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A method for the combined extraction of the mycotoxins aflatoxin B1, B2, G1, G2, ochratoxin A (OTA) und zearalenone (ZEA) in cereals is described. After extraction with acetonitril/water a clean-up for the mycotoxins was made using solid-phase columns (SiOH) or a combination of two immunoaffinity columns (aflaochra- and zearala-test-column from Vicam). The aflatoxins, ochratoxin A and zearalenone were detected after pre-column derivatization with trifluoroacetic acid in one HPLC run. The clean-up using two combined immunoaffinity columns is suitable because the detection and determination limits are low.