An investigation for the occurrence of nivalenol (NIV), deoxynivalenol (DON) and zearalenone (ZEN) in cereals (ten wheat, one rye and one corn) harvested in Canada have been carried out using a procedure, which is rapid and sensitive for Fusarium mycotoxins. NIV, DON and ZEN were detected in 4, 9 and 9 out of ten wheat samples, and their average levels in the positives were 23 ng/g, 1257 ng/g and 9 ng/g, respectively. One rye and one corn were also contaminated with a minor amount of NIV. This is the first evidence for the natural occurrence of NIV in cereals grown in Canada, though its level was far less than DON.