The present study describes the separation of syringaresinol from the legume of Mucuna sempcrvircns by high-speed countercurrent chromatography(HSCCC) with a solvent system of methyl tert-butyl ether-methanol-water(2∶ 1∶ 1,v/v/v).Crude syringaresinol of 1.28 g with a purity of 89.5% was obtained from a separation of 5 g crude extracts.The crude syringaresinol was re-crystallized to more than 98% purity of syringaresinol.The chemical structure of the substance was identified by ESI-MS,1H NMR and 13C NMR.The syringaresinol content in the legume samples collected in different districts in Hangzhou were all more than 3.0 g/kg.This shows that the legume is an excellent resource for preparation of natural syringaresino which can be used for research and development of health food and medicine.