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液相色谱法测定鱼肉中土霉素残留前处理方法的改进
引用本文:朱晓华,吴光红.液相色谱法测定鱼肉中土霉素残留前处理方法的改进[J].中国兽药杂志,2010,44(5):4-8.
作者姓名:朱晓华  吴光红
作者单位:江苏省水产质量检测中心,南京,210017;农业部渔业产品质量监督检验测试中心(南京),南京,210017;江苏省淡水水产研究所,南京,210017
基金项目:江苏省科技公共服务平台项目 
摘    要:对液相色谱法测定鱼肉中土霉素残留的前处理方法中样品提取液浓度、提取次数、不同SPE小柱、SPE小柱洗脱液及洗脱体积进行了研究改进。结果表明,用1%的高氯酸分15、10、10 mL三次提取样品,离心后经HLB小柱净化,用20 mL 5%三乙胺甲醇溶液洗脱样品,回收率高。向样品中分别添加0.05、0.1、0.15 mg/kg三个浓度水平的土霉素时,回收率为82%~86%,RSD为6%~7%,最低检测限可达0.017 mg/kg。

关 键 词:土霉素  残留  高效液相色谱法  前处理  鱼肉
收稿时间:2010/3/10 0:00:00
修稿时间:2010/3/27 0:00:00

The Improvement of Sample Pretreatment on Oxytetracyline Residue Determination in Aquatic Products by HPLC
zhuxiaohua and.The Improvement of Sample Pretreatment on Oxytetracyline Residue Determination in Aquatic Products by HPLC[J].Chinese Journal of Veterinary Drug,2010,44(5):4-8.
Authors:zhuxiaohua and
Institution:ZHU Xiao-hua1,2,3,LIU Chang1,WU Guang-hong1,3 (1.Aquatic Products Analysis , Testing Center of Jiangsu Province,Nanjing 210017,2.Fishery Products Quality Supervision , Testing Center(Nanjing),Ministry of Agriculture,3.Freshwater Fishery Research Institute of Jiangsu Province,China)
Abstract:The effects of sample pretreatment on oxytetrecycline residue measurement in fish muscle by HPLC was studied.Such factors as concentration of extraction solvent,extraction time,SPE column,eluate and eluate volume for SPE column were compared.The results show that higher recovery is achieved when drugs in samples are extracted with 1% perchloric acid solution of 15 mL,10 mL,10 mL and cleaned up with a HLB column eluted with 20 mL methanol containing 5% triethylamine.When spiked with 0.05,0.1,0.15 mg/kg of ox...
Keywords:oxytetracyline  residue  HPLC  sample pretreatment  fish muscle  
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