文章摘要
黄亚涛,毛雪飞,杨慧,张立华,陈志军,钱永忠,王富华,王敏.高效液相色谱原子荧光联用技术测定大米中无机砷[J].广东农业科学,2013,40(12):117-121
高效液相色谱原子荧光联用技术测定大米中无机砷
Determination of inorganic arsenic in rice by atomic fluorescencespectrometry coupled with high performance liquid chromatography
  
DOI:
中文关键词: 高效液相色谱  原子荧光  大米  无机砷
英文关键词: HPLC  atomic fluorescence spectrometry  rice  inorganic arsenic
基金项目:国家重大科学仪器设备开发专项(2011YQ14014904);国家公益性行业(农业)科研专项(201303088)
作者单位
黄亚涛,毛雪飞,杨慧,张立华,陈志军,钱永忠,王富华,王敏 中国农科院农业质量标准与检测技术研究所农业部蔬菜水果质量监督检验测试中心 
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中文摘要:
      采用高效液相色谱-氢化物发生-原子荧光光谱法建立了大米中无机砷的检测方法,研究了大米研磨粒径、提取剂、提取温度、提取方式对大米中砷提取效率的影响,As(Ⅲ)转化为As(Ⅴ)的方法,并对流动相进行了对比和优化。结果表明:大米研磨 过孔径0.45mm筛,采用0.02 mol/L的硝酸甲醇水溶液(V:V=50:50)作为提取剂,95℃水浴60min,5mmol/L丙二酸或15mmol/L磷酸氢二铵水溶液为流动相,提取效率可达到85%以上,加标回收率为85%~110%,相对标准偏差(RSD)小于10%,无机砷的方法检出限(LOD)为8μg/kg。该方法可以应用于大米样品标准物质和市售大米中无机砷的检测。
英文摘要:
      An improved HPLC-HG-AFS method was developed for determination of inorganic arsenic in rice, in which the effects of particle size, extractants, temperature and extracting methods on the extraction efficiency for arsenic and different mobile phase materials for chromatography column were studied. The optimized conditions of sample pre-treatment and chromatography column were as follows:the rice sample was grinded and sieved by 0.45 mm-mesh, then extracted with the methanol/water solution (V:V=50:50) containing 0.02mol/L HNO3 in a water bath at 95℃for 60 min; 5 mmol/L malonate or 15 mmol/L (NH4)2HPO4 could be chosen as the liquid phase. The results showed that the extraction efficiency was more than 85%, and the recovery were 85% ~110% with the RSD<10%, and the LOD of the method was 8 滋g/kg. By the method of HPLC-HG-AFS, inorganic arsenic in rice certified reference materials and real rice samples from markets could be detected accurately.
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