A simple and rapid method, using supercritical fluid extraction (SFE) with off-line high-performance liquid chromatography for the isolation and determination of nicarbazin, a popular broad-spectrum coccidiostatic drug used principally in poultry, is described. Results show good repeatability with a minimum quantification level of 0.4 microgram g-1 and mean 'spiked' recoveries of 98%, 100% and 99% using poultry feeds (n = 18), eggs (n = 28) and chicken tissue (n = 20), respectively. SFE using carbon dioxide is proposed as an alternative isolation method to the current Association of Official Analytical Chemists (AOAC) procedure which involves the use of large volumes of a harmful solvent (dimethylformamide) and requires a long tedious separation and clean-up regime (6 h) prior to its determination.