Analysis of trichothecene mycotoxins by gas chromatography with electron capture detection
1994
Croteau, S.M. | Prelusky, D.B. | Trenholm, H.L.
A sensitive gas chromatographic (GC) method for the quantitative analysis of 13 trichothecene mycotosins in corn was developed. Derivatives sensitive to electron capture detection (ECD) were formed using heptafluorobutyric anhydride in the presence of the acylation catalyst (dimethylamino)pyridine. Optimal reaction conditions were found to consist of reacting a sample for 20 min at 60 degrees C in a toluene-acetonitrile (8 + 2) reaction solvent. An aqueous wash with 5% (w/v) sodium bicarbonate effectively removed excess derivatizing reagent. Chromatographic separation was achieved with a DB-1701, 15 m X 0.25 mm i.d., or SE-54, 15 m X 0.32 mm i.d., fused silica capillary column with a 0.25-micrometers film thickness. Both columns were used to ascertain the identity of trichothecenes coeluting with unidentified endogenous substances. The procedure was applied to samples of corn extracted with acetonitrile-water (84 + 16). The extract was pretreated with ammonium sulfate to reduce the amount of interferences and to enhance the estraction of the less polar trichothecenes prior to cleanup on a charcoal-alumina column. The fluoroacyl derivatives were prepared and the mistures subjected to ECD-GC. Depending on the trichothecene, their minimum quantifiable limit in corn ranged from 50 to 200 micrograms/kg.
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