The effect of conventional solvent extraction, CSE, ultrasound assisted extraction, UAE, microwave assisted extraction, MAE and supercritical CO 2 extraction, SC-CO 2 on the total phenols content, total flavonoids, individual flavonoids and antioxidant activity of orange peel were compared. Neohesperidin (from 0.624 ± 0.013 for SC-CO 2 extraction to 1.045 ± 0.001 g100 g orange peel powder for MAE) and hesperidin (from 0.407 ± 0.008 for SC-CO 2 extraction to 0.836 ± 0.029 g/100 g orange peel powder for UAE) are the major flavonoids (80% of total flavonoids by MAE and 87% by CSE) of orange peel whatever the used extraction method. The method giving the highest total phenol and flavonoid contents is microwave assisted extraction (2.363 ± 0.014 g GAE/100g orange peel powder), followed by ultrasound assisted extraction, conventional solvent extraction, and supercritical CO 2 extraction. However, antioxidant activity (DPPH method) cannot be correlated to TPC, TFC or individual flavonoids. Orange peel extracted by CSE (ethanol (80%), m/v: 5 g:50 ml, 30 min, 35°C, mechanical stirring at darkness, 3 successive extractions) presents the higher radical scavenging capacity compared to the other extracts obtained by MAE (Ethanol (80%), m/v: 5 g: 50 ml, 10s, 35°C, 170 W, 3 successive extractions) and UAE (ethanol (80%), m/v: 5g:50 ml, 30 min, 35°C, magnetic stirring at darkness, 3 successive extractions, 125W), SC-CO 2 extraction (ethanol (80%), m/v:5 g:50 ml, 30 min, 35°C, 22 MPa, 3 successive extractions). Besides, no additivity on the antioxidant activity is found with the DPPH method.