Abstract: An ameliorated pretreatment method for determination of polychlorinated biphenyls(PCBs)in blubber of whale has been established. The samples were extracted with ethyl acetate-cyclohexane by ultrasonically assisted procedure. The extract was purified and condensed with GPC and PCBs were determined by GC-MS.The results showed that the recoveries of spiked matrix were between 73% and 118%, the coefficient of variation was 4.1%~9.7%. The detection limits of the method were 0.19~1.07 ng·g^-1. This method, with easy manipulation, well purification, and good accuracy and repetitiveness, is suitable to determine the contents of the PCBs in the whale.