Abstract: GC-MS was applied to the determination of polychlorinated biphenyls in polymer materials used in electrical and electronic products. The sample was extracted ultrasonically with a mixture of acetone and n-hexane (1+1). The extract was purified with a solid phase extraction column filled with neutral sllica gel and then separated on a DB-5MS UI capillary column. EI and SIM were adopted in MS. The linearity ranges of polychlorinated biphenyls (Cl1-Cl10) were all 0.1-10 mg·L-1,with the same lower limits of determination (10S/N) of 0.1 mg·kg-1. Recovery rates obtained by standard addition method were in the range of 86.0%-109%,and RSDs (n=7) were within 10%.