摘要:
通过对比优化了全自动甲基汞仪器分析系统的参数设置,得到当吹扫气N2和载气Ar流速分别为344 mL·min-1和34 mL·min-1,GC柱分离温度在约40 ℃时,Hg0、MeHg和Hg2+乙基化(1%NaBEt4溶液)后分离效果和完成时间最佳;在0—100 pg的标准工作曲线范围内,乙基化试剂的最佳投加量为40 μL;对比分析了KOH/H2O溶液和KOH/ CH3OH溶液2种常用鱼样消解方法,结果表明都有较好的准确度和精密度. 利用优化的仪器条件和鱼样前处理方法分析了实际鱼样,得到了满意的分析结果.
Abstract:
It is possible to analyze MeHg rapidly and precisely with the development of automated methylmercury (MeHg) analytical system, in which the optimization of instrumental parameters and sample pretreatment procedure are the keys. In this study,we optimized instrumental analysis conditions to obtain the best results for the separation and run time of ethylated Hg0, MeHg, and Hg2+. The optimum condition is the following: the flow rates of purging gas nitrogen and carrier gas argon were 344 mL·min-1 and 34 mL·min-1,respectively. And the GC column temperature was about 40℃. For ethylation reagent (1% NaBEt4 solution), an optimum volume of 40 μL was selected when the content of MeHg ranged from 0 to 100 pg. Finally, this optimized method was used to analyze target chemicals in fish samples digested separately by KOH/H2O and KOH/CH3OH solutions. The results showed good accuracy and precision that meet the requirement for analysis of MeHg in fish.
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