The new approach using the Peak Pattern Method was conducted for the analysis of polychlorinated biphenyls (PCBs) from the papers or paper products to provide certain hygienic data for the recycled papers as well as white papers. The height of the each peak, obtained from the PCBs standards, was transformed to the spectrum to compare with that of the samples. In addition to the results of the single PCBs standards, the pattern of mixed PCBs standards with the adequate concentration and ratios were obtained prior to the analysis of the paper samples. The test showed excellent repetition within 5% variation, and the recoveries of PCBs ranged from 92% to 97%. The PCBs, considered as a hazard material, were analyzed using the Peak Pattern Method from six different types of paper samples including the roll tissue. It could not find the same pattern of the PCBs peaks from all of the paper samples.