The mixture compound extracted by supercritical carbon dioxide extraction can attracted the insect directly,which was the new approach to search after the attractant. Volatiles could be used to bioassay. Results of behavior responses of Anoplophora glabripennis to the volatiles extracted from Acer mono under different pressure and temperature showed that extracts of 25 MPa, 35 ℃ was attractive to A. glabripennis significantly than others. Extracts of 25 MPa, 35 ℃ was the optimum supercritical fluid extraction(SFE) condition. The analysis of GC-MS showed that the main compound were 3-hexenol and ethyl acetate.