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置换色谱法分离表阿霉素和阿霉素异构体的研究
Study on Separation of Epirubicin and Doxorubicin Isomers by Displacement Chromatography
【摘要】 采用置换色谱法在KromasilKR10 0 10C18色谱柱 (2 5 0mm× 4 6mmi d ,10 μm)上成功地分离了二元异构体表阿霉素和阿霉素的混合物 ,并研究和探讨了置换剂类型、浓度、流动相的组成及流速对分离的影响。结果表明 :选用 30g/L的海胺 16 2 2为置换剂 ,流速 0 2mL/min ,以及在有机相比例较低的流动相中加样 ,而将置换剂溶解在有机相比例稍高的流动相中进行置换展开 ,可以达到较好的分离。在最佳分离条件下 ,采用置换展开方式可以在分析色谱柱上一次分离 30mg异构体的混合物。该结果充分显示了置换色谱上样量大 ,可充分利用高效的色谱填料、产率高、分辨率好以及溶剂消耗少等优点 ,适用于药物和生物制剂的制备分离。
【Abstract】 Displacement chromatography was successfully used to separate, at the preparative scale, a binary isomer mixture of epirubicin and doxorubicin, which are anthracycline antitumor antibiotics, on an analytical column (Kromasil KR100-10C18 column, 250 mm×4.6 mm i.d., 10 μm). Displacement parameters such as the type and the concentration of displacer, the composition and the flow-rate of mobile phase were investigated. The displacer employed was 30 (g/L) benzethonium chloride. The flow-rate was 0.2 (mL/min). Loading of feed at lower initial organic level of mobile phase coupled with displacement at higher organic level was found to give efficient separation. The binary isomer mixture of 30 mg was separated on the analytical column. The results have indicated that displacement mode had high efficiency, greatly reduced solvent consumption in the process of purification, and offered the possibility of both high resolution and high loading. It has also demonstrated again that high performance displacement chromatography is one of the effective methods for the purification of therapeutic compounds in industrial processes.
【Key words】 displacement chromatography; epirubicin; doxorubicin; isomers; preparative (separation);
- 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2004年02期
- 【分类号】O657.7
- 【被引频次】2
- 【下载频次】176