The study was conducted on lemon and orange peels to study the chemical composition of these residues by determinism each of carbohydrate, protein, fat, ash, and fiber contents. The pectin was also separated and purified and studied using HPLC (High Performance Liquid Chromatography) and IR (Infrared Radiation) techniques. Finally studied the activity of  antioxidant activity of pectin and methanol, ethanol  and  acetone extracts; Lemon peel contents of crude protein, ash, fiber, fat and carbohydrate were (7.89%, 5.30%, 15.40%, 2.50% and 68.91%, respectively) monoclonal and bivalent sugars and their derivatives found in pectin were arabinose, galactose and glucose. Through HPLC analysis, and by IR analysis in the region from (1619: 2049) and from (3046: 3235), there were a groups of (COOH and CH₃) and pectin sugar was presented in the hexagonal ring structure. The area (616) nm and the antioxidant activity showed that the extract of methanol for lemon peel was the highest antioxidant as well as pectin orange peel   contents of crude protein, ash, fiber, fat and carbohydrate were (5.26%, 4.30%, 9.90%, 2.75%, and 77.79% respectively) monoclonal and bivalent sugars and their derivatives were found in pectin of orange were arabinose, galactose, glucose and mannose. Through HPLC analysis and by IR analysis in the regions (2050: 2359) and (3036: 3234) containing the presence of COOH and CH₃ Pectin sugar is presented by investigation at (615nm) in the hexagonal ring structure.