摘要
为了探索悬浮进样-氢化物发生原子荧光法直接测定总Se、无机Se和Se(Ⅵ)的新方法。样品中的总硒以5mL浓盐酸提取,用悬浮进样-氢化物发生原子荧光法加以测定;以环己烷萃取分离无机硒和有机硒,水相中的无机硒在浓盐酸量为20%(V/V)的介质中以悬浮进样-氢化物发生原子荧光法加以测定,而水相中的Se(Ⅵ)在5g/L亚硫酸钠溶液中以同样的方法加以测定。利用差减法求得有机硒和Se(Ⅳ)的含量。结果表明,硒的检出限(RSN=3)为0.10μg/L,回收率为90.7%～107%,相对标准偏差(RSD,n=5)为0.7%～1.9%。本方法具有准确、操作简易、快速、灵敏度高等优点,可用于小麦面粉、大米面粉和富硒盐中总硒、无机硒和Se(Ⅵ)的测定。
A new method was developed for directly determining total Se, inorganic Se and Se（Ⅵ） using slurry sampling-hydride generation atomic fluorescence spectrometry （SS-HGAFS）. For total Se determination, samples were extracted with 5 mL of concentrated HCl, followed by SS-HGAFS analysis. Cyclohexane extraction was used for the separation between inorganic Se and organic Se, and total inorganic Se and Se（Ⅵ） dragged into the water phase were determined by SS-HGAFS in concentrated HCl medium in the absence and presence of 5 g/L Na2SO3, respectively. Organic Se could be calculated by the difference between total Se and inorganic Se, and Se（Ⅳ） by difference of the inorganic Se and the Se（Ⅵ）. The method detection limit （RSN = 3） was 0.10 μg/L for Se. Mean spike recoveries for total Se, total inorganic Se and Se（Ⅵ） in real samples of wheat flour, rice flour and Se rich salt were between 90.7% and 107%, with a relative standard deviation （RSD） ranging from 0.7% to 1.9%. The proposed method has the characteristics of accuracy, easy operation, rapidity and high sensitivity, and is most suitable for the speciation analysis of selenium in real samples.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2010年第16期225-228,共4页
Food Science
关键词
悬浮进样
氢化物发生
原子荧光
硒
形态分析
面粉
富硒盐
slurry sampling
hydride generation
atomic fluorescence spectrometry
selenium
speciation
flour
selenium rich salt
作者简介
孙汉文（1945-），男，教授，研究方向为光谱学与痕量分析。E—mail：hanwen@hbu．edu．cn
