Gel permeation chromatography was applied as a clean-up step in a HPLC multiresidue method for the determination of several pesticides in plants, not amenable to analysis by GC. The pesticides investigated were diflubenzuron, triflumuron, clofentezine, hexythiazox and flufenoxuron. The clean-up technique resulted in a good separation of analytes from co-extractive matrix compounds. Complete HPLC separation of all pesticides was achieved under the conditions selected. The analytical procedure was characterized with high accuracy and precision and acceptable sensitivity to meet requirements for monitoring these pesticides in crops.