HPLC-AFS法测定水产品中4种砷形态
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(1. 中南林业科技大学食品科学与工程学院,湖南 长沙 410004;2. 长沙海关技术中心,湖南 长沙 410004)

作者简介:

刘正华,男,长沙海关技术中心高级工程师,博士。

通讯作者:

李忠海(1960—),男,中南林业科技大学教授,博士。E-mail:lizh11@163.com

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国家质量监督检验检疫总局科技计划项目(编号:2015IK126)


Determination of four arsenic species in aquatic products by liquid chromatography-atomic fluorescence spectrometry
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(1. College of Food Science and Engineering, Central South University of Forestry and Technology, Changsha, Hunan 410004, China; 2. Technology Center of Changsha Customs District of People's Republic of China, Changsha, Hunan 410004, China)

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    摘要:

    目的:研究建立水产品中一甲基砷酸(MMA)、二甲基砷酸(DMA)、As(Ⅲ)和As(Ⅴ)的超声辅助提取—高效液相色谱—原子荧光光谱分析方法。方法:样品采用甲醇—水(V甲醇V=1∶1)溶液超声提取,15 mmol/L磷酸氢二铵溶液(pH 6.0)为流动相,经PRP-X100阴离子交换柱分离,原子荧光光谱分析方法测定。结果:在优化试验条件下,MMA、DMA、As(Ⅲ)、As(Ⅴ)4种砷形态化合物在0~100 μg/mL的质量浓度范围内线性关系良好,相关系数均在0.998以上,检出限分别为0.82,0.94,1.10,0.78 μg/L,相对标准偏差为0.8%~3.7%,加标回收率为86.0%~110.0%。结论:该方法简便,准确度、灵敏度高且试剂耗材费用低,适用于水产品中砷的形态分析。

    Abstract:

    Objective: Four arsenic species of arsenic in aquatic products were analyzed using ultrasonic-assisted extraction combined with high performance liquid chromatography-atomic fluorescence spectrometry (HPLC-AFS). Methods: Four arsenic compounds were extracted ultrasonically from the samples using 50%(v/v) methanol-aqueous solution as extraction solvent. The chromatographic separation was performed on Hamilton PRP-X100 anion exchange column using a mixture of 15 mmol/L ammonium dihydrogen phosphate solution with the pH adjust to 6.0 as the mobile phase. Results: Under the optimized conditions, there were good linear relationships in the range of 0~100 μg/L for four arsenic compounds, with correlation coefficients all above 0.998. The limit of detection (LODs) of four arsenic species MMA, DMA,As(Ⅲ),As(Ⅴ)were 0.82, 0.94, 1.10, 0.78 μg/L respectively. The relative standard deviations were in the range of 0.8%~3.7%. The recoveries ranged from 86.0% to 110.0%. Conclusion: This method is simple, accurate, sensitive, and low reagent consumption costs, can be used for the determination of the arsenic species in aquatic products.

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刘正华,李忠海. HPLC-AFS法测定水产品中4种砷形态[J].食品与机械,2023,39(8):66-70.
LIU Zhenghua, LI Zhonghai. Determination of four arsenic species in aquatic products by liquid chromatography-atomic fluorescence spectrometry[J]. Food & Machinery,2023,39(8):66-70.

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  • 收稿日期:2023-03-10
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  • 在线发布日期: 2023-10-20
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