In this paper, the dorsal meat of grass carp was used as research object. The volatile compounds of grass carp were extracted and concentrated by headspace solid phase micro-extraction (HS-SPME). Then the volatiles were identified by gas chromatography-mass spectrometry (GC-MS). The results showed that SPME-GC-MS was effective to analysis of the volatiles in grass carp meat. According to GC-MS, 42 volatile compounds were detected in dorsal meat of grass carp. The volatile components are mostly carbonyl compounds and alcohols, and the relative contents are 95.74%. The method of odor activity value was applied to determine predominant volatile components of grass carp. There are 12 predominant components were determined in dorsal meat of grass carp, including: 1-Octen-3-ol, 2,6-Nonadienal, Nonanal, (E,E)-2,4-Decadienal, (E,Z)-2,4-Decadienal, Hexanal, 2-Nonenal, Octanal, 2-Decenal, Heptanal, Heptanol and 2-Octenal etc. The study will enrich the theoretical knowledge of flavor chemistry .