Abstract
High-speed countercurrent chromatography (HSCCC) was successfully used for the isolation and purification of two closely related glycosidic flavonoids from Exocarpium Citri Grandis. n‐Hexane‐1‐butanol–methanol–0.5% acetic acid (1:3:1:4, v/v) was used as the two‐phase solvent system. From 50 mg of crude extracts of Exocarpium citri Grandis, 28.8 mg of naringin, 1.4 mg of rhoifolin, and 5.7 mg of an unknown compound were obtained with the purity of 97.1%, 95.5%, and 97.5%, respectively, in a single run. Two flavonoids fractions were characterized by ESI‐MS confirming that the data was identical to the literature values.