Anticipating the need for an analytical micro procedure for determining polychlorinated biphenyls (PCBs), dichlorodiphenyltrichloroethane (DDT) and DDT metabolites in several hundred adipose samples taken by needle biopsy, surgery, or autopsy, the authors developed an analytical micro procedure that eliminates the need for liquid-liquid partitioning in the cleanup of chlorinated pesticide residues in fat samples. In the procedure, the column chromatography step fulfills the function of both the partitioning and column chromatography steps. For the analysis of DDT and DDT metabolites, a 44% sulfuric acid on silica gel chromatography column is used to remove the bulk of lipids and other oxidizable components from the hexane extract. For the analysis of PCBs, a 10% silver nitrate on silica gel chromatography column is used to retain the lipids, DDT and DDT metabolites.