目的:建立一种简便、高效、灵敏的硝酸-盐酸混合酸-石墨消解仪消解-氢化物发生原子荧光光谱法测定猪肝样品中(干粉)全硒含量.方法:使用HCl和HNO3 对猪肝样品(干粉)进行消解,采用原子荧光光度计测定猪肝中全硒含量.结果:硒工作曲线的线性范围是2～20 μg·L-1,相关系数为0.999 7;检出限和定量限分别是 0.029 μg·L-1 和 0.098 μg·L-1,不同浓度下的加标回收率在 91.2%～111.4%,日内精密度为 1.2%,日间精密度 2.1%.同时对石墨消解仪消解样品条件进行了单因素条件优化,最优化条件为消解还原溶剂4 mL HCl和1 mL HNO3,最佳料液比1/25(0.200 g/5 mL),消解温度采用离心管最大耐受温度120℃,消解时间 3 h.结论:本研究为猪肝中全硒含量的测定提供了一种简单、快捷、高效、环保的方法.
Determination of Total Selenium in Pork Liver Powder by HNO3-HCl Acid Mixture-Graphite Digester Digestion-Atomic Fluorescence Spectrometry
Objective:To establish a simple,efficient and sensitive graphite digester digestion-atomic fluorescence spectrometry method for the determination of total selenium in pork liver powder.Method:The pig liver samples(dry powder)were digested by HCl and HNO3,and the total selenium content in pig liver was determined by atomic fluorescence spectrophotometer.Result:The linear range of selenium working curve was 2～20 μg·L-1,and the correlation coefficient was 0.999 7.The limit of detection and limit of quantitation were 0.029 μg·L-1 and 0.098 μg·L-1,respectively.The spiked recoveries at different concentrations were 91.2％～111.4％.The intra-day precision was 1.2％,and the inter-day precision was 2.1％.At the same time,the sample digestion conditions of graphite digestion instrument were optimized by single factor.The optimum conditions were as follows:4 mL HCl and 1 mL HNO3 were used as digestion and reduction solvents,the optimum ratio of material to liquid was 1/25(0.200 g/5 mL),the maximum tolerance temperature of centrifuge tube was 120℃,and the digestion time was 3 h.Conclusion:This study provides a simple,fast,efficient and environmentally friendly method for the determination of total selenium content in pig liver.
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