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Journal of AOAC International





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The performance of a liquid chromatographic method for determining fumonisins in corn, animal feeds, and culture material was evaluated. Efficiencies of extractions with the following solvent systems were determined: acetonitrile-water (50 + 50, v/v), methanol-water (75 + 25, v/v), and 100% water. The acetonitrile solvent gave both higher extraction efficiencies and faster extraction times than the other 2 solvents. Extraction was followed by C18 solid-phase extraction column cleanup. Fumonisin B1 (FB1), fumonisin B2 (FB2), and fumonisin B3 (FB3) were measured by precolumn derivatization with o-phthalaldehyde followed by isocratic separation on a C18 reversed-phase column with a mobile phase of 50 mM potassium dihydrogen phosphate (pH 3.3)-acetonitrile (60 + 40). Commercially prepared poultry feed, corn, and Fusarium spp. corn cultures were analyzed at the following levels: FB1, 1.5 to 15,000 micrograms/g; FB2, 0.5 to 4000 micrograms/g; FB3, and 0.17 to 1,500 micrograms/g. Recoveries were 91-94%, 90-100%, and 81-93% for FB1, FB2, and FB3, respectively. Precision (coefficient of variation) was determined with pooled field samples and ranged from 2% at 19 micrograms/g for FB1 to 9% at 0.17 microgram/g for FB3. Time and pH studies of the formation of the fluorescent derivative and its stability were conducted. Complete reaction occurred at pHs above 7.9, with optimal pH for chromatography between 8.0 and 8.5. No statistically significant response differences were detected for reaction times ranging from 4 to 40 min; however, the detector signal was significantly reduced when reaction times were shorter than 4 min. Chromatograms of samples were free of interferences for all feeds, corn, and culture material tested


This article is from Journal of AOAC International, 78(4); 1002-1009. Posted with permission.

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