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建立了微晶二苯甲酮富集分光光度法测定水中无机硒形态和食品中总硒的新方法。Se(Ⅳ)和3,3’-二氨基联苯胺(DAB)反应生成的苤硒脑络合物能被二苯甲酮微晶吸附富集,微晶用乙醇复溶后在430 nm处测定,试样经氢溴酸将Se(Ⅵ)还原成Se(Ⅳ)后可测定总硒并计算Se(Ⅵ)的含量。最佳实验条件下,方法的线性范围为1.0~120μg/L,r=0.9995,检出限0.18μg/L。水样中无机Se(Ⅳ)和Se(Ⅵ)的回收率在96.6%~99.0%之间,食品中总硒的回收率在97.0%~102.5%之间。
A new method for the determination of inorganic selenium in water and total selenium in food by microcrystalline benzophenone enrichment spectrophotometry was established. Selenium complex formed by the reaction of Se (Ⅳ) and 3,3’-diaminobenzidine (DAB) can be adsorbed and enriched by benzophenone microcrystal. The microcrystal was reconstituted with ethanol and determined at 430 nm The total selenium content was measured after the Se (Ⅵ) was reduced to Se (Ⅳ) by hydrobromic acid and the content of Se (Ⅵ) was calculated. Under the optimal experimental conditions, the linear range of the method was 1.0 ~ 120μg / L, r = 0.9995, the detection limit was 0.18μg / L. The recoveries of inorganic Se (Ⅳ) and Se (Ⅵ) in water samples ranged from 96.6% to 99.0%, and the total selenium recoveries in the samples ranged from 97.0% to 102.5%.