Determination of Deoxynivalenol in White Flour, Whole Wheat Flour, and Bran by Solid-Phase Extraction/Liquid Chromatography: Interlaboratory Study

Abstract

A liquid chromatographic (LC) method for determining deoxynivalenol (DON) in white flour, whole wheat flour, and bran at or above the U.S. Food and Drug Administration advisory level of 1 microgram/g was evaluated by an interlaboratory study. Test samples of processed wheat (flour and bran) were extracted by blending with acetonitrile-water (84 + 16). Extracts were filtered and passed through a solid-phase extraction (SPE) column. The eluate was then chromatographed on a reversed-phase LC column with a water-methanol gradient. DON was measured at 220 nm. Naturally contaminated white flour, whole wheat flour, and bran samples and spiking solutions of DON to be added to the 3 commodities at 0.5, 1.0, and 2.0 micrograms/g were sent to 4 collaborators in Kansas, Louisiana, Missouri, and Washington states. Three collaborators completed the study. Average recoveries of DON from the 3 commodities spiked at 0.5, 1.0, and 2.0 micrograms/g were 94, 87, and 97%, respectively. Within-laboratory relative standard deviations for repeatability (RSDr) ranged from 3.1 to 21.7% and between-laboratory relative standard deviations for reproducibility (RSDR) ranged from 10.8 to 38.7%. On the basis of the results of this study, the SPE/LC method for DON in white flour, whole wheat flour, and bran was adopted as a peer-verified method by AOAC INTERNATIONAL.