高压密闭消解-ICP-AES法在农产品分析8种元素中的应用

Application of High Pressure Closed Digestion-ICP-AES in the Analysis of 8 Elements in Agricultural Products

为了达到快速、准确的测定大批量农业产品中多种元素含量的目的,建立了基于密闭消解前处理方式结合电感耦合等离子体发射光谱法同时测定农产品中K、Na、Ca、Mg、Fe、Al、S、P元素的方法。通过谱线干扰试验,确定了S、P的最佳分析谱线,极大地提高了分析的准确性。并对消解酸试剂、消解温度、消解时间等实验条件进行探讨,建立了最优密闭消解条件。考察了方法的标准曲线线性关系、检出限、准确度和精密度,结果表明:在最优的实验条件下,在一定的浓度范围内所分析的8种元素具有良好的线性关系,线性相关系数R^(2)达到0.999以上。选择农产品国家标准物质GBW10010(大米)、GBW10011(小麦)、GBW10014(圆白菜)、GBW10015(菠菜)进行方法验证,方法检出限范围为0.007~0.11μg/g,相对误差RE为-2.91%~1.87%,相对标准偏差RSD为0.15%~4.40%。采用本实验方法进行实际农产品的加标回收实验,回收率为91%~109%。实验方法能够实现同时大批量、快速、准确的测定农产品中8元素的含量。

To quickly and accurately determine the contents of various elements in bulk agricultural products,the closed digestion pretreatment method was used for the simultaneous determination of K,Na,Ca,Mg,Fe,Al,S,and P in agricultural products by inductively coupled plasma emission spectrometry.Through the spectral line interference test,the best analysis spectral lines of S and P were determined,and the accuracy of the analysis was greatly improved.The optimum airtight digestion conditions were determined through the discussion of the digestion acid reagent,digestion temperature,and digestion time.The linear relation of the standard curve,detection limit,accuracy,and precision was also investigated.The linear correlation coefficient R^(2)of the 8 elements in a certain concentration range was higher than 0.999.The national standards for agricultural products GBW10010(Rice),GBW10011(wheat),GBW10014(cabbage),and GBW10015(spinach)were selected to validate the method.The detection limit was 0.007~0.11μg/g,the relative error RE was-2.91%~1.87%,and the relative standard deviation RSD was 0.15%~4.40%.The experimental method was used to conduct the actual recovery of agricultural products,and the recovery rate was 91%~109%.This method achieves simultaneous large-scale,rapid,and accurate determination of the contents of 8 elements in agricultural products.