An economical and systematized chromatographic separation process to isolate and purify flavonoids from Pericarpium Citri Reticulatae was developed. Solvent refluxing extraction, macroporous resin column, preparative HPLC and HSCCC (high-speed counter-current chromatography) were used for extraction, fraction, isolation, and purification of nine flavonoids including vicenin-2(42 mg), hesperidin (108 mg), isosinensetin (15 mg), sinensetin (10 mg), tetramethyl-O-isoscutellarein (11 mg), nobiletin (121 mg), 3, 5, 6, 7, 8, 3 ',4 '-heptamethoxyflavone (34 mg), tangeretin (114 mg), and 5-demethylnobiletin (13 mg) from Pericarpium Citri Reticulatae, and their purities were all above 98%. All these constituents were identified by UV, MS, H-1 NMR, and C-13 NMR. The procedure and techniques described here can provide a useful reference for the preparative-scale isolation of some flavonoids in a fast, cost-effective, and environmentally-friendly method.