Sulfamethazine residue in pork was determined by high pressure liquid chromatography. Effects of different solvent, solution pH of liquid partitioning and reuse of alumina column on sulfamethazine recovery were studied. Ace tonitrile and ethyl acetate were favor than aceton in a good recovery. Aqueous soluton pH ranged 5 to 8 was needed to extract sulfamethazine, and pH adjustment was recommended. Alumnia column could be reused 8 times without regeneration for negative samples.