On the basis of the HPLC analysis, the process and products of enzymatic degradation of rye and corn starch by amolytic enzymes in mashing by the PLS technology (pressureless liberation of starch) have been presented. The results of monitoring of the sugar substrates utilization by Saccharomyces cerevisiae: D-2 and As-4 yeasts during three-day fermentation have been presented. An effective and quick method (by capilary GC) allowing to investigate the kinetics of by-product formation, Le. higher alcohols, aldehydes, methanol, during alcoholic fermentation has been described. It was found that the synthesis of fusel alcohols proceeded according to the Ehrlich's model and was dependent on the glucose accessibility in the base. The most intense formation of the carbonyl compounds (mainly acetic aldehyde) was observed in the phase of preliminary fermentation.