6533b7d2fe1ef96bd125eb5b
RESEARCH PRODUCT
Critical study of and improvements in chromatographic methods for the analysis of type B trichothecenes
J.j. MateoMisericordia JiménezA. LlorensR. Mateosubject
ChromatographyOrganic ChemistryExtraction (chemistry)TrichotheceneGeneral MedicineSensitivity and SpecificityBiochemistryHigh-performance liquid chromatographyAnalytical ChemistryElectron capture detectorchemistry.chemical_compoundSpectrometry FluorescenceFusariumchemistryCalibrationSpectrophotometry UltravioletSample preparationSolid phase extractionGas chromatographyEdible GrainTrichothecenesDerivatizationChromatography High Pressure Liquiddescription
Various analytical methods used in the analysis of type B trichothecenes (deoxynivalenol, nivalenol, 3- and 15-acetyldeoxynivalenol) in cereals were compared and optimised in this work. These methods use either GC-electron-capture detection (ECD) of trimethylsilyl, trifluoroacetyl and heptafluorobutyryl derivatives or HPLC with UV or photodiode array detection of analytes. A new HPLC procedure using fluorescence detection prior derivatisation with coumarin-3-carbonyl chloride has been also tested. Five extraction solvents and two solid-phase extraction cartridges (silica, Florisil) plus a especial clean-up column (MycoSep 225) were compared in order to obtain the best recovery of the mycotoxins with minimal presence of coextractives in the chromatograms. The chosen extraction solvent was a mixture of acetonitrile-water (84:16, v/v). The MycoSep 225 column was chosen as the best alternative for clean-up of grain samples. For GC-ECD analysis, derivatisation of analytes with heptafluorobutyric anhydride prior the final determination was chosen as the most suitable procedure. HPLC-photodiode array (at 221 nm) analysis was more suitable for determination of type B trichothecenes than HPLC of the fluorescent coumarin-3-carbonyl derivatives. Recoveries obtained in spiked corn, rice and wheat are reported. The utility of the proposed methodology was assayed in cereal cultures of various Fusarium strains.
year | journal | country | edition | language |
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2001-06-14 | Journal of Chromatography A |