A capillary gas chromatographic-mass spectrometry with quadruple ion trap was applied to nine polychlorinated biphenyl (PCB) congeners in waste oil. The optimized procedure involves solvent extraction using dimethyl sulfoxide (DMSO) in first step and mixture of ethyl acetate and hexane in second step. Extraction efficiency was monitored by using pyrene-d10 as surrogate standard. The separation of PCB congeners was done in VF-5MS (30mx 0.25mmx 0.25 µm) column and analysed on GC-MS using selective ion monitoring mode (SIM). The method was calibrated using two internal standards; phenanthrene-d10 and chrysene-d12. Correlation coefficients of all studied congeners ranged from0.9993 to 0.9999 for 7 point calibration. Recoveries of PCB congeners fromwaste oil are over 94%with RSD below 5 % (n = 6). The method is suitable for the analysis of PCB congeners in waste oils with high sensitivity and accuracy.