The objective of this study was to assess the suitability of buckwheat grain for agricultural distillate production. The effects of the method of starch liberation on the physicochemical composition of the prepared mashes, fermentation results, the concentration of volatile compounds in the obtained distillates, and their organoleptic features, were investigated. The raw materials used were two cultivars of buckwheat grains, Panda and Kora. Both cultivars were characterized by similar starch content, however Panda cultivar had a signifi cantly higher content of reducing sugars. Fermentation of the Kora cultivar-based mashes resulted in a higher fermentation effi ciency (up to approximately 85% of the theoretical yield) compared to the Panda cultivar-based mashes (up to approx. 75%). Of the tested methods of starch liberation, the pressure-thermal treatment was revealed as superior, especially in the case of the Panda cultivar. In the case of the Kora cultivar, both the pressure-thermal method and the pressureless method of starch liberation resulted in a high process effi ciency (up to 85% of the theoretical). Supplementation of the buckwheat mashes with (NH 4) 2 HPO 4 improved fermentation results. The highest scores in sensory assessment were given to distillates from mashes prepared with the pressure-thermal treatment, which contained relatively low concentrations of undesirable compounds, such as acetaldehyde and methanol, and revealed pleasant organoleptic features.