Distinctive sensory characteristics increase the competitive advantage of distilled spirits. In Brazil, cachaça is the most consumed spirit, although consumption of whisky, mainly imported from the United States and Scotland, is also important. This study assessed the chemical and sensory quality of distilled spirits created from combinations of sugarcane juice and malted barley wort. Prepared separately and mixed in five different proportions, A – 100% sugarcane juice, B – 75% + 25%, C – 50% + 50%, D – 25% + 75%, E – 100% malted barley wort, fermented at 30°C with 1.5 g/L Saccharomyces cerevisiae LNF CA‐11 and Fermentis SafAleTM S‐33. The distillation method was based on Scotch whisky. After maturation in 2.5L oak barrels for 60 days, aged spirits were analysed for alcohol, copper, volatile congeners, ethyl carbamate, colour, total phenolic compounds, and maturation‐related congeners. Preference and descriptive tests were performed respectively by a panel of consumers and of experienced assessors. Statistical analyses used SAS (ANOVA and Tukey's test). Spirits from sugarcane juice combined with a higher percentage of malted barley wort had lower ethyl carbamate levels. The aging congeners, syringaldehyde and gallic acid were present in the highest concentrations. Spirit A ‐ 100% sugarcane juice ‐ had the highest concentration of aging congeners. Spirits A and C (50% sugarcane juice + 50% malted barley wort) achieved the best results in the sensory analysis. © 2021 The Institute of Brewing & Distilling