The valorization of the brewer’s spent grain (BSG) generated in a craft beer industry was studied by subcritical water hydrolysis in a semi-continuous fixed-bed reactor. Temperature was varied from 125 to 185 °C at a constant flow rate of 4 mL/min. Biomass hydrolysis yielded a maximum of 78% of solubilized protein at 185 °C. Free amino acids presented a maximum level at 160 °C with a value of 55 mg free amino acids/gprotein-BSG. Polar amino acid presented a maximum at lower temperatures than non-polar amino acids. The maximum in total phenolic compounds was reached at 185 °C. This maximum is the same for aldehyde phenolic compounds such as vanillin, syringic and protocatechuic aldehyde; however, for hydroxycinnamic acids, such as ferulic acid and p-coumaric, the maximum was obtained at 160 °C. This allows a fractionation of the bioactive compounds. Subcritical water addresses opportunities for small breweries to be incorporated within the biorefinery concept.
