Mallampati Swapna, Leonard Stefanie, De Vulder Sabine, Hoogmartens Jos, Van Schepdael Ann
Laboratory for Pharmaceutical Chemistry and Drug Analysis, K.U.Leuven, Leuven, Belgium.
Electrophoresis. 2005 Nov;26(21):4079-88. doi: 10.1002/elps.200500284.
A selective MEKC method was developed for the analysis of didanosine in bulk samples. Successful separation of didanosine from 13 of its potential impurities, derived from the various synthetic preparation procedures, was achieved. As CZE gave poor separation selectivity, MEKC was preferable. The use of EKC allowed achievement of the separation in a significantly shorter time than conventional HPLC. An anionic long-chain surfactant, lithium dodecyl sulfate (LiDS), was used as the pseudostationary phase and sodium tetraborate buffer as the aqueous phase. In order to obtain the optimal conditions and to test the method robustness, a central composite response surface modeling experiment was performed. The optimized electrophoretic conditions include the use of an uncoated fused-silica capillary with a total length of 40 cm and an ID of 50 microm, a BGE containing 40 mM sodium tetraborate and 110 mM LiDS at pH 8.0, an applied voltage of 18.0 kV, and the capillary temperature maintained at 15 degrees C. The method was found to be robust. The parameters for validation such as linearity, precision, and sensitivity are also reported. Three commercial bulk samples were analyzed with this system.
建立了一种用于分析散装样品中去羟肌苷的选择性胶束电动毛细管色谱法。成功地将去羟肌苷与其从各种合成制备过程中衍生出的13种潜在杂质分离。由于毛细管区带电泳的分离选择性较差，胶束电动毛细管色谱法更具优势。使用电动色谱法能够在比传统高效液相色谱法显著更短的时间内实现分离。使用阴离子长链表面活性剂十二烷基硫酸锂（LiDS）作为假固定相，硼酸钠缓冲液作为水相。为了获得最佳条件并测试该方法的稳健性，进行了中心复合响应面建模实验。优化的电泳条件包括使用总长40 cm、内径50微米的未涂层熔融石英毛细管，pH 8.0的含40 mM硼酸钠和110 mM LiDS的背景电解质，施加电压18.0 kV，毛细管温度保持在15℃。该方法被发现具有稳健性。还报告了诸如线性、精密度和灵敏度等验证参数。用该系统分析了三个商业散装样品。
