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In this study，a high performance liquid chromatography(HPLC)coupled with a variable wavelength detector(VWD)has been developed for the simultaneous determination of three anthraquinones(including emodin，physcion，emodine-8-O-β-D-glucoside)and one stilbene((E)-2,3,5,4-tetrahydroxystilbene-2-O-β-D-glucoside)in prepared roots of Polygonum multiflorum Thunb.(P. multiflorum). It is widely used in the prescription of traditional Chinese medicine(TCM)，and also edible as an invigorant. This method was simple，reliable and reproducible，and was successfully applied to determine the four target compounds in the prepared P. multiflorum for the quality control. In addition，it was the first time reported to identify another one naphthalene derivation and three stilbenes by this ESI/MS method.