Persson-Stubberud K, Aström O
Pharmaceutical RD, Astra Läkemedel, Södertälje, Sweden.
J Chromatogr A. 1998 Mar 6;798(1-2):307-14. doi: 10.1016/s0021-9673(97)00955-2.
A capillary electrophoresis method has been developed and optimized for the separation of ibuprofen, codeine phosphate and their main degradation products and impurities. In the course of developing the method, it was found that micellar electrokinetic capillary chromatography was necessary for the separation of the eleven peaks. A fractional factorial design was used for the optimization of the experiments. Six process parameters were varied at two levels: the concentration of sodium dodecyl sulfate (SDS), the pH, the concentration of acetonitrile, the concentration of boric acid, the field strength and the temperature. All these factors had a significant effect on the migration time and resolution. The optimum conditions were found to be a borate buffer of 40 mM H3BO3 at pH 10 with the addition of 40 mM SDS and 9% acetonitrile, a field strength of 515 V/cm and a temperature of 25 degrees C. This resulted in baseline separation of the eleven peaks within 12 min.
已开发并优化了一种毛细管电泳方法，用于分离布洛芬、磷酸可待因及其主要降解产物和杂质。在方法开发过程中，发现采用胶束电动毛细管色谱法才能分离这11个峰。采用分数因子设计对实验进行优化。六个工艺参数在两个水平上变化：十二烷基硫酸钠（SDS）浓度、pH值、乙腈浓度、硼酸浓度、场强和温度。所有这些因素对迁移时间和分离度均有显著影响。最佳条件为pH 10的40 mM H3BO3硼酸盐缓冲液，添加40 mM SDS和9%乙腈，场强515 V/cm，温度25℃。这使得11个峰在12分钟内实现基线分离。
