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首页> 美国卫生研究院文献>The Journal of Automatic Chemistry >Speciation Analysis of Arsenic Compounds by High-Performance Liquid Chromatography in Combination with Inductively Coupled Plasma Dynamic Reaction Cell Quadrupole Mass Spectrometry: Application for Vietnamese Rice Samples
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Speciation Analysis of Arsenic Compounds by High-Performance Liquid Chromatography in Combination with Inductively Coupled Plasma Dynamic Reaction Cell Quadrupole Mass Spectrometry: Application for Vietnamese Rice Samples

机译：高效液相色谱-电感耦合等离子体动力学反应池四极杆质谱联用分析砷化合物的形态：在越南大米样品中的应用

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In this work, high-performance liquid chromatography in combination with inductively coupled plasma dynamic reaction cell quadrupole mass spectrometry was introduced and optimized for speciation analysis of five major arsenic species including arsenobetain (AsB), arsenite (As(III)), monomethylarsonic (MMA), dimethylarsenonic acid (DMA), and arsenate (As(V)) in rice samples. Five arsenic compounds were separated on a Hamilton PRP X100 strong anion-exchange column employed with the mobile phase that is compatible with mass spectrometry, containing ammonium carbonate, methanol, and disodium ethylenediaminetetraacetic acid. Arsenic compounds were detected online by inductively coupled plasma dynamic reaction cell quadrupole mass spectrometry utilizing oxygen as the reaction gas at a flow rate of 0.7 mL·min−1. Five selected arsenic species were baseline separated at the optimum experimental conditions. The excellent LOD and LOQ values of the developed method were achieved in the range of 0.5 to 2.9 μg·kg−1 and 1.7 to 9.6 μg·kg−1 for all species of arsenic, respectively. The ionization effect in plasma during chromatographic gradient elution was systematically investigated by using postcolumn injector. Arsenic compounds in rice samples were extracted by diluted nitric acid at elevated temperature. The extraction efficiency and the interconversion of target compounds during sample preparation were also assessed. The full validation of the developed method was performed by using certified reference material, BRC 211, from European Institute of Reference and Standard for speciation analysis. The recovery of all selected arsenic species was in the range of 70 to 135.5%. The validated method was also applied to analyze rice samples collected from some contaminated rice fields. The results showed that As(III), DMA, and As(V) were found in all rice samples. Average concentration (range) of inorganic arsenic and DMA in all rice samples were 130.3 (65.5–228.1) and 32 (8.2–133.01) μg·kg−1, respectively. However, total concentration of inorganic arsenic in most of investigated rice samples was below the maximum residual level according to US-FDA and European Union standards.
机译：在这项工作中，引入了高效液相色谱法与电感耦合等离子体动态反应池四极质谱联用，并对其进行了优化，以分析五种主要砷形态，包括砷中毒（AsB），亚砷酸盐（As（III）），单甲基砷（MMA） ），大米样品中的二甲基砷酸（DMA）和砷酸盐（As（V））。在Hamilton PRP X100强阴离子交换色谱柱上分离出五种砷化合物，该色谱柱用于与质谱兼容的流动相，其中含有碳酸铵，甲醇和乙二胺四乙酸二钠。电感耦合等离子体动态反应池四极杆质谱以氧气为反应气体，流速为0.7 mL·min -1 在线检测砷化合物。在最佳实验条件下将五个选定的砷物质进行基线分离。对于所有物种，该方法的LOD和LOQ值均达到0.5至2.9μg·kg -1 和1.7至9.6μμg·kg -1 分别是砷。使用柱后进样器系统地研究了色谱梯度洗脱过程中血浆中的电离效应。大米样品中的砷化合物在高温下用稀硝酸萃取。还评估了样品制备过程中目标化合物的提取效率和相互转化。通过使用欧洲参考标准协会的认证参考材料BRC 211进行形态分析，对开发的方法进行了全面验证。所有选定的砷物种的回收率在70至135.5％之间。经过验证的方法还可以用于分析从一些受污染的稻田中采集的稻米样品。结果表明，在所有大米样品中均发现了As（III），DMA和As（V）。所有大米样品中无机砷和DMA的平均浓度（范围）分别为13g（65.5-228.1）和32（8.2-133.01）μg·kg -1 。但是，根据美国食品和药物管理局和欧盟的标准，​​大多数被调查的大米样品中无机砷的总浓度低于最大残留水平。

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