A rapid and efficient method has been developed to recover aflatoxin from cheese and other foods. The procedure involves: (a) blending the sample with a mixture of chloroform, methanol, and water (solvents are used in such proportions that a miscible (monophasic) system is formed, (b) adding more chloroform and water so the mixture becomes biphasic, (c) filtering to remove the food residue, (d) separating the lower chloroform layer which contains virtually all of the aflatoxin, and (e) purification, if necessary, of the material in step (d) after it has been concentrated. Purification is achieved by sequential addition of methanol, water, and hexane; recovery of tho methanol-water fraction; and extraction of aflatoxins from it with chloroform. Purification can be eliminated if the substrate contains little or no lipid or pigment which, if present, interfere with thin-layer chromaographic analysis. Extraction can be done in approximately 35 min and purification in approximately 20 min. When aflatoxins were added to various substrates, the method recovered 92–98% B1 and 96–100% G1 from rice; 95–96% B1 and 90–95% G1 from peanut butter; 93–94% B1 and 92–98% G1 from Cheddar cheese; 100% B1 and G1 from corn meal; 91–100% B1, 91–100% B2, 90–96% G1, and 92–100% G2 from brick cheese; and 97–100% B1, 95–100% B2, 92–100% G1, and 98–100% G2 from a liquid culture medium.