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This study evaluated the subcritical water hydrolysis (SWH) of brewer's spent grains (BSG) to obtain sugars and amino acids. The experimental conditions investigated the hydrolysis of BSG in a single flow-through reactor and in two sequential reactors operated in semi-continuous mode. The hydrolysis experiments were carried out for 120 min at 15 MPa, 5 mL water min⁻¹, at different temperatures (80 – 180 °C) and using an S/F of 20 and 10 g solvent g⁻¹ BSG, for the single and two sequential reactors, respectively. The highest monosaccharide yields were obtained at 180 °C in a single reactor (47.76 mg g⁻¹ carbohydrates). With these operational conditions, the hydrolysate presented xylose (0.477 mg mL⁻¹) and arabinose (1.039 mg mL⁻¹) as main sugars, while low contents of furfural (310.7 µg mL⁻¹), 5-hydroxymethylfurfural (<1 mg L^-1), and organic acids (0.343 mg mL⁻¹) were obtained. The yield of proteins …