In this work, the effect of Détente Instantanée Contrôlée (DIC) (French for instant controlled pressure drop) on the total polyphenol, flavonoids, α-tocopherol contents, and antioxidant activities of olive leaves was studied. Olive leaf extracts were pre-treated at one cycle DIC under 0.1 MPa pressure for 11 s and followed by an extraction with 95% ethanol at 55 °C during 3 h. The phenolic compounds, flavonoïds, oleuropein, and α-tocopherol contents were determined, showing 66.63 mg gallic acid equivalent (GAE)/g db, 12 mg catechin equivalent (CE)/g db, 43.9 mg/g db, and 0.15 mg/g db for the untreated leaves against 239.37 mg GAE/g db, 28 mg CE/g db, 70.3 mg/g db, and 0.59 mg/g db for DIC-treated leaves, respectively. Therefore, DIC allows more availability of bioactive compounds contributing to a high antiradical activity (DPPH) compared to a synthetic antioxidant butylated hydroxytoluene (BHT). Both extracts showed a total antioxidant capacity (method of phosphomolybdenum) greater than that of the standard BHT. Likewise, both extracts have a reducing power (FRAP test) significant concentration-dependent. The DIC-treated leaves showed a higher antioxidant capacity compared to that of untreated leaves. Thus, DIC could be an effective treatment to promote the extraction of bioactive molecules of high antioxidant activities from olive leaves.