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Starch and VB12 wastewater with higher COD and ammonia nitrogen concentration, contains a large number of difficult biodegradable material, complex composition, is difficult to deal with. In recent years, with the increasingly stringent wastewater discharge standards, require the use of a stable and efficient wastewater treatment process for purification treatment of high concentration of ammonia nitrogen in wastewater and the refractory organic pollutants, to achieve discharge standards. Upflow Anaerobic Sludge Blanket (UASB)—Anoxic/Oxic(A/O) process was employed in a wastewater treatment of starch and Vitamin B12 wastewater, which was 5 000 m3/d with highly concentrated organic pollutants and ammonia. The efficiency and reliability of the process has been proven. The results of the system operation show that the concentration of the effluent COD, ammonia and total nitrogen (TN) were at 78.4 mg/L, 18.7 mg/L and 41.1 mg/L, and the treatment efficiencies of COD, ammonia and TN reached over 99%, 92.1%, 82.7%, respectively, when the influent COD and TN concentration were in the ranges of 8 544~9 720 mg/L and 240~250 mg/L. The quality of the treated wastewater met the first-class discharge standards in Integrated Wastewater Discharge Standard(GB 8978—1996).