An efficient separation and purification method by microwave-assisted extraction coupled with countercurrent chromatography and preparative liquid chromatography was developed. The extracts obtained from microwave-assisted extraction were rapid separated with counter-current chromatography, and then the fractions were further purified with preparative liquid chromatography. With this method, six furocoumarins including xanthotoxin, bergapten, columbianetin acetate, osthole, isoimperatorin and columbianadin can be obtained from original Angelica Pubescentis Radix samples within total time of 450 min. Their purities were 98%, 98%, 99%, 99%, 99% and 99% respectively, as determined by HPLC. The structures of these compounds were identified by H-1 NMR and MS spectroscopy. The proposed method was economic, rapid and effective, and it can be used to prepare and purify targets from natural products. (C) 2014 Elsevier B.V. All rights reserved.