食品科学 ›› 2005, Vol. 26 ›› Issue (1): 176-179.

• 分析检测 • 上一篇    下一篇

高效液相色谱法同时测定鳗鱼及其制品中八种磺胺类药物

 林海丹, 谢守新, 吴映璇   

  1. 广州出入境检验检疫局食品实验室; 广州出入境检验检疫局食品实验室
  • 出版日期:2005-01-15 发布日期:2011-09-19

Determination of Sulfonamides Veterinary Drugs Residues in Eels and Roasted Eels by SPE-HPLC

 LIN  Hai-Dan, XIE  Shou-Xin, WU  Ying-Xuan   

  1. Technical Center for Inspection and Quarantine on Food of Guangzhou CIQ
  • Online:2005-01-15 Published:2011-09-19

摘要: 建立了高效液相色谱测定鳗鱼及其制品中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺甲氧嗪、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺间二甲氧嘧啶、磺胺喹噁啉等八种磺胺类药物残留量的方法。研究了鳗鱼及其制品中八种磺胺类药物残留的提取、净化和高效液相色谱条件。样品经二氯甲烷提取、MCX阳离子固相萃取小柱净化,以CloversilC18柱,甲醇、1%乙酸(V/V)梯度洗脱分离,紫外检测器检测、外标法定量。结果表明,样品添加0.1mg/kg的回收率为80%~93%,定量测定低限为0.02mg/kg。方法已应用于实际样品的测定。

关键词: 鳗鱼, 磺胺, 高效液相色谱法, 固相萃取

Abstract: The determination of sulfonamides veterinary drug residues in eels and roasted eels,including sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxypyridazine,sulfamethoxaz-ole,sulfamonomethoxine,sulfadimethoxine,sulfaquinoxa- line was studied. Homogenized tissue was extracted with dichloromethane and centrifuged. The supernatant was filtrated and evaporated. The dry residue was dissolved in 1% acetate acid-methanol(65:35, V/V). After addition of hexane, the aqueous layer was collected and diluted with 5% acetate acid. The diluent was applied to a pre-conditioned MCX SPE column, washed with 5% acetate acid-methanol(50:50, V/V) and eluted with 5% ammonia methanol. Elution was analysed by LC on a column (250mm× 4.6mm i.d.) of Cloversil C18 ODS, with 1% acetate acid-methanol as mobile phase(1.0ml/min) and detection at 265nm. The correlation coefficient was larger than 0.999. The detection limit were 0.020mg/kg. The recoveries were in the range of 80%~93%.

Key words: SPE-HPLC, sulfonamides, eels and rosted eels