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采用二元液相分离系统,通过对比柱色谱硅胶、聚合物微球和反相硅胶3种不同类型色谱介质的分离效果和洗脱参数,开发普那霉素ⅡA的制备工艺。结果显示,选用反相硅胶C18为色谱介质,洗脱剂为乙腈∶0.05%磷酸二氢钾溶液(45∶55),上样量0.8 g/100 ml,纯化所得产品纯度≥98.5%,纯化收率≥75%。
The separation and elution parameters of three different types of chromatographic media, including column chromatography silica gel, polymer microsphere and reverse phase silica gel, were compared with binary liquid phase separation system to develop the preparation technology of pristinamycin ⅡA. The results showed that the reversed-phase silica gel C18 was used as the chromatographic medium. The eluent was acetonitrile: 0.05% potassium dihydrogen phosphate solution (45:55), the amount of sample was 0.8 g / 100 ml. The purity of purified product was ≥98.5% Rate ≥ 75%.