Microwave-assisted, aqueous two-phase extraction was investigated to obtain effective constituents, including piceid, resveratrol and emodin in Polygonum cuspidatum. An aqueous two-phase system consisting of 25% (w/w) ethanol 21% (w/w) (NH4)(2)SO4 gave equal yields of piceid, and 1.1- and 1.9-times higher yields of resveratrol and emodin, respectively, than that achieved by microwave-assisted extraction and heat reflux extraction. Three-separate operations, extraction, clarification and concentration, are hereby integrated into a single step to get higher yields at lower cost. This is therefore a potentially useful method for the extraction and purification of target products.