Doehlert Matrix Design for Optimization of the Determination of Bound Deoxynivalenol in Barley Grain with Trifluoroacetic Acid (TFA)
2007
Zhou, B. | Li, Y. | Gillespie, J. | He, G.Q. | Horslev, R. | Schwarz, P.
Fusarium head blight (FHB) is an impediment to barley production in many regions of the world. Tricothecene toxins, associated with FHB-infected grain, particularly, deoxynivalenol (DON), pose a serious threat to human and animal health. Recent research has suggested that a portion of the DON present on grain is bound and escapes detection through conventional determination. The objective of this study was to optimize a method for determination of nonextractable DON in barley grain using trifluoroacetic acid (TFA). A Doehlert matrix design was performed to determine the optimal conditions for time, temperature, and TFA concentration. These conditions were treated with 1.25 N TFA in 86:14 acetontrile/water for 54 min at 133 °C. Cleanup, derivatization, and determination of DON by a gas chromatography electron capture detector (GC-ECD) was as normal. Treatment of the test sample resulted in the release of an additional 58% DON under the optimized conditions and an increase of 9-88% in a set of verification samples.
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