高效液相色谱-原子荧光法测定水产品中甲基汞含量

建立水产品中甲基汞含量的高效液相色谱-原子荧光测定方法。样品经硫脲加氯化钾、盐酸溶液提取，提取液过固相萃取小柱净化，用流动相定容，过0.45μm微孔滤膜，采用高效液相色谱-原子荧光法检测，外标法定量。结果表明，甲基汞在2～50μg/L质量浓度范围内，色谱峰面积与甲基汞质量浓度之间线性关系良好(相关系数为0.9995)，以20、200、1000μg/kg 三个添加量在空白样品中添加甲基汞，样品平均回收率为80.2%～87.1%，相对标准偏差为3.4%～6.8%，方法的定量限为20μg/kg。该方法简便快速，基体干扰小，精密度、准确性均能满足水产品中甲基汞分析。

Determination of Methylmercury in Aquatic Products by HPLC-AFS

A high performance liquid chromatography-atomic fluorescence spectrometry(HPLC-AFS) method was developed for the determination of methylmercury in aquatic products.Samples were extracted with a mixture of vitriol,potassium chloride and hydrochloric acid.Then the extract was cleaned up on an SPE column,diluted with the HPLC mobile phase and filtrated through a 0.45 μm pore size membrane prior to HPLC-AFS analysis.The quantification of methylmercury was carried out using the external standard method.Good linearity between chromatographic peak area and methylmercury concentration ranging from 2 to 50μg/L was found(R2=0.9995).Average recoveries for methylmercury in different blank aquatic products spiked at 20,200,1000μg/kg were 80.2%-87.1% with relative standard deviations(RSD) between 3.4% and 6.8%.The method exhibited a detection limit of 20μg/kg.The method had the advantages of simplicity and little matrix interference,and meanwhile its precision and accuracy could meet the requirements for the analysis of methylmercury in aquatic products.