Managing deoxynivalenol (DON) risks is crucial for the sustainability of small grain farms. One approach involves profitable utilization of contaminated grain resources, addressing potential losses from food safety concerns. This study explored distillation as a high-value alternative for utilizing DON-contaminated grain. Naturally DON-contaminated rye and wheat were used in two pilot-scale distillation runs involving milling, mashing, fermentation, and distillation. The ground grain, slurry, fermented mash, and post-distillation mash were sampled during process. For the distilled spirit, 29 fractionated samples, each containing 125 ml, were collected starting with the first drop of liquor. The fractionated samples were sequentially combined into 6 pooled samples of up to 5 individual fractions. If a pooled sample had a DON level above the lower limit of quantification, samples of the pool were tested individually. All distillate samples were tested by ELISA with a limit of quantification at 0.05 µg/ml and a limit of detection at 0.01 µg/ml. For both rye and wheat runs, DON levels in all distillate fractions were consistently below 1 µg/ml, reducing from barely quantifiable to below 0.01 µg/ml. The DON levels in ground rye and wheat were 3.62 and 2.69 µg/g, respectively. In the rye distilled spirit, the first pooled sample had a DON level of 0.1 µg/ml, and the first two fractions of that pool had DON levels of 0.1 and 0.06 µg/ml. In the wheat distilled spirit, the first pooled sample had a DON level of 0.05 µg/ml, and the first fraction of that pool had DON level of 0.12 µg/ml. All other distilled spirits had DON levels below 0.01 µg/ml. The results showed that distilled liquor from DON-contaminated rye and wheat contains very low DON levels at most. From a food safety perspective, considering DON-contaminated grain as an ingredient for distilled spirits appears viable.