Assessment of extraction procedures in the analysis of naturally contaminated grain products for deoxynivalenol (vomitoxin).

A comparison of 2 extraction solvent systems (acetonitrile-water, 21 + 4 and methanol-water, 1 + 1) and 3 mixing apparatus (high-speed blender, wrist-action shaker, and mechanical stirrer) was carried out for different extraction time periods. Methods were evaluated using uncontaminated corn spiked with pure deoxynivalenol (DON), field-inoculated (Fusarium graminearum) corn, and uncontaminated and naturally infected wheat in swine diets. After sample extraction, aliquots were passed through alumina-charcoal cleanup columns, evaporated to dryness, dissolved in 8% aqueous methanol, and injected onto the liquid chromatograph. Results confirm published reports of recoveries from DON-spiked samples; however, longer extraction times (less than or equal to 120 min) were required for naturally contaminated samples. Use of the high-speed blender resulted in faster extractions, but in our laboratory more samples could be more conveniently extracted simultaneously with the wrist-action shaker or mechanical stirrer. Less carryover (co-extraction) of interfering contaminants was observed when acetonitrile-water was used vs methanol-water. Results emphasize the importance of careful evaluation of extraction procedures with not only spiked samples but also naturally contaminated samples to establish extraction times required for maximum deoxynivalenol recoveries.