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

Determination of total arsenic in sea fsh powder by ashing digestion-atomic fluorescent spectrometry after being soaked in magnesium nitrate/ethanol solution

  • 摘要:
    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0.00~10.00 μg/L;相关系数≥ 0.999 0;检出限为0.05 μg/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818 μg/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。

     

    Abstract:
    Objective To establish a method of ashing digestion-atomic fluorescent spectrometry (AFS) for determination of total arsenic in aquatic animal products after being soaked in magnesium nitrate/ethanol solution.

    Methods Samples were ashing digested after being soaked in magnesium nitrate/ethanol solution for a whole night. Then, the digestion solution was pre-reduced and determined by AFS. The result was verified using sea fish powder standard sample.

    Results In terms of the proposed method, the standard curve range was 0.00-10.00μg/L; the correlation coefficient was ≥ 0.9990; the detection limit was 0.05 μg/L. The recoveries of the method were 95.4%-100.4%, with relative standard deviation ≤ 4.83%. All six verified values of sea fish powder standard sample were within the permitted range of (780±80) μg/kg, with a mean value of 818 μg/kg and a relative standard deviation of 3.42%.

    Conclusion The method of ashing digestion-atomic fluorescent spectrometry after being soaked in magnesium nitrate/ethanol solution is safe, stable, and accurate for the determination of total arsenic in animal seafood.

     

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