The material investigated were 27 maize grain-milled products, i.e.: corn flour (n = 12) and corn grits (n = 15) purchased in supermarkets in 2008. Contents of trichothecene of A and B types and of Zearalenone were determined in the material investigated using a high performance liquid chromatography (HPLC ) with MS/MS. Based on the analyses performed, it was found that the corn flours contained 9 of 12 mycotoxins under investigation. The mycotoxins found were as follows: NIV, DON, 3-AcDON, 15- AcDON, DAS, HT-2, T-2, T-2 TETRAOL, and ZON. It was reported that three mycotoxins were not present in this group, namely: FUS-X, NEO, and T-2 TRIOL. Six toxins were identified in the corn grits analysed, i.e.: NIV, DON, 3-AcDON, 15-AcDON, HT-2, and ZON. DON was found to be a prevailing toxin of the highest concentration in all the samples studied.