In order to improve the extraction efficiency and quality of Cyperus esculentus oil,three kind of oil extraction techniques such as solvent method,aqueous-enzyme method and aqueous-enzyme and freeze-thaw coupling technique were compared using gas chromatography/mass spectrometry(GC-MS) with oil-extraction rate and physical-chemical properties as index.A new preparation technology of Cyperus esculentus oil was developed using aqueous-enzyme and freeze-thaw coupling technique.The technological parameters of aqueous-enzyme and freeze-thaw coupling technique were optimized through single factor experiment and orthogonal test.The results showed that the most appropriate conditions in the process of enzymolysis were as follows: alkali protease and cellulose enzyme composite enzyme were adopted,ratio of material to solvent was 1∶ 7,enzyme amount was 2.5% of dried Cyperus esculentus powder weight,temperature was 70℃ and enzymolysis time was 4h,then it was frozen at-30℃,molten at room temperature,centrifugalized at 4 000r/min for 20min.Under these conditions,the oil extraction rate was up to 74.92%,which was higher than aqueous-enzyme method.The quality of oil obtained by aqueous-enzyme and freeze-thaw coupling technique was the best.The aqueous-enzyme and freeze-thaw coupling technique was regarded as the ideal extraction process of Cyperus esculentus oil.This paper can offer some reference for industrial production of Cyperus esculentus oil.