A sensitive and specific high-performance liquid chromatographic method for the identification and quantitation of chlorophacinone in animal tissues has been developed. Residues were extracted with chloroform-acetone (1:1, v/v). Clean-up of extracts was accomplished with a combined gel permeation-adsorption chromatographic procedure using Bio-Beads SX-3 and incorporating an on-line Sep-Pak silica cartridge. Residues were determined by ion-pair liquid chromatography, with the tetrabutylammonium ion as counter-ion, using a fixed-wavelength UV detector at 280 nm or a diode array detector at 285 nm. Recoveries from spiked liver tissue were around 90% at levels from 0.05 to 1 mg kg-1. A detection limit of 0.001 mg kg-1 could be achieved in animal tissues. The diode array detector confirmed identification by matching spectra for residues down to 0.1 mg kg-1 and below this level by multi-wavelength monitoring.