Abstract: The sample of cereals was extracted with a mixture of acetonitrile-H2O (84+16), and the extract obtained was separated by centrifugation and purified by passing through self-made SPE column of neutral alumina-activated carbon-SiO2. The purified deoxynivalenol (DON) and nivalenol (NIV) in the solution after filtration were derivatized with a mixture of TMSI-BSA-TMCS (3+3+2), and the derivatized products were used for GC analysis. RTX-5MS capillary column was used for separation and electron-capture detector (ECD) was adopted in determination. Linear relationships between values of peak area and mass concentration of DON and NIV were obtained in the same range of 0.05-4.0 mg·L-1, with same detection limits of 0.01 mg·kg-1. The proposed method was applied to the analysis of wheat meal, giving values of recovery in the ranges of 92.6%-96.6% for DON and 90.9%-94.1% for NIV. Values of RSD′s (n=5) found were less than 6%.