Abstract: A method for the analysis of bromophenols in fishery product was developed. The sample was acidified to make sure that all of the bromophenol compounds were converted to molecular status. The molecular bromophenol was extracted by n-hexane-ethylether, purified by GPC, acetylize by acetic anhydride, and then extracted by n-hexane and determined by GC/MS. The result indicated that all of the bromophenol compounds were finely separated on the DB-17ms column with good chromatographic peak, and the derivatization with acetic anhydride was enhanced the signal sensitivity by almost a hundred times. The detection limit is 0.3—0.5 μg/kg, with recoveries of 70.2%—102% and relative standard deviations of 5.3%—10.3%. The proposed method is applied to the analysis of bromophenol in fishery product, and it is found that the bromophenol contents are between 0.3 μg/kg and 5.0 μg/kg, among which 2,4,6-TBP has the highest level.