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.