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高效液相色谱法测定池塘底泥中呋喃西林的研究
引用本文:魏涯,岑剑伟,郝淑贤,黄卉,赵永强,辛少平,李来好.高效液相色谱法测定池塘底泥中呋喃西林的研究[J].南方水产,2014(1):71-77.
作者姓名:魏涯  岑剑伟  郝淑贤  黄卉  赵永强  辛少平  李来好
作者单位:中国水产科学研究院南海水产研究所,农业部水产品加工重点实验室,国家水产品加工技术研发中心,广东广州510300
基金项目:现代农业产业技术体系建设专项资金(CARS-49);国家科技支撑计划项目(2012BAD28B00);茂名市科技计划项目(2011A01002)
摘    要:文章研究了池塘底泥中呋喃西林残留量的提取和检测方法,以上V(甲醇):V(二氯甲烷)=3:7混合溶剂提取,提取效果较好;比较了振荡提取和超声波辅助加热提取法,后者提取能力较强;优化了高效液相色谱测定的色谱条件,在C18反相色谱柱上分离,梯度洗脱比等度洗脱能获得更好峰形,分离效果更好。以V(甲醇):V(二氯甲烷)=3:7作为提取溶剂、超声波辅助加热法(35 kHz,强度100%,40 ℃)提取,回收率为80%~95%,相对标准偏差小于10%,检测限达到0.250 μg?kg-1。该方法回收率高、稳定性好、灵敏度高、操作简便。

关 键 词:底泥  呋喃西林  超声波提取  高效液相色谱

HPLC determination of nitrofurazone in sediment of aquaculture pond
WEI Ya,CEN Jianwei,HAO Shuxian,HUANG Hui,ZHAO Yongqiang,XIN Shaoping,LI Laihao.HPLC determination of nitrofurazone in sediment of aquaculture pond[J].South China Fisheries Science,2014(1):71-77.
Authors:WEI Ya  CEN Jianwei  HAO Shuxian  HUANG Hui  ZHAO Yongqiang  XIN Shaoping  LI Laihao
Institution:(Key Lab. of Aquatic Product Processing, Ministry of Agriculture; National R&D Center for Aquatic Product Processing; South China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Guangzhou 510300, China)
Abstract:This paper studies the extraction and detection methods for nitrofurazone residues in sediment of aquaculture pond. The extraction by methanol-methylene chloride (3:7) mixed solvent achieved good effects. We compared oscillation extraction with ultrasonic-assisted heating extraction, finding that the latter extracted more. The HPLC chromatographic conditions had been optimized. Isolated on a C18 reversed-phase column, gradient elution obtained better peaks and better separation than isocratic elution. With methanol-methylene chloride (3:7) as extraction solvent, the ultrasonic-assisted heating method (35 kHz, intensity of 100%, 40 ℃) for extraction obtained 80%~95% recovery, and the relative standard of deviation was less than 10% and the detection limit reached 0.250 μg?kg-1. The user-friendly method has high recovery, good stability and high sensitivity.
Keywords:sediment  nitrofurazone  ultrasonic extraction  HPLC
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