Abstract: 【Objective】 To screen plant volatiles with biological activity against Monolepta hieroglyphica (Motschulsky) adults.【Method】The volatile compounds of cotton and maize were identified and quantitatively analyzed by gas chromatography and mass spectrometry (GC-MS). The electroantennogram (EAG) technique was used to determine the electrophysiological responses of the female and male Monolepta hieroglyphica to 10 volatiles.【Result】The response of M. hieroglyphica male to Tricyclo, Dragosantol, α-Pinene, Myrcene, 3-Carene, 1,3-Butadiene, Palmitic acid were relatively obvious. The response of M. hieroglyphica female to 10 kinds of volatile with part concentration was relatively obvious.【Conclusion】The response of M. hieroglyphica males to 3-Carene is the most sensitive, the response of M. hieroglyphica females to Dragosantol is the most sensitive.