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  

Determination of Selenium in Food by Hydride Generation-Atomic Fluorescence Spectroscopy Using Semi-Fusion Separation with Aiskaer Reagent

作　　者：马娜[1] 张灵火 顾雪 孙彬彬[1] 白金峰[1] 陈海杰[1] MA Na;ZHANG Linghuo;GU Xue;SUN Binbin;BAI Jinfeng;CHEN Haijie(Key Laboratory of Geochemical Exploration,Ministry of Natural Resources,Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang065000,China)

机构地区：[1]中国地质科学院地球物理地球化学勘查研究所自然资源部地球化学探测重点实验室,廊坊065000

出　　处：《理化检验（化学分册）》2022年第1期95-98,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：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)。

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)0.50g和样品0.50g于石英坩埚中,混匀,再覆盖1.25g艾斯卡试剂,于750℃焙烧60min;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6mL左右时,再加入6mL盐酸,继续煮沸10min,取下冷却,加入2mL铁盐溶液,再用水定容至25mL,采用HGAFS测定食物中硒的含量。结果显示:硒的质量浓度在16.0μg·L^(-1)以内与其对应的响应值呈线性关系,检出限(3s)为6.0ng·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%。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 0.50g and sample of 0.50g were mixed well in a quartz crucible and covered with aiskaer reagent of 1.25g to calcinate at 750℃for 60min.1drop 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 6mL at 200℃,and hydrochloric acid of 6mL was added to boil for 10min.Ferric salt solution of 2mL was added after cooling,and the solution was made its volume up to 25mL 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 16.0μg·L^(-1),with detection limit(3s)of 6.0ng·g^(-1).3national 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%.

关 键 词：艾斯卡试剂 氢化物发生-原子荧光光谱法 硒 

分 类 号：O657.31[理学—分析化学]