Abstract: GC-MS was applied to the simultaneous determination of 10 polychlorinated phenol residues in Cork stoppers. Samples were extracted with methanol. After the extract was acetylated with acetic anhydride in a potassium carbonate solution, the mixture was extracted with n-hexane and separated on a DB-5MS capillary chromatographic column. EI⁺ and SRM were adopted in MS analysis. The linearity range of 10 polychlorinated phenols was 1.0-100.0 mg·L^-1, with detection limits (3S/N) in the range of 0.03-0.21 mg·kg^-1. Recovery rates obtained by standard addition method were in the range of 88.4%-104%, and RSDs (n=6) were in the range of 2.1%-4.6%. The method was used to determine 10 polychlorinated phenols in commercially available Cork stopper, giving the detection rate of 77.8%.