Canada produces annually vast amounts of barley and canola straws. In this study, barley and canola straws were hydrolyzed using subcritical water (sCW) and pressurized aqueous ethanol (PAE) at 140-220 degrees C, 50-200 bar and 20-100% (v/v) ethanol concentrations for maximum removal of carbohydrates and phenolics. Total carbohydrates, phenolics, antioxidant activity and brown color formation were quantified via UV-spectrophotometer. Temperature and ethanol concentration were important process parameters for the removal of biocompounds from barley and canola straws. Optimum process conditions for removal of phenolics (45.4 +/- 1.8 mg GAE/g barley straw and 52.9 +/- 2.0 mg GAE/g canola straw) and carbohydrates (527.6 +/- 0.5 mg GE/g barley straw and 442.7 +/- 14.8 mg GE/g canola straw) were 180 degrees C, 50 bar and 20% ethanol. Furthermore, 54 and 45% of total lignin were removed using PAE (20%) from barley and canola straws, respectively. The FT-IR, TG, DTG and SEM analysis confirmed the removal of non-cellulosic materials.