N,N-dimethyl-trimethylsilyl-carbamate as a derivatizing agent in gas chromatography of trichothecene mycotoxins

摘要

N,N-dimethyl-trimethylsilyl-carbamate, a commercially available silylating agent, has been tested in the derivatization of trichothecenes for the first time. Its reaction with alcohols is an autocatalytic, non-equilibrium process with volatile by-products. As a consequence of these advantageous characteristics N,N-dimethyl-trimethylsilyl-carbamate proved to be easily utilizable and effective for the derivatization of all studied trichothecenes, namely deoxynivalenol (DON), nivalenol (NIV) and 4,15-diacetoxyscirpenol (DAS). During testing also, optimum conditions (temperature: 15 degreesC, reaction time: 35 min) were established for the trimethylsilylation and for the gas chromatographic determination of the above-mentioned three trichothecenes. The linearity of the detector response was found to be proper in the 5-1100 ng range. (Given in the grams of trichothecene equivalent to the derivatives injected). The limit of detection is less than I ng for each of the studied trichothecenes. Relative standard deviations of the peak heights ranged from 0.75 to 4.32%. (C) 2004 Elsevier B.V. All rights reserved.