Gas Chromatography with Electron Capture and Mass Spectrometric Detection of Deoxynivalenol in Wheat and Other Grains

Abstract

A method for determining deoxynivalenol (DON) in wheat has been developed in conjunction with an assessment of contamination in Canada. The sample is extracted with methanol-water; the extract is treated with 30% aqueous ammonium sulfate solution and extracted with 4 portions of ethyl acetate. After further cleanup by column chromatography, the sample extract is derivatized with AT-heptafluorobutyrylimidazole, and the DON tris-heptafluorobutyrate is determined by gas-liquid chromatography with electron capture detection. Mass spectrometric single ion monitoring at m/z 884 is used for confirmation. Detection limits are ≤0.01 μg DON/g and recoveries from wheat, using the proposed method, averaged 72 and 80% in 2 different laboratories, with coefficients of variation of 10.2 and 10.0%, respectively. The method is also applicable to determining DON in barley and corn and T-2 toxin in wheat. Virtually 100% contamination by DON of the 1980 Ontario white winter wheat and Quebec red spring wheat crops was found, based on 72 analyses made in this laboratory, but western Canadian wheat contained little or no DON.

Effect of Cultural Practices, Soil Phosphorus, Potassium, and pH on the Incidence of Fusarium Head Blight and Deoxynivalenol Levels in Wheat

“…14% moisture). The grain was placed in a freezer at -14°C until analyzed for DON concentration by Research Foods of Toronto by the method of Scott et al (12). The grain was ground, and a 50-g subsample was used for analysis.…”

Chronic Feeding Study of deoxynivalenol in B6C3F1 male and female mice

“…l), a trichothecene mold metabolite with structural similarities to several other toxic products (T-2, HT-2, diacetoxyscirpenol) produced by strains of Fusarium. While the initial analytical data indicated that levels in grain were generally below 1 pprn DON, some samples of wheat and corn exceeded 8.0 ppm [1,2], and this prompted a concerted effort by the Canadian Health Protection Branch to determine the potential human health hazard associated with this toxicologically uncharacterized material.…”

Detection of Scab‐Damaged Hard Red Spring Wheat Kernels by Near‐Infrared Reflectance

“…Numerous procedures are available for measurement of DON level concentration in wheat meal and flour, including those based on thin-layer chromatography (Truckness et al 1984;Fernandez et al 1994), liquid chromatography (Chang et al 1984;Trenholm et al 1985;Rajaklyä et al 1987), gas chromatography (GC) (Terhune et al 1984;Ware et al 1984;Scott et al 1986;Tacke et al 1996), GC with mass spectrometry (Scott et al 1981), and enzyme-linked immunosorbent assay (ELISA) (Casale et al 1988;Usleber et al 1991Usleber et al , 1993Abramson et al 1998). However, these procedures are not adaptable to rapid (<1 min/sample) testing for inspection or process control.…”