Polychlorinated biphenyls (PCB's), which are used in industry worldwide (i), have been found as residues in numerous wildlife species (2-7). Because of the similarity in chemical characteristics, PCB compounds interfere with gas liquid chromatographic (GLC) analysis of certain chlorinated hydrocarbon insecticides (8). In the present study, we sought a rapid microanalytical procedure for separation of PCB's from DDT and its analogues before analysis with GLC. A small silica gel column was found to be suitable for removing two of the Aroclor series of PCB's (1254 and 1260) from DDT and its analogues.