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作 者:龚考才[1] 陈碧群[1] 杜曦[1] 刘可[1] 杜军[1]
出 处:《泸州医学院学报》2006年第6期503-506,共4页Journal of Luzhou Medical College
摘 要:目的:为合成新的高效、低毒靛玉红腭衍生物需对对原料靛玉红进行前处理,分离除去干扰性异构体杂质,建立合成靛玉红腭衍生物及其晶体培养的后继工作中有指导意义的常规色谱离析方法。方法:进行色谱筛选研究,用分离度Ks,选择因子a确定色谱离析系统。结果:S、t、Ks,、a、k显示乙酸乙酯/氯仿、乙酸乙酯/石油醚二元组分展开剂,G-CMC-Na、硅胶H-CMC-Na的色谱离析可用于对原料的处理,以硅胶H-CMC-Na/乙酸乙酯/氯仿的色谱离析经重结晶可得到靛玉红暗红色细小针状晶体。结论:根据实验确定的Ks,a的色谱离析系统,可以实现合成反应中对原料靛玉红的前处理。Objective:In order to synthesize efficient and low toxic indirubin palate, indirubin, as a raw material, its pretreatment, especially the separation of isomer, would be essential to establish chromatography of indirubin palate derivatives and to develop crystal.Methods:Research on chromatography conditions was carried out, resolution and relative retention were used for determining the chromatography system. Results: All the following parameters, such as distance, retention time, resolution, relative retention and capacity factor showed that the separation conditions which ethyl acetate/choloform or ethyl acetate petroleum either as tile developing solvent,GCMC-Na or silica gel H-CMC-Na as the stationary phase, were suited to the pretreatment of the raw material, especially after pretreatment with silica gel H-CMC-Na/ethyl acetate/choloform, and the dark red indirubin crystal could be obtained.Conclusion: The results indicated that the separation conditions decided by the experiment could be applied to the pretreatment of indirubin in the synthetic-reaction.
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