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• 分析检测 •    下一篇

HPLC-HG-AFS测定蜂花粉中的4种砷形态

吴黎明1,王素芬2   

  1. 1. 中国农业科学院蜜蜂研究所
    2. 福建农林大学
  • 收稿日期:2012-03-20 修回日期:2013-04-28 出版日期:2013-06-25 发布日期:2013-06-17
  • 通讯作者: 吴黎明 E-mail:apiswu@126.com
  • 基金资助:
    国家蜂产业技术体系专项经费资助

Determination of Four Arsenic Species Present in Bee Pollen by High Performance Liquid Chromatography-Hydride Generation-Atomic Fluorescence Spectrum

Wu Liming1,Su-fen WANG   

  • Received:2012-03-20 Revised:2013-04-28 Online:2013-06-25 Published:2013-06-17
  • Contact: Wu Liming E-mail:apiswu@126.com

摘要: 建立了高效液相色谱-氢化物发生-原子荧光光谱(HPLC-HG-AFS)联用技术分析蜂花粉中亚砷酸(AsⅢ)、砷酸(AsV)、一甲基砷酸(MMA)和二甲基砷酸(DMA)的方法。以0.20 mol/L硫酸做提取溶剂,经超声、离心提取,用0.22 μm滤膜过滤后,经高效液相色谱-氢化物发生-原子荧光仪分离测定。结果表明:AsⅢ、DMA、MMA和AsV的检测限分别是1.0、2.1、1.2、3.1 μg/kg,加标回收率均在79%~100%之间,精密度试验结果(n=4)显示四种砷形态的相对标准偏差分别为4.5%、2.3%、11.0%、7.7%。该方法快速准确,灵敏度高,是一种较好的定性和定量分析蜂花粉中不同形态砷的方法。

关键词: 蜂花粉, 砷形态, 高效液相色谱-氢化物发生-原子荧光仪

Abstract: To establish a high performance liquid chromatography- hydride generation-atomic fluorescence spectrum(HPLC-HG-AFS) method for the determination of arsenite(AsIII), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and arsenate(AsV) in bee pollen. Sample preparation was achieved by extraction with 0.20 mol/L sulfuric acid with ultrasonic processing, centrifugation, and filtering by 0.22μm filter membrane. Results: The detection limits for As (Ⅲ), DMA, MMA and As (Ⅴ) were 1.0、2.1、1.2、3.1μg/kg, respectively, and the spiked recoveries were in the range of 79%~100% with that the relative standard deviations (RSDs) were 4.5%、2.3%、11.0%、7.7%, respectively. It is a good and fast qualitative and quantitative analysis method for arsenic compounds in bee pollen, with high sensitivity and good accuracy.

Key words: Bee pollen, Arsenic speciation, HPLC-HG-AFS

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