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建立了高分辨-连续光源石墨炉原子吸收光谱法(HR-CS GFAAS)测定富硒大蒜中不同形态硒含量的方法,研究富硒有机肥对大蒜中硒元素及其形态的影响。通过单因素试验优化得出硒元素最佳测定条件,即最佳基体改进剂为Pd(NO_3)_2(1 g/L)和Mg(NO_3)_2(0.5 g/L)混合溶液,且最佳添加体积为5μL。参照标准DBS 42/002—2014制备出富硒大蒜总硒和无机硒测定试样,再使用HR-CS GFAAS法测定总硒含量为8.933~9.476μg/g,无机硒含量为5.784~6.021μg/g,计算出有机硒含量为3.124~3.491μg/g,所占百分比为34.16%~36.84%,这说明富硒有机肥能有效提高大蒜中总硒和有机硒的含量。该方法的精密度为3.0%~5.2%,总硒和无机硒的加标回收率分别为96.3%和93.7%,这表明参照DBS 42/002—2014分析富硒大蒜中硒元素含量及其形态,结果准确可靠,添加的标样(无机硒)几乎全部在待测无机硒试样中。该方法快速、准确且稳定,具有较高的实用价值,为分析食品中微量元素含量及其形态提供科学依据。
A method for the determination of selenium in Se-enriched garlic by high resolution and continuous light source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) was established. The effects of selenium enriched organic fertilizer on selenium and its speciation in garlic were studied. The optimum conditions for the determination of selenium were obtained by single factor experiments, that is, the best matrix modifier was Pd (NO_3) _2 (1 g / L) and Mg (NO_3) _2 Add volume 5μL. According to the standard DBS 42 / 002-2014, the total selenium and inorganic selenium of the selenium-enriched garlic were determined. The total selenium content was 8.933 ~ 9.476μg / g and the inorganic selenium content was 5.784 ~ 6.021μg / g by HR-CS GFAAS method. g, calculated the organic selenium content of 3.124 ~ 3.491μg / g, the percentage of 34.16% ~ 36.84%, indicating that Se-enriched organic fertilizer can effectively improve the garlic in total selenium and organic selenium content. The precision of this method was 3.0% -5.2%, and the spiked recoveries of total selenium and inorganic selenium were 96.3% and 93.7%, respectively. This indicated that the content of selenium in Se-enriched garlic and its speciation with reference to DBS 42 / 002-2014 , The results are accurate and reliable, adding the standard (inorganic selenium) almost all in the test inorganic inorganic selenium samples. The method is rapid, accurate and stable, has high practical value, and provides a scientific basis for the analysis of trace elements in food and its morphology.