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采用氢化物发生原子荧光光谱法定量分析大米中无机砷的形态。

SPE speciation of inorganic arsenic in rice followed by hydride-generation atomic fluorescence spectrometric quantification.

作者信息

Chen Guoying, Chen Tuanwei

机构信息

U.S. Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 E. Mermaid Lane, Wyndmoor, PA 19038, USA.

College of Food Science, Fujian Agriculture and Forestry University, Fuzhou, Fujian 350002, China.

出版信息

Talanta. 2014 Feb;119:202-6. doi: 10.1016/j.talanta.2013.11.016. Epub 2013 Nov 11.

Abstract

Due to high toxicity, inorganic arsenic (iAs) species are the focus of monitoring effort worldwide. In this work arsenic was first extracted from rice by microwave-assisted digestion in HNO3-H2O2, during which As(III) was oxidized to As(V). Silica-based strong anion exchange cartridges were used to separate As(V) from organic forms. After prereduction by iodide, iAs was quantified by hydride-generation atomic fluorescence spectrometry (HG-AFS). This method achieved 1.3 ng g(-1) limit of detection (LOD), and 94 ± 3% and 93 ± 5% recoveries, respectively, for As(III) and As(V) at 100 ng g(-1). Validation was performed using standard reference material NIST 1568a (102 ng g(-1)) and ERM BC211 (124 ng g(-1)) rice flour. By eliminating chromatography, SPE speciation gained throughput and cost advantages. HG-AFS, at 10% budget and operation cost of a typical inductively-couple plasma mass spectrometer (ICPMS), proved highly sensitive and specific for iAs quantification.

摘要

由于无机砷(iAs)具有高毒性,它是全球监测工作的重点。在本研究中,首先通过在硝酸 - 过氧化氢体系中进行微波辅助消解从大米中提取砷,在此过程中As(III)被氧化为As(V)。使用基于硅胶的强阴离子交换柱将As(V)与有机形态分离。经碘化物预还原后,采用氢化物发生原子荧光光谱法(HG - AFS)对无机砷进行定量分析。该方法的检出限(LOD)为1.3 ng g(-1),对于100 ng g(-1)的As(III)和As(V),回收率分别为94 ± 3%和93 ± 5%。使用标准参考物质NIST 1568a(102 ng g(-1))和ERM BC211(124 ng g(-1))米粉进行了方法验证。通过省去色谱法,固相萃取(SPE)形态分析获得了通量和成本优势。HG - AFS以典型电感耦合等离子体质谱仪(ICPMS)10%的预算和运行成本,被证明对无机砷定量具有高灵敏度和特异性。

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