A rapid procedure for the determination of sulfamethazine in swine muscle and kidney is described. The method comprises sonication-aided extraction with dichloromethane, cleaning-up of the extract on a combination of silica and reversed-phase C18 Sep-Pak cartridges and analysis by high-performance liquid chromatography on a Hypersil ODS column using acetonitrile/ammonium acetate solution (10 mmol X 1(-1), pH 6.8) 1 + 3 v/v as the mobile phase. Detection was performed at 254 nm. Mean recoveries of added sulfamethazine from swine muscle and kidney, at levels of 0.05 to 0.5 micrograms X g-1, were 89.5 and 80.5%, respectively. After intramuscular injection of sulfamethazine into swine, residues in tissues were also determined. The application of ultrasonic energy for the extraction of sulfamethazine residues from animal tissues is also discussed.