固相萃取-高效液相色谱法检测鱼粉中三聚氰胺

Determination of Melamine in Fish Meal by SPE-HPLC

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%。

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%.