This study described procedures for extracting and quantitation of hesperidin in the waste orange peel of Dezful. Two extracting procedure were used. In procedure A hesperidin was isolated from orange peel by extracting the dry peel first with petroleum ether, removing the essential oil and then with methanol. In procedure B alkaline extraction followed by acidification of the extract was used. It was purified by treatment with formamide-activated charcoal. Detailed analysis of UV, IR, 1HNMR, 13CNMR and Mass spectroscopic data confirm the structure and extent of purity of extracted hesperidin. The spectroscopic results of two extract showed that procedure A produced high extraction yield and more purified hesperidin. Pure hesperidin in gram quantity (11.7% for procedure A and 7.39% for procedure B) was obtained in one purification cycle.

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