Preparative separation of quinolone alkaloids in Evodia rutaecarpa (Juss.) Benth was conducted by high performance counter-current chromatography (HPCCC) with a pair of two solvent systems consisting of n-hexane-methanol-water-acetic acid (2:1:1:0.2, v/v) and (5:4:2:0.1, v/v). Consequently, 31.78mg 1-methyl-2-nonyl-4 (1H)-quinolone (I), 59.25mg 1-methyl-2-(6-undecenyl)-4 (1H)-quinolone (II), 333.27mg evocarpine (III), 101.13mg 1-methyl-2-(6,9-pentadecadienyl)-4(1H)-quinolone (IV), 132.17mg dihydroevocarpine (V), and 86.99mg 1-methyl-2-(10-pentadecenyl)-4(1H)-quinolone (VI) were obtained from 1.3g of the crude extract. The structures of these compounds were identified by mass spectrometer (MS), nuclear magnetic resonance (1H NMR and 13C NMR).