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[采用固相萃取和高效液相色谱法同时测定牛奶中九种磺胺类药物残留量]

[Simultaneous determination of nine sulfonamide residues in milk using solid phase extraction and high performance liquid chromatography].

作者信息

Wu Yinliang, Zhao Li, Liu Yongjun, Jiang Yanbin, Liu Xingguo, Shen Jianzhong

机构信息

Quality Control and Inspection Center for Domestic Animal Products, Ministry of Agriculture, Beijing 100026, China.

出版信息

Se Pu. 2007 Sep;25(5):728-31.

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 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.

摘要

建立了一种简单、快速、灵敏且可靠的高效液相色谱法,用于同时测定牛奶中的9种磺胺类药物(SAs)(磺胺嘧啶、磺胺噻唑、磺胺二甲嘧啶、磺胺甲氧嗪、磺胺间甲氧嘧啶、磺胺氯哒嗪、磺胺甲恶唑、磺胺二甲氧嘧啶和磺胺喹恶啉)。该方法包括用磷酸盐缓冲液振荡牛奶、离心,以及在C18固相萃取柱上进行净化。用C18柱先后用水冲洗,并用甲醇洗脱SAs。蒸发后,残渣溶解于乙酸乙酯中,并在氨基固相萃取柱上进行净化。在梯度条件下,于Inertsil ODS-3柱上进行分析分离,采用光电二极管阵列检测,检测波长为270nm。SAs在10、20、40μg/L加标水平下的平均回收率在72.1%至88.3%之间。相对标准偏差在2.3%至5.0%之间。检测限为1.7 - 2.8μg/L,定量限为5.7 - 9.2μg/L。

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