In recent years, agricultural and industrial residues have attracted a lot of interest in the recovery of phytochemicals used in the food, pharmaceutical, and cosmetic industries. In this paper, a study on the recovery of phenol compounds from Lycium spp. leaves is presented. Ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) have been used with alcoholic and hydroalcoholic solvents. Methanolic UAE was the most successful technique for extracting phenols from Lycium leaves, and we used on leaves from L. barbarum and L. chinense cultivated in Italy. The extracts were then characterized as regards to the antioxidant properties by in vitro assays and the phenol profiling by a high performance liquid chromatography-diode array detector (HPLC-DAD). Chlorogenic acid and rutin were the main phenol compounds, but considerable differences have been observed between the samples of the two Lycium species. For example, cryptochlorogenic acid was found only in L. barbarum samples, while quercetin-3-O-rutinoside-7-O-glucoside and quercetin-3-O-sophoroside-7-O-rhamnoside only in L. chinense leaves. Finally, multivariate statistical analysis techniques applied to the phenol content allowed us to differentiate samples from different Lycium spp. The results of this study confirm that the extraction is a crucial step in the analytical procedure and show that Lycium leaves represent an interesting source of antioxidant compounds, with potential use in the nutraceutical field.