[1]凌云,万夕和,张朝晖,等.微波加湿法分段消解-原子荧光法测定贝藻产品中总砷含量[J].江苏农业学报,2017,(03):695-700.[doi:doi:10.3969/j.issn.1000-4440.2017.03.031]
　LING Yun,WAN Xi-he,ZHANG Zhao-hui,et al.Determination of total arsenic content in shellfish and algae products by microwave and wet digestion-hydride generation atomic fluorescence spectrometry[J].,2017,(03):695-700.[doi:doi:10.3969/j.issn.1000-4440.2017.03.031]
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微波加湿法分段消解-原子荧光法测定贝藻产品中总砷含量()
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江苏农业学报[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2017年03期
页码:
695-700
栏目:
加工贮藏·质量安全
出版日期:
2017-06-30

文章信息/Info

Title:
Determination of total arsenic content in shellfish and algae products by microwave and wet digestion-hydride generation atomic fluorescence spectrometry
作者:
凌云1;2; 万夕和1; 张朝晖3; 史文军1; 黎慧1; 王李宝1; 沈辉1; 乔毅1; 陆勤勤1
（1.江苏省海洋水产研究所，江苏南通226007；2.浙江经贸职业技术学院应用工程系，浙江杭州310018；3.江苏省渔业技术推广中心，江苏南京210036）
Author(s):
LING Yun1;2; WAN Xi-he1; ZHANG Zhao-hui3; SHI Wen-jun1; LI Hui1; WANG Li-bao1; SHEN Hui1; QIAO Yi1; LU Qin-qin1
(1.Institute of Oceanology & Marine Fisheries, Jiangsu Province, Nantong 226007, China;2.Practical Engineering Department of Zhejiang Institute of Economics and Trade, Hangzhou 310018, China;3.Fisheries Technology Extension Center of Jiangsu Province, Nanjing 210036, China)
关键词:
微波消解; 湿法消解; 砷; 贝藻产品; 原子荧光光谱法
Keywords:
microwave digestion; wet digestion; arsenic; shellfish and algae; atomic fluorescence spectrometry
分类号:
X836
DOI:
doi:10.3969/j.issn.1000-4440.2017.03.031
文献标志码:
A
摘要:
建立了微波加湿法分段消解作为前处理,并通过氢化物发生原子荧光法测定贝藻产品中总砷含量的方法。研究了微波消解加酸体系和程序、湿法消解中高氯酸和硫酸用量对砷含量测定的影响，并通过添加质量控制标准样品计算回收率，检测了该方法的准确性。结果表明：用5 ml硝酸进行微波消解后再加1 ml高氯酸、2～3 ml硫酸进行湿法分段消解使样品溶液成无色的样品前处理方法，具有消解效率高、操作过程可控、反应终点判断准确、试剂消耗少、环境污染少、检测数据准确稳定等优点。通过检测样品添加同类质量控制标准样品测得的砷回收率在90%以上，满足贝藻产品中总砷含量测定要求。
Abstract:
A digestion method which consists of microwave digestion and wet digestion for subsection by using hydride generation atomic fluorescence spectrometry was established to determine the total arsenic content in the shellfish and algae products. The effects of different acid systems and digestion processs in microwave digestion and different contents of perchloric acid and sulfuric acid in wet digestion were studied. The sample prepared by microwave digestion with 5 ml nitric acid and wet digestion with 1 ml perchloric acid and 2-3 ml sulfuric acid were digest to colorless solution. The pretreatment showed such advantages as high digestion efficiency, controllable operation process, well-judged reaction end point, less reagent consumption, environment friendly, and accurate and stable test data. The spiked recovery rate of arsenic was over 90%, which satisfied the requirement of total arsenic determination in shellfish and algae products.

参考文献/References:

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备注/Memo

备注/Memo:
收稿日期：2016-09-12 基金项目：江苏省农业自主创新基金项目[CX(13)3039]；江苏省大型仪器平台新方法开发项目（BZ201304）；国家海洋公益性行业科研专项(201105023、2013418007-1） 作者简介：凌云（1982-），女，江苏南通人，硕士，高级工程师，主要从事海洋环境监测、水产品质量研究。(Tel)15962909639;( E-mail)lingyun20110520@163.com 通讯作者：万夕和，(Tel)13814608515；(E-mail)wxh1708@163.com
更新日期/Last Update: 2017-06-29