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本文采用2,3-二氨基萘荧光法测定人尿(或鼠尿)中总硒含量。以往采用的HClO_4+H_2SO_4+Na_2MoO_4混合消化液消化尿样时,不能把正常及高硒地区尿中总硒全部转变成Se~(+4),特别是测定尿硒含量较高的样品,得出的结果明显偏低。本法改用HNO_3+HClO_4(+HCl)混合酸作消化液后,能全量地把尿中总硒转变成Se~(+4)。于尿样中加入不同量的TMSe~+-Se后,硒的回收率为95.9~103.4%。本法硒的最低检出量为2ng。人尿中硒含量在0.022~0.251μg/ml范围内时,测出结果的变异系数不超过5%。本方法适用于高硒尿中总硒含量的分析,结果稳定。
In this paper, 2,3-diaminonaphthalene fluorescence method for the determination of total urinary (or rat urine) selenium content. In the past, when using HClO_4 + H_2SO_4 + Na_2MoO_4 mixed digestive juice to digest urine samples, the total selenium in urine of normal and high selenium areas could not be converted into Se ~ (+4), especially for the samples with higher urinary selenium content, The result is obviously low. The law to use HNO_3 + HClO_4 (+ HCl) mixed acid for digestion, the total amount of urine to the total Se into Se ~ (+4). After adding different amount of TMSe ~ + -Se to urine samples, the recoveries of selenium were 95.9 ~ 103.4%. The minimum detectable amount of selenium in this method is 2ng. When the content of selenium in human urine is in the range of 0.022 ~ 0.251μg / ml, the coefficient of variation of the measured results does not exceed 5%. The method is suitable for the analysis of total selenium content in high-selenium urine, the result is stable.