OBJECTIVE：To establish a method for the simultaneous determination of euphol and euphorbol in Euphorbium resinifera，and to optimize the extraction technology. METHODS ：HPLC method was adopted. The determination was performed on Agilent ZORBAX Eclipse Plus C 8 column with mobile phase consisted of acetonitrile-water （90∶10，V/V）at the flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm，and column temperature was 30 ℃. The sample size was 10 μL. Using the contents of euphol and euphorbol ，yield of the extract as evaluation index ，comprehensive score was conducted. The extraction technology was optimized by L （9 34）orthogonal tests ，with ethanol volume fraction ，extraction time and solvent dosage as factors. RESULTS：The linear ranges of euphol and euphorbol were 0.030 4-1.216 mg/mL（r＝0.999 6）and 0.01-0.4 mg/mL（r＝0.999 9）， respectively. RSDs of precision ，stability（24 h）and producibility tests were all lower than 2％. Average recoveries were 100.46％ （RSD＝1.03％，n＝6）and 99.36％（RSD＝0.91％，n＝6）. The optimized technology was extracting with 40 mL 95％ ethanol for 1 h. After 3 times of validation tests showed that average content of euphol was 94.43 mg/g（RSD＝0.92％，n＝3），and that of euphorbol was 25.42 mg/g（RSD＝0.98％，n＝3）；average yield of the extract was 51.42％（RSD＝1.95％，n＝3），and average comprehensive score was 98.87（RSD＝0.92％，n＝3）. CONCLUSIONS ：Established method is simple ，accurate and reproducible ， which can be used for the quality control of E. resinifera . The optimized extraction technology is simple and stable.