为目前通过离子色谱法测定托吡酯制剂和原料药中无机降解产物硫酸盐和氨基磺酸盐的替代方法。这些阴离子在含有铬酸钾和硼酸的背景电解质中分离，随后进行间接紫外检测。通过向电解质中加入溴化十四烷基三甲基铵，在共电渗流条件下进行分析。进样体积和迁移时间的变化通过使用内标进行补偿。该方法按照国际人用药品注册技术协调会（ICH）指南[1]进行验证，包括特异性、准确性、线性、精密度、灵敏度和稳健性。此外，通过该CE方法获得的实际片剂样品分析结果经统计学显示与通过离子色谱法获得的结果非常一致。
