silica gel multilayer column, samples were analyzed by GC-MS/MS. This method was fast, effective and easy to operate. The limit of quantitation of the method was calculated to be 0.78 μg/kg for total PCBs. The recovery and the coefficient of variation of PCBs (n=5) from 6 fishes (Japanese sea perch, chub mackerel, yellowtail, salmon, pacific saury, and sardine) of total PCBs were 91-108% and 1-3%, respectively.