Fractionation or cleanup of samples extracts prior to instrumental analysis is used to remove coextracted materials that often interfere with the determination of target analytes. Such fractionations and cleanups are usually accomplished by column chromatography, gel permeation chromatography, or acid-base partitioning. This paper describes the application of solid-phase extraction cartridges containing silica gel, Florisil, or alumina to the fractionation and cleanup of sample extracts containing organochlorine pesticides, polychlorinated biphenyls, and phthalate esters. Several solvents were evaluated for cartridge elution to establish a procedure that will allow separation of polychlorinated biphenyls and phthalate esters from organochlorine pesticides. Furthermore, cartridge loading and the effects of matrix interferents such as those present in corn oil and diesel hydrocarbons were investigated.