LC-氢化物-ICP联用技术分析测定水产动物及其制品中汞的形态

Determination of Mercury Speciation in Aquatic Animals and Their Products by LC-hydride Generation-ICP

本文将电感耦合等离子体发射光谱仪与高效液相色谱-氢化物发生相结合,建立一种简单、高效的分析方法用于检测水产动物及其制品中的甲基汞(Met Hg)、乙基汞(Et Hg)及无机汞(Hg2+)。采用微波酸提取对样品进行前处理,优化色谱条件,载液浓度等,进而验证方法的精密度、检出限、准确度、加标回收率。结果表明:当流动相中甲醇含量为5%,L-半胱氨酸浓度为0.10%时,分离效果、峰型和仪器响应值较好,基本消除汞的记忆效应。在7min内实现了无机汞、甲基汞、乙基汞的分离。线性关系良好(r>0.9990),相对标准偏差(RSD%)<10.00%,方法定量限分别为0.023、0.032和0.038 mg/kg。以鱼类、贝类、甲壳类三种基质样品进行加标回收实验,回收率在82.50%~98.40%之间,采用两种水产动物标准物质BCR463和TORT-3验证了方法的准确性好。本方法前处理简单、分离效果、精密度好、准确度高,适用于水产动物及其制品中汞形态的分析测定,为汞的形态分析研究提供了一种新的方法依据。

A simple and efficient method for the determination of methylmercury(MetHg),Ethyl Mercury(EtHg)and inorganic mercury(Hg2+)in aquatic animals and their products was developed by combining Inductively coupled plasma with High-performance liquid chromatography hydride generation.Microwave acid extraction was used to pretreat the sample,optimize the chromatographic conditions and carrier concentration,and then verify the method’s precision,detection limit,accuracy and standard recovery.The results showed that when the methanol content in the mobile phase was 5%and the l-cysteine content was 0.10%,the separation effect,the peak type and the instrument response value were good,and the Mercury memory effect was basically eliminated.The separation of inorganic mercury,methyl mercury and ethyl mercury was realized within 7 minutes.The linear relationship was good,r>0.9990,RSD%<10.00%.The quantitative limits(LOQ)were 0.023,0.032 and 0.038 mg/kg,respectively.The recovery rate was 82.50%~98.40%.The accuracy of the method was verified by two aquatic animal reference materials,BCR463 and TORT-3.The method is simple,effective,accurate and suitable for the determination of mercury species in aquatic animals and their products.It provides a new method for mercury speciation analysis.