Study on circulating column chromatographic extraction of hesperidin and polysaccharide from navel orange peel
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摘要: 目的:研究联合提取并分离脐橙皮的橙皮苷和多糖的最佳工艺条件。方法:通过柱层析循环法确定最佳的洗脱液分别是40%乙醇和水,吸涨时间均为1h,吸涨体积分别为5倍和7倍(mL/g)。结果:脐橙皮中橙皮苷的含量为4.85%,多糖的含量为1.93%,循环提取第1轮第1份的橙皮苷和多糖的提取率分别是92.7%和90.2%,从第2轮开始,第1份的提取率均达到99%以上。各轮两洗脱液的第1份合并,80%醇沉淀多糖,分别得橙皮苷和多糖粗产品,含量分别为60.27%和15.42%;橙皮苷的粗产品经过结晶和重结晶,橙皮苷的纯度为97.84%,总得率为85.55%,多糖粗产品经水溶,醇沉两次,产品纯度85.32%,总得率89.53%。结论:利用柱层析循环法可同时提取橙皮苷和多糖,并通过乙醇沉淀可把两种成分一次性分离开来,工艺简单,时间短,乙醇用量少,提取效率高,具有广阔前景。Abstract: Obiective:To explore technical process and conditions for the circulating extraction of hesperidin and polysaccharides by using column chromatography from navel orange peel. Methods:The optimal eluent was40% (v/v) ethanol and water. The time for the material to be fully absorbed in the two solvents were both for 1h, the volume of solvent for the plant material to be fully absorbed were 5-fold and 7-fold (mL/g) . Results:A fully absorbed volume was a collection unit, as a fraction. Two fractions were collected in each eluate, retained the first, the second for eluent of next circulation. Results showed that the content of hesperidin and polysaccharide were 4.85% and 1.93% in navel orange peel, respectively. The extraction rate of hesperidin and polysaccharides of the first fractions was 92.7% and 90.2% in the first circulation, respectively. The rest of the extraction rate was more than 99%. Merged all the first fraction eluate in circulation. 80% ethanol precipitated the polysaccharide.The crude product hesperidin and polysaccharide were separated, purity was 60.27% and 15.42%, respectively.The purity of hesperidin was 97.84%, recovery rate was 85.55% after crystallization and recrystallization. The purity of polysaccharide was 85.32%, recovery rate was 89.53% after dissolved in water and precipitation in ethanol for twice. Conclusion:By using the circulating column chromatography and ethanol precipitation, hesperidin and polysaccharide from navel orange peel could be extracted and purified at the same time. The process was simple and short, with less consumption of ethanol and high extraction rates.
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Keywords:
- navel orange peel /
- column chromatography /
- circulating extraction /
- hesperidin /
- polysaccharide
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