食品科学 ›› 2012, Vol. 33 ›› Issue (4): 234-237.doi: 10.7506/spkx1002-6630-201204050

• 分析检测 • 上一篇    下一篇

高效液相色谱-原子荧光法测定水产品中甲基汞含量

陈雪昌,梅光明,张小军,朱敬萍,郭远明,顾 捷,郑 斌   

  1. 1.浙江省海洋水产研究所 2.浙江省海水增养殖重点实验室 3.浙江省海洋开发研究院
  • 出版日期:2012-02-25 发布日期:2012-02-14
  • 基金资助:
    2009 年农业部行业标准制定项目

Determination of Methylmercury in Aquatic Products by HPLC-AFS

CHEN Xue-chang,MEI Guang-ming,ZHANG Xiao-jun,ZHU Jing-ping, GUO Yuan-ming,GU Jie,ZHENG Bin   

  1. 1. Marine Fisheries Research Institute of Zhejiang, Zhoushan 316100, China;2. Key Laboratory of Mariculture and Enhancement of Zhejiang Province, Zhoushan 316100, China;3. Zhejiang Marine Develepment Research Inisitite, Zhoushan 316100, China
  • Online:2012-02-25 Published:2012-02-14

摘要: 建立水产品中甲基汞含量的高效液相色谱-原子荧光测定方法。样品经硫脲加氯化钾、盐酸溶液提取,提取液过固相萃取小柱净化,用流动相定容,过0.45μm微孔滤膜,采用高效液相色谱-原子荧光法检测,外标法定量。结果表明,甲基汞在2~50μg/L质量浓度范围内,色谱峰面积与甲基汞质量浓度之间线性关系良好(相关系数为0.9995),以20、200、1000μg/kg 三个添加量在空白样品中添加甲基汞,样品平均回收率为80.2%~87.1%,相对标准偏差为3.4%~6.8%,方法的定量限为20μg/kg。该方法简便快速,基体干扰小,精密度、准确性均能满足水产品中甲基汞分析。

关键词: 甲基汞, 水产品, 高效液相色谱-原子荧光法

Abstract: A high performance liquid chromatography-atomic fluorescence spectrometry (HPLC-AFS) method was developed for the determination of methylmercury in aquatic products. Samples were extracted with a mixture of vitriol, potassium chloride and hydrochloric acid. Then the extract was cleaned up on an SPE column, diluted with the HPLC mobile phase and filtrated through a 0.45 μm pore size membrane prior to HPLC-AFS analysis. The quantification of methylmercury was carried out using the external standard method. Good linearity between chromatographic peak area and methylmercury concentration ranging from 2 to 50μg/L was found (R2=0.9995). Average recoveries for methylmercury in different blank aquatic products spiked at 20, 200 ,1000μg/kg were 80.2%-87.1% with relative standard deviations (RSD) between 3.4% and 6.8%. The method exhibited a detection limit of 20μg/kg. The method had the advantages of simplicity and little matrix interference, and meanwhile its precision and accuracy could meet the requirements for the analysis of methylmercury in aquatic products.

Key words: methylmercury, aquatic product, HPLC-AFS

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