A liquid chromatographic (LC) method is described for determination of ochratoxin A in animal feeds and cereal grains. Samples are initially extracted with chloroform-ethanol (8 + 2) and 5% acetic acid in water. Extracts are purified using a silica gel cartridge followed by a cyano cartridge. The samples are evaporated, diluted to a known volume, and analyzed using a 10 cm column of 3 micron C18 and a fluorescence detector. The method was applied to a variety of animal feeds and cereal grains at levels of 1.0-0.005 ppm added ochratoxin A. The overall recovery was 90.6% +/- 3.6.