食品科学 ›› 2012, Vol. 33 ›› Issue (4): 230-233.doi: 10.7506/spkx1002-6630-201204049

• 分析检测 • 上一篇    下一篇

高效液相色谱-在线柱后衍生荧光检测法同时测定水产品中14种磺胺类药物残留

郑 斌,余海霞,杨会成,廖妙飞,傅光明,张小军   

  1. 1.浙江省海洋开发研究院 2.浙江大学舟山海洋研究中心 3.浙江省海洋水产研究所
  • 出版日期:2012-02-25 发布日期:2012-02-14
  • 基金资助:
    浙江省优先主题重点农业项目(2009C12008)

Simultaneous Determination of 14 Sulfonamide Residues in Fishery Products by High Performance Liquid Chromatography with online Postcolumn Derivatization and Fluorescence Detection

ZHENG Bin,YU Hai-xia,YANG Hui-cheng,LIAO Miao-fei,FU Guang-ming,ZHANG Xiao-jun   

  1. 1. Zhejiang Marine Development Research Institute, Zhoushan 316100, China;2. Ocean Research Institute of Zhoushan, Zhejiang University, Zhoushan 316100, China; 3. Zhejiang Marine Fisheries Research Institute, Zhoushan 316100, China
  • Online:2012-02-25 Published:2012-02-14

摘要: 建立水产品中14种磺胺类药物的高效液相色谱-柱后衍生荧光检测法。均质后的水产品试样用乙酸乙酯提取、盐酸溶液反萃取、正己烷脱脂、反相色谱柱分离、在线柱后衍生、荧光检测器检测、内标法定量。14种磺胺类药物(磺胺、磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶、磺胺5-甲氧嘧啶、磺胺二甲基嘧啶、磺胺甲氧哒嗪、磺胺氯哒嗪、磺胺6-甲氧嘧啶、磺胺甲基异噁唑、磺胺多辛、磺胺异噁唑、磺胺二甲氧哒嗪、磺胺喹噁啉)的线性范围为2.5~800μg/L,线性相关系数均大于0.9934;在2.5~200μg/kg三个添加水平范围内的平均回收率为88.9%~98.6%,相对标准偏差均小于6.96%。14种磺胺类药物的定量检出限为2.5~20μg/kg。方法重现性好、灵敏度高,杂质干扰少,广泛适用于水产品中磺胺类药物残留的检测。

关键词: 水产品, 高效液相色谱, 在线柱后衍生, 磺胺类药物

Abstract: A new method for the determination of 14 sulfonamide (sulfanilamide, sulfadiazine, sulfathiazole, sulfamerazine, sulfameter, sulfamethazine, sulfamethoxypyridazine, sulfachlorpyridazine, sulfamonomethoxine, sulfamethoxazole, sulfadoxine, sulfafurazole, sulfadimethoxine, and sulfaquinoxaline) residues in fishery products using high performance liquid chromatography (HPLC) equipped with fluorescence detector was established. Homogenized samples were extracted with ethylacetate, reverse-extracted into hydrochloric acid, defatted with hexane, separated by reversed-phase column chromatography, treated by on-line post-column derivatization, detected using a fluorescence detector, and quantified using the internal standard method. The linear range of the method for detecting the sulfonamides was from 2.5 to 800 μg/L, and the relative coefficients were all above 0.9934. The mean recoveries across spike levels varying from 2.5 to 200μg/kg were between 88.9% and 98.6% with RSDs less than 6.96%. The limits of quantification for the sulfonamides were 2.5-20μg/kg. The method exhibited good repeatability, high sensitivity, little interference and was widely suitable for the determination of sulfonamide residues in aquatic products.

Key words: fishery products, high performance liquid chromatography, online post-column derivatization, sulfonamides

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