摘要
建立了以微波消解和微波萃取实现对鱼肉组织快速高效前处理的方法,对萃取剂的组成及萃取条件进行了优化。使用原子荧光光谱和液相色谱-原子荧光联用仪分析鱼肉组织中总汞（Hg）、无机汞（Hg^2＋）和甲基汞（CH3Hg^＋）含量,并研究了流动相对分析测试效果的影响。经过优化实验,在以0.5%（V/V）2-巯基乙醇、5%（V/V）CH3OH和0.15%（m/V）KCl混合溶液作为萃取剂、萃取温度125℃、萃取时间15 min条件下对鱼肉中甲基汞萃取效率最高。流动相最佳组成为5%（V/V）HCl、5%（m/V）KBH4和0.15%（m/V）KCl溶液。分析结果表明,样品鱼肉中的汞形态可分为无机汞和甲基汞,但主要以甲基汞的形式存在。总汞与甲基汞重复测定结果 RSD〈5%。微波消解处理样品总汞的加标回收率达到94%~106%,微波萃取样品甲基汞的加标回收率达到90%~109%。
In this article,the rapid and effective methods for fish tissue pretreatment were established by microwave digestion and microwave extraction, and the composition of extraction solution and extraction conditions were optimized. Subsequently,the concentrations of total mercury（ Hg）,inorganic mercury（ Hg^2 ＋）and methylmercury（ CH3Hg^＋） were determined by using atomic fluorescence spectrometer and liquid chromatography-atomic fluorescence spectrometry,and the influence of mobile phase was investigated as well.According to the results,the optimum extraction efficiency was achieved under the condition that 0. 5%（ V/V）2-mercapoethanol,5%（ V/V） CH3 OH and 0. 15%（ m/V） KCl were used as extraction solution,extraction temperature was 120 ℃,and extraction time was 15 min. The mobile phase composed by 5%（ V/V） HCl,5%（ m/V） KBH4,and 0. 15%（ m/V） KCl reveals the best result. We can demonstrated from the results that the mercury in fish tissue existed as Hg^2 ＋and CH3Hg^＋,while mainly in the form of CH3Hg^＋. Precisions（ RSD）were all less than 5%. The recoveries of total Hg of microwave digested samples and CH3Hg^＋of microwave extracted samples were 94% ~ 106% and 90% ~ 109%,respectively.
出处
《分析试验室》
CAS
CSCD
北大核心
2015年第11期1259-1262,共4页
Chinese Journal of Analysis Laboratory
基金
国家科技支撑计划项目(2011BAD15B02)
863计划(2012AA021405)
省科技支撑计划项目(BE2010359)资助
关键词
原子荧光光谱
液相色谱-原子荧光联用仪
微波萃取
鱼肉
甲基汞
Atomic fluorescence spectrometry
Liquid chromatography-atomic fluorescence spectrometry
Microwave extraction
Fish tissues
Total mercury
Methylmercury
