Doehlert Matrix Design for Optimization of the Determination of Bound Deoxynivalenol in Barley Grain with Trifluoroacetic Acid (TFA)

Abstract

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 degrees 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.

A survey of free and conjugated deoxynivalenol in the 2008 corn crop in Ontario, Canada

“…DON recovery following acid digestion was not as great as previously reported in optimization studies with corn and wheat,20 except for one sample showing an increase of 85%. Recovery was also lower than those reported by Liu et al 28 for wheat and by Zhou et al 29 for barley. Reasons for these differences are unclear.…”

Optimization of mesoporous titanosilicate catalysts for cyclohexene epoxidation via statistically guided synthesis

“…Hence, the DM approach has been widely utilized in analytical sciences, as an optimization tool and as a simple alternative to orthogonal design [47]. The method has been utilized successfully in oil refining, homogeneous catalysis, heavy metal analysis and food science, for optimization of experimental and analytical parameters [54][55][56][57][58][59]. ESI, Sects.…”

Doehlert uniform shell designs and chromatography

“…After this first application, uniform shell designs have been primarily used in the development of GC sample treatment procedures by optimizing the recovery [14,15,[27][28][29] and the intensity of the analytical signals [24,[30][31][32][33]. The optimization of the GC instrumental parameters by means of Doehlert designs has been rarely considered in the literature.…”