Rapid and economical removal of extraneous co-extractives from pesticide residue extracts of water is made possible by the use of microcleanup columns. Three adsorbents–alumina, silica gel, and Florisil–as well as a variety of solvent systems were investigated. The recovery and cleanup of aldrin, chlordene, p,p’-DDD, p,p’-DDE, o,p’-BDT, p,p’-DDT, dieldrin, endrin, heptachlor, heptachlor epoxide, hexachlorobicycloheptadiene, hexachlorocyclopentadiene, isodrin, lindane, and methoxychlor were satisfactory, using any of the 3 adsorbents. The phosphorothioate pesticides malathion, methyl parathion, and parathion, however, could not be successfully recovered from Florisil when a modified Mills procedure was attempted. The micro-cleanup columns may also be used to perform a preliminary separation of a number of compounds that are difficult to resolve by GLC.