Abstract: Headspace solid phase micro-extraction coupled with gas chromatography-mass spectrometry(HS-SPME-GC-MS)were utilized in this study for the analysis of volatile flavors in marinated beef. In order to establish the most suitable method,the optimization of the extraction conditions was carried out by selecting fibers and performing single-factor experiment combined with response surface methodology. As a result,65 μm PDMS/DVB fiber was used and the extraction was conducted as follows:2.0 g sample was treated under 70 ℃ for 45 min and then desorbed under 240 ℃. Results showed that,there were 44 volatile flavor compounds identified in the target samples,including aldehydes,alcohols,ketons,ethers,esters,acids,hydrocarbons,and nitrogen and sulfur heterocyclics. Of those,aldehydes and nitrogen and sulfur heterocyclics showed higher contents,being 51.29%±2.80% and 16.78%±1.10%,respectively,which were determined as the dominant volatile flavor compounds in the marinated beef.