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中全硒含量  

Determination of Total Selenium in Pork Liver Powder by HNO3-HCl Acid Mixture-Graphite Digester Digestion-Atomic Fluorescence Spectrometry

作　　者：刘倩 夏淼 杨晓灵 LIU Qian;XIA Miao;YANG Xiaoing(Changzhou Center for Disease Control and Prevention,Changzhou 213001,China)

机构地区：[1]常州市疾病预防控制中心,江苏常州213001

出　　处：《食品安全导刊》2024年第3期92-95,共4页China Food Safety Magazine

基　　金：常州市科技项目:应用基础研究计划(中补助)(CJ20220067);常州市卫生健康青苗人才(CZQM2023027)。

摘　　要：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HNO+3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2~20μg·L^(-1),相关系数为0.999 7;检出限和定量限分别是0.029μg·L^(-1)和0.098μg·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 HNO+3,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。Objective:To establish a simple,efficient and sensitive graphite digester digestion-atomic f luorescence 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 f luorescence spectrophotometer.Result:The linear range of selenium working curve was 2~20μg·L^(-1),and the correlation coefficient was 0.9997.The limit of detection and limit of quantitation were 0.029μg·L^(-1) and 0.098μg·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.

关 键 词：石墨消解仪消解 氢化物发生原子荧光光谱法 猪肝粉 全硒 

分 类 号：O657.31[理学—分析化学] TS251.9[理学—化学]