Abstract: Oil and cyanogenic glycosides were extracted simultaneously from flaxseed by two-liquid-phase system of ethanol-hexane-water. The technology was optimized by single-factor experiment, orthogonal experiment and response surface methodology(RSM). Results show that the optimum extracting conditions are ethanol concentration 85%(w/w), the ratio of material to ethanol 1∶3.4; the ratio of material to hexane 1∶5.4; extraction time 78.5 min, extraction temperature 55℃, NaOH concentration 0.12%. The hydrous ethanol/hexane system has good effect on simultaneous extracting oil and cyanogenic glycosides from flaxseed, and the extraction rates of oil and cyanogenic glycosides are 45.1% and 96.8% respectively under optimum extracting conditions.