Territrems A and B, tremorgenic mycotoxins in the rice culture of Aspergillus terreus, were extracted with hot chloroform. The toxins were cleaned on a silica gel column by direct adsorption-concentration of the extracts followed by desorption with chloroform-acetone (9:1, vol/vol). Crude toxin mixtures were separated by silica gel column chromatography and eluted with benzene-ethyl acetate (65:35, vol/vol). The method gave 112 mg of territrem A, 379 mg of territrem B, and 80 mg of their mixture from 4 kg of rice per batch. The criteria of extraction, cleanup, and separation are provided.