高效液相色谱原子荧光联用技术测定大米中无机砷
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0．02mol／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。...
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| Published in | 广东农业科学 Vol. 40; no. 12; pp. 117 - 121 |
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| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| Published |
中国农科院农业质量标准与检测技术研究所,北京,100081%农业部蔬菜水果质量监督检验测试中心,广东广州,510640
2013
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| Subjects | |
| Online Access | Get full text |
| ISSN | 1004-874X |
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| Summary: | 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0．02mol／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。 |
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| Bibliography: | 44-1267/S HPLC; atomic fluorescence spectrometry; rice; inorganic arsenic HUANG Ya-tao, MAO Xue-fei, YANG Hui, ZHANG Li-hua, CHEN Zhi-jun, QIAN Yong-zhong, WANG Fu-hua, WANG Min （1. Institute of Quality Standard Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081 China; 2. Supervision and Testing Center far Vegetables and Fruits Quality, Ministry of Agriculture, Guangzhou 510640, China） 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 0.02 mol/L HNO3 in a water bath at 95℃ for 60 min; 5 mmol/L malonate or 15 mm |
| ISSN: | 1004-874X |