Abstract: For the study of characteristic volatiles of mullet, the flavor compounds variation of mullet during cold storage at 0 ℃under vacuum-packed were detected using HS-SPME-GC-MS.As a result of totally 76 volatiles which could be divided into 7classes were identified during storage of mullet. The generation sources sensory characteristics and relative contents of flavor compounds were further discussed in details.Among these compounds, most of them were hydrocarbons aromatics alcohols and aldehydes.The eight flavor compounds can be detected which are dodecane, cetane, octacosane, toluene, naphthalene, 2, 4-2tertiary butyl phenol, dibutyl hydroxy toluene and sulfurous acid during cold storage, respectively. Four principal component factors were extracted using PCA method during cold storage characteristic mullet volatiles and laid a foundation to further study mullet volatile flavour compounds.