In order to improve comprehensive utilization value of Fructus aurantii immaturus, based on existing extraction process of Fructus aurantii Immaturus, cogeneration technology of hesperidin and synephrine in Fructus aurantii Immaturus was presented. HPLC method for determination of hesperidin and synephrine were used, Fructus aurantii Immaturus was crushed and extracted by pH 0.3 Hydrochloric acid solution, the filtrate use Dowex 50(H+) strong acid cation to exchange, through vacuum concentration to get synephrine; while using alkali extracting the residue, after acid precipitation and vacuum drying process to obtain hesperidin, the cogeneration technical parameters were optimized, and 16 repeated trials were condcted. With cogeneration technology optimized, the purity of hesperidin was 95.0%~98.0%, and extraction rate was 24.0%~28.0%; purity of synephrine was more than 20.0%, and extraction rate of synephrine was above 3‰. Compared with traditional process, the production quality was improved, and the yields was increased.