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    固相萃取-原子荧光光谱法测定大米中无机硒的含量

    Determination of Inorganic Selenium in Rice by Atomic Fluorescence Spectrometry with Solid Phase Extraction

    • 摘要: 建立了固相萃取-原子荧光光谱法测定大米中无机硒含量的方法。大米粉样品0.5 g用水20 mL提取,离心后上清液中加入5 g·L-1氢氧化钠溶液,调至pH 4~7,过滤即得提取液。将提取液上SAX强阴离子交换柱进行固相萃取,收集洗脱液10 mL以分离无机硒,再采用原子荧光光谱法测定大米中无机硒的含量。结果表明:无机硒的质量浓度在10 μg·L-1以内与其对应的荧光强度呈线性关系,检出限(3s)为2.52 μg·kg-1。按标准加入法进行回收试验,回收率为90.3%~98.2%,测定值的相对标准偏差(n=6)为9.9%~19%。

       

      Abstract: A method was established for determination of inorganic selenium in rice by atomic fluorescence spectrometry with solid phase extraction. The rice sample of 0.5 g was extracted with 20 mL of water. After centrifugation, 5 g·L-1 sodium hydroxide solution was added into the supernatant solution to adjust pH to 4-7. The extract obtained by filtration was passing through solid phase extraction with SAX strong anion exchange column, and the eluate of 10 mL was collected in order to separate inorganic selenium. Then the content of inorganic selenium in rice was determined by atomic fluorescence spectrometry. As shown by the results, linear relationship between values of mass concentration of inorganic selenium and its respective fluorescence intensity was kept within 10 μg·L-1, with detection limit (3s) of 2.52 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 90.3%-98.2%, with RSDs (n=6) of the determined values ranged from 9.9% to 19%.

       

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