Volatile compounds in whey sample in different stages during traditional brewing processing were analyzed by headspace solid phase micro-extraction (HS—SPME) and gas chromatography-mass spectrum (GC—MS) technique. The results indicated that 59 kinds of volatile components were identified，including alcohols, olefins, aldehydes and ketones, esters, acids. Totally 24, 29, 34, 34 and 36 kinds of volatile components were identified in whey samples fermented for 0, 24th, 48th, 72th, and 96th hours, respectively. Among them, twelve volatile compounds were common to the five samples. With the fermentation, the amounts of volatile components were increased, and esters were newly detected. The relative contents of alcohols and olefins were decreased, whereas the relative contents of esters and acids were increased at the fermentation early stage. However, the relative contents of all kinds of volatile components changed slightly at the post-fermentation stage. In addition, the relative contents of aldehydes and ketones had no obviously changed. Among these volatile compounds, dipentene, ethyl acetate, hexanal, pinene, phenethyl alcohol, hexyl alcohol, acetic acid, propyl acetate had an important contribution to the flavor of whey during the fermentation processing.