The amount of higher alcohols produced in the tested samples of raw spirits was low and oscillated in the range of 1.680–4.134 g/L EtOH. The highest amount of isobutanol was noted in the general content of fusel alcohols. The content of fusel alcohols is a crucial parameter regarding the spirit use in the production of ethyl tert-butyl ether. Quality requirements for biofuels biocomponents strictly determine the amount of higher alcohols, i.e., they cannot exceed 2% [v/v].