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固相萃取-高效液相色谱法检测鱼粉中三聚氰胺
引用本文:黄武,章晶晶,郁小朴,孙艳波.固相萃取-高效液相色谱法检测鱼粉中三聚氰胺[J].广州化工,2010,38(8):192-194.
作者姓名:黄武  章晶晶  郁小朴  孙艳波
作者单位:1. 湛江出入境检验检疫局检验检疫技术中心,广东,湛江,524001
2. 湛江师范学院化学科学与技术学院,广东,湛江,524048
摘    要:建立了鱼粉中三聚氰胺的固相萃取-高效液相色谱分析方法。色谱柱为Waters symmetry C18柱(4.6mm×150mm,5μm),柱温35℃;流动相为0.01mol/L庚烷磺酸钠-0.01mol/L柠檬酸(pH=3.0)缓冲液∶乙腈混合溶液(92∶8,V∶V);检测波长为240nm,流速1.0mL/min,进样量20μL,保留时间约7.313min。此条件下三聚氰胺在0.2~10mg/L范围内具有良好的线性关系,添加回收率为86.3%~100.1%,RSD小于5.0%。

关 键 词:三聚氰胺  固相萃取  液相色谱  鱼粉

Determination of Melamine in Fish Meal by SPE-HPLC
HUANG Wu,ZHANG Jing-Jing,YU Xiao-pu,SUN Yan-bo.Determination of Melamine in Fish Meal by SPE-HPLC[J].GuangZhou Chemical Industry and Technology,2010,38(8):192-194.
Authors:HUANG Wu  ZHANG Jing-Jing  YU Xiao-pu  SUN Yan-bo
Affiliation:1 Inspection and Quarantine Technology Center of Zhangjiang Entry-Exit Inspection and Quarantine Bureau,Guangdong Zhanjiang 524001;2 Chemistry Science and Technology School,Zhanjiang Normal University,Guangdong Zhanjiang 524048,China)
Abstract:A solid phase extraction-high performance liquid chromatography(SPE-HPLC) method was developed for the determination of melamine in fish meal and the effects of the mobile phase composition on separation were investigated.The melamine after being extracted by 0.2 mol/L perchloric acid solution from samples was separated completely on a waters symmetry C18 column(4.6mm × 150mm,5μm) with 0.01 mol/L heptane sulfonic-0.01 mol/L citric acid solution and acetonitrile (pH = 3,92∶8,by volume) as mobile phase.The UV detection wavelength was set at 240nm.The result showed that the retention time was about 7.313min.The standard curve was 0.2mg/L ~ 10mg/L (R =0.99995).And the recoveries at three fortification levels(1,2,5 mg/kg) were 86.3% ~100.1% with RSD 5%.
Keywords:melamine  SPE  HPLC  fish meal
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