食品科学 ›› 2009, Vol. 30 ›› Issue (8): 235-237.doi: 10.7506/spkx1002-6630-200908052

• 分析检测 • 上一篇    下一篇

高效液相色谱-荧光检测法测定水产品中4种磺胺类药物残留量

张小军,郑 斌*,陈雪昌   

  1. 浙江省海洋水产研究所
  • 收稿日期:2008-06-21 修回日期:2008-12-06 出版日期:2009-04-15 发布日期:2010-12-29
  • 通讯作者: 郑 斌*, E-mail:zhengbin67@163.com

Simultaneous Determination of 4 Sulfonamide Residues in Fishery Products by High Performance Liquid Chromatography with Fluorescence Detection

ZHANG Xiao-jun ZHENG Bin* CHEN Xue-chang   

  1. (Zhejiang Marine Fisheries Research Institute, Zhoushan 316100, China)
  • Received:2008-06-21 Revised:2008-12-06 Online:2009-04-15 Published:2010-12-29
  • Contact: ZHENG Bin* E-mail:zhengbin67@163.com

摘要:

建立高效液相色谱-荧光检测法测定水产品中4种磺胺类药物残留量的方法。均质后的样品用乙酸乙酯提取,稀盐酸反萃取,正己烷脱脂,荧光胺衍生,反相色谱柱分离,荧光检测器检测,磺胺5-甲氧嘧啶为内标物,内标法定量。4种磺胺类药物磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶和磺胺甲基异噁唑的线性范围为0.01~0.2mg/kg,线性相关系数均大于0.9934;在0.01~0.2mg/kg 范围内四个添加水平范围内的平均回收率为83.0%~91.3%,相对标准偏差为3.89%~8.80%,方法检出限为0.01mg/kg。

关键词: 水产品, 高效液相色谱, 荧光检测, 磺胺类药物

Abstract:

A method for determination of sulfonamide residues in fishery products by using high performance liquid chromatography (HPLC) equipped with fluorescence detector was established. The homogenized sample was extracted with ethyl acetate, back extracted with 2 mol/L hydrochloric acid, degreased with hexane, derived with fluorescamine, separated by reverse-phase chromatographic column, determined by a fluorescence detector and quantified with an internal standard of sulfamete. The results showed that the linear ranges of sulfadiazine, sulfamerazine, sulfamethazine, sulfamethoxazole are between 0.01 mg/kg and 0.2 mg/kg, and their linear correlation correlations are over 0.9934. Furthermore, in the ranges of 0.01 to 0.2 mg/kg, their average recoveries are between 83.0% and 91.3% with the RSDs of 3.89% to 8.80%, and their detection limits are 0.01 mg/kg.

Key words: fishery products, high performance liquid chromatography (HPLC), fluorescence detection, sulfonamide

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