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首页> 外文期刊>Journal of AOAC International >Speciation and determination of inorganic arsenic in rice using liquid chromatography-inductively coupled plasma/mass spectrometry: collaborative study.
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Speciation and determination of inorganic arsenic in rice using liquid chromatography-inductively coupled plasma/mass spectrometry: collaborative study.

机译:液相色谱-电感耦合等离子体/质谱法测定大米中无机砷的形态和测定:合作研究。

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摘要

An analytical method to speciate two inorganic As forms [arsenite, As(III) and arsenate, As(V)] in indica and japonica types of rice (both husked and polished) and determine the inorganic As concentration as the sum of these two was internationally validated. The method can additionally determine two organic As compounds, monomethylarsonic acid and dimethylarsinic acid, in rice as separate LC peaks. The method is based on LC separation and inductively coupled plasma (ICP)-MS detection. The method was evaluated through the International Union of Pure and Applied Chemistry/International Organization for Standardization/AOAC harmonized protocol. Sixteen laboratories from four countries participated in the study, and 13 laboratories returned valid data. Twenty test portions of 10 blind duplicates of indica and japonica type rice samples (both husked and polished) were used in this study. Repeatability RSD (RSDr) and reproducibility RSD (RSDR) were calculated at five concentrations of total inorganic As between 0.03 and 0.68 mg/kg. The RSDr was in a range of 3.8 to 7.7% and the RSDR was in a range of 10 to 36%. These performance characteristics were found to be sufficient for determination of inorganic As at or higher than 0.03 mg/kg. Applicability of the method was estimated to be in a range of 0.02-2.0 mg/kg.
机译:在analytical稻和粳稻类型(去壳和精制稻米)中确定两种无机砷形式[亚砷酸盐,As(III)和砷酸盐,As(V)]的分析方法,并确定无机砷的含量为这两种物质的总和国际认可。该方法还可以测定稻米中两种有机砷化合物,即单甲基砷酸和二甲基砷酸,作为单独的LC峰。该方法基于LC分离和电感耦合等离子体(ICP)-MS检测。通过国际纯粹与应用化学联合会/国际标准化组织/ AOAC协调协议对该方法进行了评估。来自四个国家的16个实验室参加了研究,其中13个实验室返回了有效数据。在这项研究中,使用了10个blind稻和粳稻型大米样品(去壳和精制)的10个盲品的20个测试部分。在0.03至0.68 mg / kg的五种总无机砷浓度下,计算了重复性RSD(RSDr)和重现性RSD(RSDR)。 RSDr的范围为3.8%至7.7%,RSDR的范围为10%至36%。发现这些性能特征足以确定0.03 mg / kg或更高的无机As。该方法的适用性估计为0.02-2.0 mg / kg。

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