Abstract:

A simple, rapid, sensitive and reliable high performance liquid chromatographic method for the simultaneous determination of nine sulfonamides (SAs) (sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxypyridazine, sufamonomethoxine, sulfachloropyridazine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline) in milk was developed. The method includes the shaking of the milk with phosphate buffer, centrifugation, and cleaning up on a C18 solid-phase extraction cartridge. The C18 cartridge was washed with water, and the SAs were eluted with methanol. After the evaporation, the residue was dissolved in ethyl acetate, and cleaned up on an amino solid-phase extraction column. Analytical separation was performed on an Inertsil ODS-3 column with photodiode-array detection at 270 nm under the gradient condition. The mean recoveries of SAs at the spiked levels of 10, 20, 40 μg/L were between 72.1% and 88.3%. The relative standard deviations were between 2.3% and 5.0%. The detection limits were 1.7-2.8 μg/L, and the quantification limits wer 5.7-9.2 μg/L.

Key words: milk , residue analysis, solid phase extraction (SPE), sulfonamides, high performance liquid chromatography （HPLC）