Six compounds were isolated from ethanol extract of fresh fruit peel of Fortunella margarita (Lour.) Swingle by column chromatography. By means of MS and NMR technique, the six compounds are identified as follows: fortunellin(Ⅰ), phloretin-3′,5′-di-C-β-glucopyranoside (Ⅱ), rutin(Ⅲ), 4′-methoxy vitexin-2″-O-α-L-rhamnopyranoside(Ⅳ),rhoifolin(Ⅴ) and β-daucosterol (Ⅵ), in which contents of compound Ⅰ and Ⅱ are the highest and compound Ⅴ is obtained from fruit peel of F.margarita at the first time.