A simple and sensitive method has been developed for the analysis of two trichothecene mycotoxins (deoxynivalenol and nivalenol) in cereals. These toxins were extracted with acetonitrile/water (3:1), defatted with n-hexane and purified by a two-step chromatographic procedure using Florisil and Sep-pak columns. The amounts of deoxynivalenol (DON) and nivalenol (NIV) in the column eluates were quantitated by gas chromatography with electron capture detector and gas chromatography-mass spectrometry (selected ion monitoring). The limits of detection of the method were 2.0 micrograms/kg for DON and NIV with recoveries of the toxins spiked into polished rice, wheat and corn at 300 micrograms/kg averaging 87% and 86% respectively.
About 30% and 60% of nivalenol and deoxynivalenol, respectively, and less than 10% of zearalenone in naturally contaminated wheat remained after the wheat flour milling process. However, their contents in bran were 2.4-3.4 times those of the original wheat. The baking process (170C for 30min) did not affect the amounts of these toxins in either naturally contaminated flour or spiked flour.
By adopting a rapid and sensitive method for simultaneous detection of nivalenol (NIV), deoxynivalenol (vomitoxin, DON) and zearalenone (ZEN), the natural occurrence of these mycotoxins in Japan in retail marked cereal flours, popcorn and health foods (totalling 76 samples) was surveyed. Significant contamination by NIV and DON was observed in commercial wheat and barley flours, and partially milled grains which are consumed as rice ingredients. Of particular interest was the presence of DON in popcorn imported from the United States, and the high-level contamination of NIV and ZEN in job's-tears (Hatomugi in Japanese), a widely marketed health food.
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