A fast and sensitive gas chromatographic/negative ion chemical ionization mass spectrometric method for the simultaneous detection and quantification of several simple trichothecene mycotoxins and related molecules with good precision has been developed. The method consists of the conversion of the polar trichothecenes into their volatile and stable heptafluorobutyryl esters, followed by gas chromatographic/mass spectrometric analysis of the derivatives. The derivatives were ionized under chemical ionization conditions and the negative ions were monitored. The samples were screened for the presence of trichothecenes by monitoring one characteristic ion by selected ion monitoring for each analyte. The detected compounds were confirmed by monitoring 5-6 characteristic ions by selected ion monitoring whenever the amount of analyte present was insufficient to obtain a full scan negative ion chemical ionization mass spectrum. Two semi-synthetic trichothecenes, 4-deoxyverrucarol and 16-hydroxyverrucarol, were investigated and found to be adequate internal standards both for detection and quantification of these toxic compounds. Femtogram and low picogram (1-5 pg) quantities of these compounds could be detected and confirmed, respectively, by this procedure. A short clean-up procedure using Sep-Pak (silica gel) cartridges was developed and found to be applicable for the analysis of some real samples. Several spiked and real samples were analysed by this method, with excellent sensitivity and precision.