A very simple and effective method for the extraction and determination of oleanolic acid (OA) and ursolic acid (UA) in Radix Actinidiae chinensis was developed using ultrasound-assisted dispersive liquid–liquid microextraction (UA-DLLME) and high performance liquid chromatography–mass spectrometry (HPLC–MS). Ethanol was used as the solvent to extract OA and UA from Radix Actinidiae chinensis, assisted by ultrasonic waves. When the extraction process was finished, the two target analytes in the extraction solvent were rapidly transferred from the ethanol extract to another extraction solvent (chloroform) with the help of a dispersive solvent (tetrahydrofuran) by using DLLME. A series of extraction parameters were investigated and optimized. Under the most favorable conditions, the limits of detection (LOD, S/N = 3) and enrichment factors were 2.0 ng g−1, 89.4 and 6.0 ng g−1, 84.5 for OA and UA, respectively. The recoveries of the spiked sample solutions at three different concentration levels of 200, 500 and 1000 ng g−1 ranged between 88.2 and 96.6%. The proposed method was the first successfully applied for the extraction and determination of OA and UA in Radix Actinidiae chinensis.
