Mango (Mangifera indica L.) is one of the most important fruits in the world. Mango peel is an important by-product that is rich in polyphenols and it could have high economic value if it is effectively utilized. Phenolic characterization is an essential step in the commercial utilization of mango peel by-products as food ingredients. Herein, qualitative and quantitative analyses of two Australian mango peel “Keitt” and “Kensington Pride” (K&P) by-products were conducted while using liquid chromatography coupled to electrospray ionisation and quadrupole time of flight mass spectrometry (LC-ESI-QTOF/MS) and high-performance liquid chromatography coupled to photodiode array detector (HPLC-PDA). A total of 98 polyphenols compounds were tentatively identified in both Keitt peel and K&P peel extracts, with greater concentrations of these compounds being detected in Keitt peel. The total phenolic content (TPC), total flavonoid content (TFC), and a total tannin content (TTC) were determined. The antioxidant activity of mango peel by-products was determined while using 2,2-diphenyl-1-picrylhydrazyl (DPPH) antioxidant assay, ferric reducing antioxidant power (FRAP) assay, and 2,2-azino-bis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS) radical scavenging assay. Keitt peel contained higher concentrations of total phenolic compounds, flavonoids, and tannins and had higher antioxidant capacity in DPPH, FRAP, and ABTS assays as compared to K&P peel. In HPLC-PDA quantification, the predominant phenolic compounds in Keitt peel and K&P peel were catechin (62.32 ± 0.01 mg/gd.w.) and syringic acid (17.78 ± 0.01 mg/gd.w).