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An interlaboratory study was performed on behalf of the UK Food Standards Agency to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatographic (LC) method for the determination of deoxynivalenol in a variety of cereals and cereal products at proposed European regulatory limits. The test portion was extracted with water. The sample extract was filtered and applied to an immunoaffinity column. After being washed with water, the deoxynivalenol was eluted with acetonitrile or methanol. Deoxynivalenol was quantitated by reversed-phase LC with UV determination. Samples of artificially contaminated wheat-flour, rice flour, oat flour, polenta, and a wheat based breakfast cereal, naturally contaminated wheat flour, and blank (very low level) samples of each matrix were sent to 13 collaborators in 7 European countries. Participants were asked to spike test portions of all samples at a range of deoxynivalenol concentrations equivalent to 200–2000 ng/g deoxynivalenol. Average recoveries ranged from 78 to 87%. Based on results for 6 artificially contaminated samples (blind duplicates), the relative standard deviation for repeatability (RSDr) ranged from 3.1 to 14.1%, and the relative standard deviation for reproducibility (RSDR) ranged from 11.5 to 26.3%. The method showed acceptable within-laboratory and between-laboratory precision for all 5 matrixes, as evidenced by HorRat values <1.3.

The validation of a rapid, reliable and sensitive method for the simultaneous determination of Aflatoxins, Ochratoxin A, Zearalenone, Deoxynivalenol, Fumonisins, T-2 and HT-2 toxins, in nuts and cereals is reported. This method is based on a single extraction step using an acetonitrile/water mixture followed by the analysis of the diluted crude extract using ultra highperformance liquid chromatography with tandem mass spectrometry. The method performance characteristics were determined after spiking blank samples. The mean recoveries in spiked nuts ranged from 74.4% to 131.7%, while in cereals ranged from 52.8% to 113.9%. Limits of detection and quantification for nuts and cereals ranged 0.08-30.0 and 0.25-99.0 μg/kg, respectively. Validated method was used for monitoring mycotoxins in 120 samples. A total of 97 samples (81%) were contaminated with at least one of these mycotoxins, but only the 3% of the samples exceeded the maximum levels of the EU legislation.

An interlaboratory study was performed on behalf of the UK Food Standards Agency to evaluate the effectiveness of an affinity column cleanup liquid chromatography (LC) method for the determination of zearalenone (ZON) in a variety of cereals and cereal products at proposed European regulatory limits. The test portion is extracted with acetonitrile:water. The sample extract is filtered, diluted, and applied to an affinity column. The column is washed, and ZON is eluted with acetonitrile. ZON is quantified by reversed-phase LC with fluorescence detection. Barley, wheat and maize flours, polenta, and a maize-based baby food naturally contaminated, spiked, and blank (very low level) were sent to 28 collaborators in 9 European countries and 1 collaborator in New Zealand. Participants were asked to spike test portions of all samples at a ZON concentration equivalent to 100 μg/kg. Average recoveries ranged from 91–111%. Based on results for 4 artificially contaminated samples (blind duplicates) and 1 naturally contaminated sample (blind duplicate), the relative standard deviation for repeatability (RSDr) ranged from 6.9–35.8%, and the relative standard deviation for reproducibility (RSDR) ranged from 16.4–38.2%. The method showed acceptable within- and between-laboratory precision for all 5 matrixes, as evidenced by HorRat values <1.7.

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