A simple and sensitive procedure is described for the analysis of aflatoxins B1B2, G1and G2in cereal and animal feedstuff samples. Aflatoxins are extracted with dichloromethane:water (10:1). Gel permeation chromatography (GPC) using a column packed with Bio‐beads S‐X3 and dichloromethane:hexane (3:1) as the eluent is used for clean‐up of extracts prior to separation and quantification of aflatoxins by HPLC. The eluent fraction containing the aflatoxins is concentrated by evaporation under reduced pressure and the aflatoxins separated by reverse phase HPLC on an ODS column. Quantitative results have been obtained at levels down to 1μg/kg, and average recoveries from samples of wheat, maize and compound feed spiked at levels of 10 and 40μg/kg were greater than 80%, 70% and 65% respectively.