Vaessen H A, van Ooik A, Zuydendorp J
Z Lebensm Unters Forsch. 1985 Sep;181(3):189-93. doi: 10.1007/BF02425575.
A method for the determination of selenium in food and biological materials has been developed. The method involves sample decomposition in a closed system at 150 degrees C with nitric acid, perchloric acid treatment of the digest, reduction of selenium to the tetravalent state with hydrochloric acid followed by Se-2,3-diaminonaphthalene (DAN) complex formation and extraction in a single-step operation. Performance characteristics of the method (accuracy and repeatability) were extensively tested for eleven reference materials and ten practice samples covering both a wide variety of matrices and a wide range of selenium content. Almost all results for reference materials were within the 95% confidence range of the certified value or the best estimate thereof. The coefficient of variation for all samples ranged from 2.3 to 10.1%, average value 4.7%. Average recovery for spiking experiments-levels 0.060, 0.075 and 0.150 micrograms/g was 102%; range 84-114%.
已开发出一种测定食品和生物材料中硒的方法。该方法包括在封闭系统中于150℃用硝酸进行样品分解，对消化液进行高氯酸处理，用盐酸将硒还原为四价态，随后在一步操作中形成硒 - 2,3 - 二氨基萘（DAN）配合物并进行萃取。针对11种标准物质和10个实际样品广泛测试了该方法的性能特征（准确度和重复性），这些样品涵盖了各种各样的基质和广泛的硒含量范围。几乎所有标准物质的结果都在认证值或其最佳估计值的95%置信范围内。所有样品的变异系数范围为2.3%至10.1%，平均值为4.7%。加标实验（水平为0.060、0.075和0.150微克/克）的平均回收率为102%；范围为84%至114%。
