Leaves of Xushu-18 was used as raw material to have established a method for isolation and preparation of chemical compositions from sweet potato stalk by high speed counter-current chromatography-high performance liquid chromatography (HSCCC-HPLC). N-hexane-ethyl acetate-methanol-water(0.5% acetic acid) (0.5∶5∶1∶5, V/V) was used as the two-phase solvent system. The upper one was used as the stationary phase, while the lower phase was used as the mobile one. Separation was performed twice at a flow-rate of 2 mL/min and a revolution speed of 900 r/min. Seven compounds were got and HSCCC was separated in the same solvent system and preparation high performance liquid chromatography. The structures were identified primarily by colour reaction, UV spectrometry and HPLC. The results showed one of them was rutin and the other was quercitrin.