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福建水产 ›› 2013, Vol. 35 ›› Issue (1): 40-46.

• 论文与报告 • 上一篇    下一篇

液相色谱-柱后衍生法测定水产品中磺胺类药物检测条件优化

汤水粉   

  1. 福建省水产研究所
  • 收稿日期:2012-11-12 修回日期:2012-12-26 出版日期:2013-02-25 发布日期:2013-02-22
  • 通讯作者: 汤水粉

Optimization of testing conditions for determinating sulfonamides residues in aquatic products by post-column derivation high performance liquid chromatography

Shui-Fen TANG   

  • Received:2012-11-12 Revised:2012-12-26 Online:2013-02-25 Published:2013-02-22
  • Contact: Shui-Fen TANG

摘要: 在水产品中八种磺胺类药物测定的高效液相色谱-柱后衍生法方法标准的基础上,对检测条件进行优化和改进,实现了水产品中八种磺胺类(磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲噁唑、磺胺多辛、磺胺异噁唑、磺胺喹噁啉)药物残留的高灵敏检测。磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶和磺胺二甲基嘧啶线性范围:0.025~0.5 μg/ml;磺胺甲噁唑、磺胺多辛、磺胺异噁唑线性范围:0.05~1.0 μg/ml;磺胺喹噁啉线性范围:0.1~2.0 μg/ml。线性相关系数均大于0.9990。对鲈鱼空白样品进行八种磺胺类药物的加标实验,加标量为5μg/kg~100μg/kg时回收率在84.2%~109%之间,相对标准偏差为1.64%~10.6%。

关键词: 磺胺, 水产品, 柱后衍生, 高效液相色谱, sulfonamides, aquatic products, post-column derivatization, high performance liquid chromatography

Abstract: The testing conditions for determinating sulfonamides residues was optimized, base on the standard method of determinating eight sulfonamides in aquatic products by post-column derivatization high performance liquid chromatography (HPLC) method. In the optimized conditions, eight sulfonamides (sulfadiazine, sulfathiazole, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfamethoxypyridazine, sulfisoxazole, sulfaquinoxaline) residues in aquatic products were separated and detected. The calibration curves were linear in a concentration range of 0.025~0.5μg/ml for sulfadiazine, sulfathiazole, sulfamerazine, sulfamethazine; 0.05~1.0μg/ml for sulfamethoxazole, sulfamethoxypyridazine, sulfisoxazole and 0.1~2.0μg/ml for sulfaquinoxaline, with r > 0.999. The average recoveries were 84.2%~109% and the relative standard deviation was in the range of 1.64%~10.6% for spiked weever sample with 5μg/kg~100μg/kg of sulfonamides.

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