湿法消解-氢化物发生原子荧光光谱法测定动物性农产品中硒含量

Determination of selenium content in animal agricultural products by hydride generation atomic fluorescence spectrometry with wet digestion

目的通过对消解条件、预还原方式、铁氰化钾屏蔽效果、硼氢化钾浓度、氢化反应酸度等反应条件的比较分析,建立湿法消解-氢化物发生原子荧光光谱法测定肉蛋奶等动物性农产品中硒含量的分析方法。方法牛奶、鸡蛋、猪肉、鱼肉样品经混合酸消解后,加入6 mol/L的盐酸溶液低温预还原,于氢化物原子荧光光谱仪上进行检测。结果方法检出限为0.01μg/kg,线性相关系数为1.0000,样品加标回收率为96.5%~104.6%,相对标准偏差(relative standard deviation,RSD)小于4%。结论本方法具有良好的灵敏度、精密度和准确度,可操作性强,可实现快速准确的测定动物性农产品中硒含量。

Objective To establish a wet digestion hydride generation atomic fluorescence spectrometry(HG-AFS)method for the determination of selenium content in meat,eggs,milk and other animal agricultural products by comparing and analyzing the digestion conditions,pre reduction methods,shielding effect of potassium ferricyanide,concentration of potassium borohydride and acidity of hydrogenation reaction.Methods The samples of milk,egg,pork and fish were digested with mixed acid,pre reduced at low temperature in 6 mol/L hydrochloric acid solution,and detected by hydride generation atomic fluorescence spectrometry.Results The limit of detection was 0.01μg/kg,the linear correlation coefficient was 1.0000,and the recoveries were 96.5%-104.6%.The relative standard deviation(RSD)was less than 4%.Conclusion The method has good sensitivity,precision and accuracy and strong operability,and can realize rapid and accurate determination of selenium content in animal agricultural products.