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目的建立甲苯萃取-原子荧光光谱检测鱼肉中甲基汞的方法。方法样品经48%氢溴酸水解、甲苯萃取、0.05 mol/L硫代硫酸钠反萃取后,应用AFS-9230原子荧光光谱法进行测定,同时经此前处理后的样品采用DMA-80直接测汞仪进行测定,与原子荧光光谱法的结果进行对比。结果原子荧光光谱法以及直接测汞仪直接测定的结果与标准物质定值吻合,确证该方法的可靠性,适用于鱼、贝等水产品中甲基汞的测定。采用该方法对鱼肉中总汞与甲基汞成分分析标准物质GBW10029以及英国食品分析水平评估计划(food analysis performance assessment scheme,FAPAS)的罐装鱼肉样品(样品编号07189)进行了检测,检测结果与参考物定值吻合,回收率分别为96.1%,97.5%。结论该方法操作简单,灵敏度高,重现性好,适用于鱼肉中甲基汞含量的定量检测。
Objective To establish a method for the determination of methylmercury in fish by toluene extraction - atomic fluorescence spectrometry. Methods The sample was hydrolyzed with 48% hydrobromic acid, extracted with toluene and stripped with 0.05 mol / L sodium thiosulfate. The sample was analyzed by AFS-9230 atomic fluorescence spectrometry. The sample was treated with DMA-80 for mercury Instrument was measured, and atomic fluorescence spectrometry results were compared. Results The results of atomic fluorescence spectrometry and direct mercury analyzer were in good agreement with those of reference materials. The reliability of this method was confirmed and it was suitable for the determination of methylmercury in fish, shellfish and other aquatic products. This method was used to test the canned fish samples (sample number 07189), which is the standard substance for the analysis of total mercury and methylmercury in fishmeal, GBW10029, and the food analysis performance assessment scheme (FAPAS) Reference value consistent, the recovery rates were 96.1%, 97.5%. Conclusion The method is simple, sensitive and reproducible. It is suitable for the quantitative determination of methylmercury in fish.