The aim of this research was to introduce a new rapid analysis method (heating of the multi-layer silica gel column/alumina column) for polychlorinated biphenyls in insulating oils, and to compare our new method with the analytical method currently used in Korea. The entire pretreatment procedure was completed within 2 hr, using about only 20 mL of solvents via our rapid analytical method. Furthermore, the pretreatment procedure can always be uniformly performed, regardless of oil type (JIS 1~JIS 7 and KS 1~KS 7). The recovery rates were more than 89%, with relative standard deviations below 6.0%. In conclusion, this rapid analytical method could reduce the pretreatment time and solvent usage by 1/10 and between 1/25 and 1/50, respectively, compared to analytical method currently used in Korea.