程序控温石墨消解/微波灰化-氢化物发生-原子荧光光谱法测定食用海藻中总砷
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(北京市疾病预防控制中心,北京 100013)

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张妮娜 女 主管检验师 研究方向为元素的光谱和质谱分析 E-mail:znnms@sina.com通讯作者:┣┣(中)通信作者┫┫刘丽萍 女 主任技师 研究方向为光谱和质谱分析 E-mail:liulp@bjcdc.org

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Determination of total arsenic in alga by hydride generation-atomic flourence spectrometry with program temperature graphite digestion/microwave ashing for sample preparation
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(Beijing Center for Disease Control and Prevention,Beijing 100013,China)

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    摘要:

    建立采用程序控温石墨消解/微波灰化-氢化物发生-原子荧光光谱法分析测定食用海藻中总砷的方法。方法 样品加入5 ml HNO3,190 ℃程序控温石墨预消解30 min;加入灰化辅助剂硝酸镁,550 ℃微波灰化5 min,用HCl溶解灰分,采用氢化物发生-原子荧光光谱法(HG-AFS)测定总砷含量。结果 方法检出限为0.42 μg/L,RSD<5.0%,加标回收率为96%~109%。测定程序控温石墨消解/微波灰化后消解液中砷形态,确认食用海藻中99%以上的有机砷均消解为无机砷。本方法测定了海带(GBW08517)和紫菜(GBW10023)标准物质,分析结果均在标准值范围内。结论 本方法重现性好、结果准确可靠,适用于食用海藻中总砷的测定。

    Abstract:

    A hydride generation-atomic flourence spectrometry (HG-AFS) method with program temperature graphite digestion/microwave ashing for sample preparation was developed for the determination of total arsenic in alga.Methods The alga, into which 5 ml HNO3 was added, was heated at 190 ℃ for 30 min with program temperature graphite digestion, then ashed at 550 ℃ for 5 min with microwave using magnesium nitrate as ashing auxiliary agent. The ashes were dissolved with hydrochloric acid and total arsenic was determined by HG-AFS. Results The detection limit was 0.42 μg/L, and the RSD was less than 5%. The recoveries were between 96% and 109%. The arsenic forms were detected in digested alga by program temperature graphite digestion/microwave ashing, the results confirmed that more than 99% of organic arsenic in alga had been digested into inorganic arsenic. The method was applied to determine the total arsenic in two certified reference materials of Laminaria japonica (GBW08517) and laver(GBW10023), and the analysis results were all in the reference range. Conclusion The method had good accuracy and precision, and was suitable for the determination of total arsenic in alga.

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张妮娜,刘丽萍,陈绍占.程序控温石墨消解/微波灰化-氢化物发生-原子荧光光谱法测定食用海藻中总砷[J].中国食品卫生杂志,2015,27(6):629-633.

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  • 收稿日期:2015-03-30
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  • 在线发布日期: 2015-12-14
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