In order to extract antioxidant phenolic compounds from spent grain (SG) two extraction methods were studied: the ultrasound-assisted method (US) and the Ultra-Turrax method (high stirring rate) (UT). Liquid to solid ratios, solvent concentration, time, and temperature/stirring rate were optimized. Spent grain extracts were analyzed for their total phenol content (TPC) (0.62 to 1.76 mg GAE/g SG DW for Ultra-Turrax pretreatment, and 0.57 to 2.11 mg GAE/g SG DW for ultrasound-assisted pretreatment), total flavonoid content (TFC) (0.6 to 1.67 mg QE/g SG DW for UT, and 0.5 to 1.63 mg QE/g SG DW for US), and antioxidant activity was measured using 2, 2-diphenyl-2-picrylhydrazyl (DPPH) free radical (25.88% to 79.58% for UT, and 27.49% to 78.30% for UT). TPC was greater at a high stirring rate and high exposure time up to a certain extent for the Ultra-Turrax method, and at a high temperature for the ultrasound-assisted method. P-coumaric acid (20.4 ± 1.72 mg/100 SG DW for UT, and 14.0 ± 1.14 mg/100 SG DW for US) accounted for the majority of the phenolic found compounds, followed by rosmarinic (6.5 ± 0.96 mg/100 SG DW for UT, and 4.0 ± 0.76 mg/100 SG DW for US), chlorogenic (5.4 ± 1.1 mg/100 SG DW for UT, and non-detectable for US), and vanillic acids (3.1 ± 0.8 mg/100 SG DW for UT, and 10.0 ± 1.03 mg/100 SG DW for US) were found in lower quantities. Protocatechuic (0.7 ± 0.05 mg/100 SG DW for UT, and non-detectable for US), 4-hydroxy benzoic (1.1 ± 0.06 mg/100 SG DW for UT, and non-detectable for US), and caffeic acids (0.7 ± 0.03 mg/100 SG DW for UT, and non-detectable for US) were present in very small amounts. Ultrasound-assisted and Ultra-Turrax pretreatments were demonstrated to be efficient methods to recover these value-added compounds.