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We have applied a high-speed counter current chromatography (CCC) technique to the separation and purification of polyphenols from Vitis quinguangularis Rehd.Polyphenols were separated in a solvent system composed of n-hexane–ethyl acetate–methanol–water.The chemical structures of two complex polyphenols were elaborated by means of electrospray ionization MS and NMR analysis.