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Nivalenol (NIV) and Deoxynivalenol (DON) belong to a class of natural-occurring mycotoxins produced by Fusarium sp.NIV and DON are frequently detected mycotoxins in agricultural commodities worldwide.A method consists of extraction, immunoaffinity column cleanup and reversed phase liquid chromatographic (RPLC)/UV separation and quantitation, was validated for the determination of NIV and DON in wheat and corn.