OBJECTIVE：To sepa rate and identify the phenols compounds in Aurantii Fructus Immaturus ，and to provide reference for basic research of its effective substances. METHODS ：The phenols compounds were isolated and separated by silica gel，HW-40F gel column ，ODS reversed column and preparation HPLC. Their physicochemical properties and spectral data were used to identify the structures. RESULTS & CONCLUSIONS ：Totally 12 compounds were isolated from Aurantii Fructus Immaturus，identified as 6′-O-trans- cinnamoyl- 3，5-dihydroxyphenyl β-D-glucopyranoside（compound 1），methyl 3-（2′，4′- dihydroxy phenyl ）propionate（compound 2），phloroglucinol（compound 3），aurantiside A （compound 4），5，7，4′-trihydroxy-8， 3′-dimethoxyflavone-3-O-6″-（3-hydroxyl-3-methylglutaroyl） β-D-glucopyranoside （compound 5）， aromadendrin-7-O-β-D- glucopyranside（compound 6），hesperidin-7-O-β-D-glucoside（compound 7），naringin（compound 8），hesperidin（compound 9）， narirutin （compound 10），neoeriocitrin （compound 11），eriocitrin （compound 12）. Among them ，compound 1 is a new compound，and compounds 2 and 3 are isolated from Critus for the first time.