We report a hyphenated procedure for the extraction of oleanolic acid (OA) and ursolic acid (UA) from Hedyotis diffusa. The hyphenated ultrasound-assisted extraction (HUAE) procedure consists of heat-reflux extraction (HRE) followed by ultrasound-assisted extraction (UAE). This hyphenated technique uses a lower temperature, consumes less solvent and is faster than previous methods. Compared to heat-reflux and traditional ultrasound-assisted extractions, HUAE gave a 12% higher yield of OA and UA from H. diffuse and required less severe operating conditions. Thus, mild operating conditions can be used, which results in a higher quality product. HUAE is an effective and selective method for the extraction of OA and UA. Additionally, the HUAE of OA and UA from H. diffuse were interpreted using a second-order kinetic model to predict the extraction parameters at various temperatures. Furthermore, the activation energies for the extractions of OA and UA were 9.073 and 10.575 kJ/mol, respectively, based on the second-order extraction rate constants used to build the models. By fitting the main parameters of the model, we could compare the effects of the extraction parameters on the H. diffuse material and better understand the extraction process. (C) 2014 Elsevier B.V. All rights reserved.