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目的建立微波密闭H2O2鄄HNO3消解、分离测定植物样品中不同形态硒(Se)。方法以氢化物发生原子荧光光谱法直接测定水溶态的无机Se(IV),还原后测定Se(VI)。用XAD鄄2树脂消除可溶有机质对测定的干扰,以差减法获得可溶态硒、不溶态硒、无机Se(IV)和Se(VI)以及有机硒。结果氢化物发生原子荧光光谱法测定Se(IV)的线性范围为0～80μg/L,最低检出限0.05μg/L。微波消解、原子荧光法测定植物样品硒总量的RSD为1.7%(n=5)。标准参考物质的硒总量测定结果与标准值相吻合。结论微波消解法处理植物样品避免了硒的挥发损失;XAD鄄2树脂消除有机基体对荧光法直接测定植物样品中Se(Ⅳ)的干扰,扩大了该方法在形态分析中的应用;建立的硒形态系统分析流程可以分析植物样品中6种形态的Se,操作简便,方法实用。
Objective To establish a microwave-sealed H2O2-HNO3 digestion and separate the determination of different forms of selenium (Se) in plant samples. Methods Direct determination of water-soluble inorganic Se (IV) by hydride generation-atomic fluorescence spectrometry and Se (VI) reduction after reduction. XAD Juan 2 resin was used to eliminate the interfering effect of soluble organic matter on the determination. The soluble selenium, insoluble selenium, inorganic Se (IV) and Se (VI) and organic selenium were obtained by subtractive method. Results The linear range of Se (IV) was 0 ~ 80μg / L and the lowest limit of detection was 0.05μg / L when the hydride generation atomic fluorescence spectrometry was used. The RSD of total selenium in plant samples was 1.7% (n = 5) by microwave digestion and atomic fluorescence spectrometry. The standard reference material selenium total amount of determination results and the standard value match. Conclusion The microwave digestion method can avoid the loss of selenium. XAD-2 resin eliminates the interference of organic matrix on the direct determination of Se (Ⅳ) in plant samples by fluorescence spectrometry, and enlarges the application of this method in the morphological analysis. The morphological system analysis process can analyze six kinds of Se in plant samples, which is easy to operate and practical.