[Simultaneous determination of nine sulfonamide residues in milk using solid phase extraction and high performance liquid chromatography].
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 microg/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 microg/L, and the quantification limits wer 5.7 - 9.2 microg/L.
Wu
Yinliang
Y
Quality Control and Inspection Center for Domestic Animal Products, Ministry of Agriculture, Beijing 100026, China. wupaddyfield@tom.com
Zhao
Li
L
Liu
Yongjun
Y
Jiang
Yanbin
Y
Liu
Xingguo
X
Shen
Jianzhong
J
D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D013412:Sulfadimethoxine / Q000032:analysis / Q000737:chemistry; D013418:Sulfamethazine / Q000032:analysis / Q000737:chemistry; D013421:Sulfamethoxypyridazine / Q000032:analysis / Q000737:chemistry; D000077589:Sulfathiazole; D013432:Sulfathiazoles / Q000032:analysis / Q000737:chemistry; D013449:Sulfonamides / Q000032:analysis / Q000737:chemistry*
D013432:Sulfathiazoles; D013449:Sulfonamides; D013412:Sulfadimethoxine; D013418:Sulfamethazine; D013421:Sulfamethoxypyridazine; D000077589:Sulfathiazole