An HPLC method for the determination of aflatoxins is described. The aflatoxins are extracted with aqueous acetone and interfering compounds precipitated with CuCO₃. After defatting, the aflatoxins are extracted into CH₂Cl₂ for cleanup with silica Sep-pak® which eliminates other interfering compounds. The resulting extract is then treated with TFA to form the hemiacetal derivatives prior to final HPLC analysis. Data indicated that the method exhibits excellent accuracy and precision. In addition, it is time and solvent conservative.