Current efforts are taken to increase resource efficiency, close material loops, and improve sustainable waste and by-products management. Thus, networking agro-food by-products andc onverting them into valuable products completely exhausting the potential of the raw material becomes significant. Model lignocellulosic and starch based biomass were subjected to pre-treatment with the application of acidic compounds, i.e. sulphuric (SA) and acetic (AA) acids. The response, i.e. total sugar content and derivatives content is investigated depending on variables changed during hydrolysis: concentration of acid, process duration, temperature and the size of the biomass particles. After saccharification, the hydrolysates were analysed via HPLC. Total reducing sugars concentration was in the range of 0.1 – 15.53 g/LAmong the substances present in the hydrolysates, protein, peptides, hydroxybenzyl acid (HA), 5-HMF, furfural (FF), vanillin (V), vanillic acid (VA), formic acid (FA) and levulinic acid (LA) were found in the range of 0.44 – 9.05 g/L and determined as total derivatives concentration. The aim of the study was to evaluate the measurable effects of the research and deliver information about the statistically important parameters for the process course and relations between the variables.