title: 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.
authors.affiliation: Department of Plant Sciences, North Dakota State University, Fargo, North Dakota 58105, USA.
authors.forename: Bing
authors.initials: B
authors.lastname: Zhou
authors.forename: Yin
authors.initials: Y
authors.lastname: Li
authors.forename: James
authors.initials: J
authors.lastname: Gillespie
authors.forename: Guo-Qing
authors.initials: GQ
authors.lastname: He
authors.forename: Richard
authors.initials: R
authors.lastname: Horsley
authors.forename: Paul
authors.initials: P
authors.lastname: Schwarz
mesh_terms: D005670:Fusarium / Q000378:metabolism; D001467:Hordeum / Q000737:chemistry* / Q000382:microbiology; D010935:Plant Diseases / Q000382:microbiology; D012044:Regression Analysis; D012639:Seeds / Q000737:chemistry; D014255:Trichothecenes / Q000032:analysis* / Q000378:metabolism; D014269:Trifluoroacetic Acid
chemical_list: D014255:Trichothecenes; D014269:Trifluoroacetic Acid; C007262:deoxynivalenol