A common method for analyzing polychlorinated biphenyls (PCBs) in foods, uses alkaline saponification, n-hexane extraction, column chromatography purification, and GC/MS measurement. It has been reported that this method is complicated, uses a large amount of organic solvents, and is susceptible to contaminants. The application described here introduces an analytical method used for analysis of PCBs in five fish samples distributed (1 great amberjack sample, 3 sea bream samples, and 1 flounder sample) which were purified using a commercial silica gel minicolumn, followed by analysis with GC/MS/MS. The use of GC/MS/MS greatly reduces the impact of contaminants.