Abstract: The volatile components of Liangzhou fumigated vinegar before and after fumigating were inspected by headspace solid phase micro-extraction (SPME) and gas chromatography-mass spectrum (GC-MS) technique.The results showed that 58 and 57 kinds of compounds existed in two samples respectively, the major compounds were alcohols, acids, esters, aldehydes, ketones, herterocylics and alkanes in both materials.The major volatile compounds of liangzhou fumigated materials before fumigating were ammonium acetate (18.223%) , ethyl acetate (15.853%) , acetic acid (15.236%) and 3-hydroxybu-2-tanone (19.532%) .The compounds after fumigating were ammonium acetate (49.959%) , ethyl, acetate (5.352%) , 3-hydroxybu-2-tanone (9.530%) , furfural (12.007%) .Preliminary proved the changes of flavor substancesin roasted materials of liangzhou fumigated vinegar before and after fumigating.