Deoxynivalenol (DON), a mycotoxin produced in cereal grains infected by Fusarium Head Blight produced by Fusarium graminearium and Deoxynivalenol-3-β-D-glucopyranoside (DON-3G), were studied during processing using LC-MS-MS and GC. DON reduced significantly (P<0.05) 61.8% during milling into flour. Therefore, DON was concentrated mostly in the bran and germ. DON increased 40.8% during the fermentation stage of baking. DON increased in dough more than flour and mixed dough. Milling reduced by 23.7% but fermentation did not. But bread was significantly lower in DON-3G at 0.15 ppm than flour and dough at 0.31 ppm. The baking increased DON and decreased DON-3G showing a difference in stability of the mycotoxins during processing. Enzyme hydrolysis on DON using α-amylase, cellulase, protease, and xylanase, showed a significant increase with cellulase (20.8%), protease (11.4%), and xylanase (35.6%) compared to wheat composite. DON may be bound to the cell wall or protein component of the kernel.