title: Use of a multifunctional column for the determination of deoxynivalenol in grains, grain products, and processed foods.
abstract: Deoxynivalenol (DON), also known as vomitoxin, belongs to a class of naturally occurring mycotoxins produced by Fusarium spp. DON, 12, 13-epoxy-3,7 trihydroxytrichothec-9-en-8-one, is one of the most frequently detected mycotoxins in agricultural commodities worldwide. A method consisting of extraction, filtration, column cleanup, and RP-HPLC-UV separation and quantitation was validated for the determination of DON in grains (rice and barley), grain products (whole wheat flour, white flour, wheat germ, and wheat bran), and processed foods (bread, breakfast cereals, and pretzels). A 25 g test portion was extracted with 100 mL acetonitrile-water (84 + 16, v/v). After blending for 3 min, the supernatant was applied to a multifunctional column (MycoSep 225). The purified filtrate (2 mL) was evaporated to dryness and redissolved in the mobile phase. The toxins were then subjected to RP-HPLC-UV analysis. The accuracy and repeatability characteristics of the method were determined. Recoveries of DON added at levels ranging from 0.5 to 1.5 microg/g for all test matrixes were from 75 to 98%. SD and RSD(r) ranged from 0.7 to 11.6% and 0.9 to 12.7%, respectively. Within-laboratory HorRat values were from 0.1 to 0.7 for all matrixes analyzed. The method was found to meet AOAC method performance criteria for grains, grain products, and processed foods. The identity of DON in naturally contaminated test sample extracts was confirmed by HPLC/MS/MS analysis.
authors.affiliation: U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Office of Regulatory Science, Division of Bioanalytical Chemisty, College Park, MD, USA. baoleiqd@yahoo.com.cn
authors.forename: Lei
authors.initials: L
authors.lastname: Bao
authors.forename: Carolyn J
authors.initials: CJ
authors.lastname: Oles
authors.forename: Kevin D
authors.initials: KD
authors.lastname: White
authors.forename: Chelsea
authors.initials: C
authors.lastname: Sapp
authors.forename: Mary W
authors.initials: MW
authors.lastname: Trucksess
mesh_terms: D001939:Bread / Q000032:analysis; D002851:Chromatography, High Pressure Liquid; D002523:Edible Grain / Q000737:chemistry*; D005433:Flour / Q000032:analysis; D005504:Food Analysis / Q000379:methods*; D001467:Hordeum / Q000737:chemistry; D013058:Mass Spectrometry; D012275:Oryza / Q000737:chemistry; D012015:Reference Standards; D015203:Reproducibility of Results; D012996:Solutions; D013056:Spectrophotometry, Ultraviolet; D053719:Tandem Mass Spectrometry; D014255:Trichothecenes / Q000032:analysis*; D014908:Triticum / Q000737:chemistry
chemical_list: D012996:Solutions; D014255:Trichothecenes; C007262:deoxynivalenol