Enzymatic hydrolysis of dark muscle of skipjack was optimized by using response surface methodology. Three factors of independent values were pH (4.2 to 9.8), time (0.6 to 3.4 hrs) and temperature (34℃ to 76℃), and independent values were optical density and brix. The optimum conditions for enzymatic hydrolysis were pH 7.0 to 8.0, 55℃ and 3 hrs. The headspace volatile compounds of reaction flavors using the enzymatic hydrolysate, cysteine and xylose were identified by using the combination of a canister system, gas chromatography and mass selective detector. Among 67 compounds, we identified 8 sulfur-containing compounds and 7 furans which were thought to be highly related to meat-like flavors.