Determination of Selenium in Food by Hydride Generation-Atomic Fluorescence Spectroscopy Using Semi-Fusion Separation with Aiskaer Reagent
摘 要
建立了艾斯卡试剂半熔法分离-氢化物发生-原子荧光光谱法(HG-AFS)测定食物中硒含量的方法。称取艾斯卡试剂(质量比为3:1的氧化镁-碳酸钠的混合物)0.50 g和样品0.50 g于石英坩埚中,混匀,再覆盖1.25 g艾斯卡试剂,于750℃焙烧60 min;加入1滴0.1%(质量分数)苯酚红指示剂,再加入盐酸使溶液由红色变为黄色,于200℃加热至溶液体积为6 mL左右时,再加入6 mL盐酸,继续煮沸10 min,取下冷却,加入2 mL铁盐溶液,再用水定容至25 mL,采用HG-AFS测定食物中硒的含量。结果显示:硒的质量浓度在16.0 μg·L-1以内与其对应的响应值呈线性关系,检出限(3s)为6.0 ng·g-1;对3个国家标准物质(大米、紫菜、蒜粉)进行测定,测定值的相对标准偏差(RSD,n=12)为3.4%~5.2%。方法用于16种国家标准物质的分析,测定值与认定值的相对误差为-10%~17%。
Abstract
A method for determination of selenium in food by hydride generation-atomic fluorescence spectroscopy (HG-AFS) using semi-fusion separation with aiskaer reagent. Aiskaer reagent (a mixture of magnesium oxide and sodium carbonate at mass ratio of 3:1) of 0.50 g and sample of 0.50 g were mixed well in a quartz crucible and covered with aiskaer reagent of 1.25 g to calcinate at 750℃ for 60 min. 1 drop of 0.1% (mass fraction) phenol red indicator was added, and the color of the solution was changed from red to yellow with hydrochloric acid. The solution was heated to about 6 mL at 200℃, and hydrochloric acid of 6 mL was added to boil for 10 min. Ferric salt solution of 2 mL was added after cooling, and the solution was made its volume up to 25 mL by water. Selenium content in food was determined by HG-AFS. As shown by the results, linear relationship between mass concentration of selenium and its response value was kept within 16.0 μg·L-1, with detection limit (3s) of 6.0 ng·g-1. 3 national reference materials (rice, laver and garlic powder) were determined, and RSDs (n=12) of the determined values were in the range of 3.4%-5.2%. This method has been applied for analysis of 16 national reference materials, and the relative errors between the measured values and the certified values were ranged from -10% to 17%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx202201016
所属栏目 工作简报
基金项目 国家重点研发计划项目(2016YFC0600601);地质调查项目(DD20190522);物化探所中央级公益性科研院所基本科研业务费专项(AS2020J05,AS2020J08)
收稿日期 2020/10/28
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备注马娜,工程师,硕士,主要从事地球化学样品配套分析方法研究
引用该论文: MA Na,ZHANG Linghuo,GU Xue,SUN Binbin,BAI Jinfeng,CHEN Haijie. Determination of Selenium in Food by Hydride Generation-Atomic Fluorescence Spectroscopy Using Semi-Fusion Separation with Aiskaer Reagent[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(1): 95~98
马娜,张灵火,顾雪,孙彬彬,白金峰,陈海杰. 艾斯卡试剂半熔法分离-氢化物发生-原子荧光光谱法测定食物中硒的含量[J]. 理化检验-化学分册, 2022, 58(1): 95~98
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【6】孟君,董梦娜,张峻松,等.富硒豆芽培育条件研究[J].食品研究与开发, 2019,40(22):57-61.
【7】史潜玉,刘立,林杰,等.微波消解-ICP-MS法测定富硒大米中5种元素的含量[J].食品研究与开发, 2016,37(10):144-146.
【8】刘金巍,刘雪松,边超,等.甲烷动态反应电感耦合等离子体质谱法测定地下水中痕量硒[J].岩矿测试, 2019,38(1):85-91.
【9】贺攀红,杨珍,荣耀,等.氢化物发生-电感耦合等离子体发射光谱法测定铀矿地质样品中痕量硒[J].岩矿测试, 2016,35(2):139-144.
【10】吕莉,李源,井美娇,等.氢化物发生-原子荧光光谱法测定三种鸡蛋中硒含量的研究[J].光谱学与光谱分析, 2019,39(2):607-611.
【11】刘冰冰,韩梅,贾娜,等.控温消解-氢化物发生-原子荧光光谱法测定水中硒形态[J].理化检验-化学分册, 2019,55(6):644-649.
【12】屈明华,汤富彬,倪张林,等.原子荧光光谱法测定食品硒的前处理方法研究[J].分析科学学报, 2015,31(3):435-438.
【13】章剑扬,张琳,黄聪薇,等.微波消解-ICP-MS测定桐乡杭白菊中硒含量[J].食品工业, 2020,41(1):321-323.
【14】刘亚轩,李晓静,白金峰,等.植物样品中无机元素分析的样品前处理方法和测定技术[J].岩矿测试, 2013,32(5):681-693.
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