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[目的]建立硝酸镁/乙醇溶液浸泡后灰化消解-原子荧光光谱法测定海鱼粉中总砷的检测方法。[方法]样品用硝酸镁/乙醇溶液浸泡过夜后,再进行灰化消解;消解液经过预还原,用原子荧光光度计测定,同时采用海鱼粉质控样品进行方法验证。[结果]砷标准曲线范围0.00~10.00μg/L;相关系数≥0.999 0;检出限为0.05μg/L;加标回收率95.4%~100.4%,相对标准偏差≤4.83%;本法6次测定海鱼粉质控样品结果均在指定值的容许范围内[指定值(780±80)μg/kg],均值为818μg/kg,相对标准偏差3.42%。[结论]用硝酸镁/乙醇溶液浸泡后灰化消解-原子荧光法测定海鱼粉中总砷,操作安全,稳定性好,准确度高,尤其适用于动物类海产品中总砷的测定。
[Objective] The research aimed to establish a method for determination of total arsenic in marine fish meal by ashing-digestion-atomic fluorescence spectrometry after soaking magnesium nitrate / ethanol solution. [Method] After the sample was soaked in magnesium nitrate / ethanol solution overnight, the sample was further digested and digested. The digestion solution was pre-reduced and determined by atomic fluorescence spectrophotometer. The method was also used to verify the quality of the sample. [Results] The range of arsenic standard curve was 0.00-10.00μg / L, the correlation coefficient was 0.9999, the detection limit was 0.05μg / L, the recoveries were in the range of 95.4% -100.4% and the relative standard deviations were less than 4.83% The results of the determination of the quality control samples of the fish meal were within the allowable range of the specified value [780 ± 80 μg / kg], with a mean of 818 μg / kg and a relative standard deviation of 3.42%. [Conclusion] Determination of total arsenic in marine fish meal by soaking with magnesium nitrate / ethanol solution after ashing digestion - atomic fluorescence method was safe, stable and accurate. It was especially suitable for the determination of total arsenic in animal products.