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高效液相色谱-荧光检测法测定鳗鲡中孔雀石绿和结晶紫残留

Determination of malachite green and gentian violet residues in Anguilla japonica by high performance liquid chromatography with fluorescence detector

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【作者】 郑斌赵红萍冷凯良于慧娟汪云泉陈雪昌钟志

【Author】 ZHENG Bin1,ZHAO Hong-ping2,LENG Kai-liang3,YU Hui-juan4,WANG Yun-quan5,CHEN Xue-chang1,ZHONG Zhi1(1.Zhejiang Marine Fisheries Research Institute,Zhoushan 316100,China;2.Chinese Academy of Fishery Sciences,Beijing 100039,China;3.Yellow Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Qingdao 266071,China;4.East China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Shanghai 200090,China;5.Zhoushan Entry-Exit Inspection and Quarantine Bureau,Zhoushan,316000,China)

【机构】 浙江省海洋水产研究所中国水产科学研究院中国水产科学研究院黄海水产研究所中国水产科学研究院东海水产研究所舟山市出入境检验检疫局浙江省海洋水产研究所 浙江舟山316100北京100039山东青岛266071上海200090浙江舟山316000浙江舟山316100

【摘要】 本研究建立了高效液相色谱-荧光检测法测定鳗鲡(Anguilla japonica)中孔雀石绿和结晶紫残留量的新方法。样品中残留的孔雀石绿或结晶紫用硼氢化钾还原为其相应的代谢产物隐色孔雀石绿或隐色结晶紫,用乙腈、乙酸铵缓冲溶液提取,二氯甲烷液液萃取,PRS固相萃取柱净化,反相色谱柱分离,荧光检测器检测,外标法定量。孔雀石绿和结晶紫混合标准工作溶液质量浓度范围为1~600μg/L时,该方法的线性关系极好,相关系数均为0.9999。该方法定量检出限为0.4μg/kg。当空白样品中孔雀石绿和结晶紫添加水平为0.4~100μg/kg时,孔雀石绿回收率为70.0%~90.6%,结晶紫回收率为73.0%~87.2%,相对标准偏差均小于10%。

【Abstract】 Due to its potential carcinogenicity,mutagenity and teratogenicity to animals,malachite green(MG) has been forbidden as a veterinary medicine in the European Union.MG has also been forbidden in aquaculture industry in China.Since MG is easily available at low cost and highly effective,concern about its illegal use in fishery should still begiven.In fish,MG can be easily absorbed into tissues and extensively metabolized to the reduced,colourless compound,leucomalachite green(LMG).A new method for determination of MG and gentian violet(GV) residues in Anguilla japonica using high performance liquid chromatography(HPLC) equipped with fluorescence detector was established.The sample was extracted with acetonitrile-buffer mixture followed by partitioning with dichloromethane.Cleaning up and isolation was performed on PRS solid phase extraction(SPE) column.The extract was analyzed by using a HPLC system incorporating purospher C18 column and fluorescence detector and external standard.Linearity was demonstrated with standards over the range 1-600 μg/L with relative coefficient of 0.999 9.The limit of quantification was 0.4 μg/kg.Recoveries of MG and GV from sample tissues fortified at 0.4-100 μg/kg were 70.0%-90.6% and 73.0%-87.2%,respectively.The RSDs were less than 10%.

【基金】 国家标准(20051850-T-326)
  • 【文献出处】 中国水产科学 ,Journal of Fishery Sciences of China , 编辑部邮箱 ,2007年06期
  • 【分类号】S948
  • 【被引频次】32
  • 【下载频次】544
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