A method is described for the determination of eight trichothecenes of type A and B in a variety of complex matrices including heavily moulded and pigmented cereals, whole cereal ears, cereal-based foods, mixed feeds and faeces from swine. Trichothecenes were determined as their trifluoroacetyl derivatives by gas chromatography with ion-trap mass spectrometry detection operating in chemical ionization mode. Isobutane was chosen as reactant gas and optimum parameters of measurement were determined. For sample preparation a clean-up procedure was developed using a combination of Florisil and cation-exchange cartridges for solid-phase extraction. Limits of detection and quantification as well as recoveries are described.