A novel and efficient extraction/hydrolysis method was developed for the recovery of resveratrol and emodin from a well-known traditional chinese medicinal herb, Polygonum cuspidatum. By using a 85% aqueous acetone solution containing 1.0 mol/L HCl as extractant, extraction of resveratrol and emodin from P. cuspidatum and conversion of resveratrol-3-O-β-glucoside and emodin-8-O-β-D-glucoside into the products could be achieved in one step. The effects of several key parameters including concentration of HCl and acetone, temperature, ratio of solvent to material, extraction duration and extraction times on the process efficiency was systematically investigated. The results showed that the optimal conditions for maximizing the recovery yield were 85% acetone containing 1.0 mol/L HCl as extractant, temperature 70 ℃, ratio of liquid to solid 50 mL /g and extraction duration 30 min. This one-pot extraction/hydrolysis process increased the yield of resveratrol and emodin to 524% and 302%, respectively, compared to a raw sample without hydrolysis. Compared with conventional method, the developed process not only achieved high yield of resveratrol and emodin, but simplified the procedures and reduced time. The results demonstrated that the simultaneous extraction/hydrolysis process is simple and efficient which could act as a useful approach for enhanced recovery of resveratrol and emodin from P. cuspidatum. A novel and efficient extraction / hydrolysis method was developed for the recovery of resveratrol and emodin from a well-known traditional Chinese medicinal herb, Polygonum cuspidatum. By using a 85% aqueous acetone solution containing 1.0 mol / L HCl as extractant, extraction of resveratrol and emodin from P. cuspidatum and conversion of resveratrol-3-O-β-glucoside and emodin-8-O-β-D-glucoside into the products could be achieved in one step. The effects of several key parameters including concentration of HCl and acetone, temperature, ratio of solvent to material, extraction duration and extraction times on the process conditions was systematically investigated. The results showed that the optimal conditions for maximizing the recovery yield were 85% acetone containing 1.0 mol / L HCl as extractant, temperature 70 ° C, ratio of liquid to solid 50 mL / g and extraction duration 30 min. This one-pot extraction / hydrolysis process increased the yield of resveratrol and emodin to 524% and 302% Compared with a raw sample without hydrolysis. Compared with conventional method, the developed process not only achieved high yield of resveratrol and emodin, but simplified the procedures and reduced time. The results of that the simultaneous extraction / hydrolysis process is simple and efficient which could act as a useful approach for enhanced recovery of resveratrol and emodin from P. cuspidatum.