Trichothecene mycotoxins are commonly distributed in crop fields in the world, and zearalenone has been found in cereals. Rapid and accurate methods for the determination of these mycotoxins is required to prevent the intoxication of humans, and to contribute to the supply of safe foods and feeds for human and livestock. Gas chromatography-mass spectrometry (GC-MS) is a useful method for the determination of these toxins. We describe here our current GC-MS analysis for the simultaneous determination of trichothecenes and zearalenone contaminants in cereals.