Nitrogenous compounds in hydrolysate of skipjack processing by-product(SPB) was increased 6.4 times in amount comparing that of raw SPB. The major compounds in hydrolysate were anserine, histidine, leucine, hydroxyproline, arginine, phenylalanine and taurine, and composed 56.25% of total nitrogenous compounds. In fatty acid composition, the highest amount was saturated fatty acids in both samples. Polyunsaturated fatty acids such as $C_{20:5}$ and $C_{22:6}$ were increased after hydrolysis. A total of 99 volatile compounds was detected in raw and hydrolysate of SPB by vacuum simultaneous steam distillation-solvent extraction/gas chromatography/mass chromatorgraphy. Of these, 75 compounds were identified in raw SPB, while 72 compounds were identified in hydorlysate of SPB. There compounds were composed mainly of 28 aldehydes, 20 ketones, 19 alcohols, 5 nitrogen containing compounds, 5 aromatic hydrocarbons, 4 furans and 12 miscellaneous compounds. Levels of aldehydes and aromatic hydrocarbons decreased after hydrolysis, whereas heterocyclic compounds such as pyrazies, furans increased.