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Accurate fast screening for total and inorganic arsenic in rice grains using hydride generation atomic fluorescence spectrometry (HG-AFS)

机译:使用氢化物​​发生原子荧光光谱法(HG-AFS)准确快速筛查米粒中的总砷和无机砷

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摘要

Two novel methods based on hydride generation atomic fluorescence spectrometry for the accurate screening of total and inorganic arsenic (As) in rice grain digests in 5 and 2 minutes, respectively, are proposed here. Total As determination was achieved using online UV photolysis aided by alkaline potassium persulphate oxidation, which converted all organic As to arsenate and thus allowed quantitative hydride generation. Determination of inorganic As in rice grains was accomplished by selective hydride generation at high acidity (4.8 M HCl), which allowed ~50 times higher efficiency for hydride generation of arsenite than the prevalent form of organic As in rice, namely dimethylarsonic acid (DMA), after pre-reduction of all inorganic As using potassium iodide/ascorbic acid. The accuracy of the method was verified by (1) excellent agreement with the certified value of total As and the literature values of inorganic As in NIST SRM 1658a; (2) complete recovery of total As in NIST SRM 1568a spiked with additional 2 ng As g~(-1) of DMA; (3) excellent agreement of total and inorganic As values in 80 samples of different types, origins and treatments (standing for different matrices) compared to ICP-MS and HPLC-ICP-MS measurements; (4) ~100% recovery of inorganic As in ERM-BC-211 and a round grain rice sample even spiked with DMA up to 200 ng As g~(-1). Additionally, the low data dispersion was indicated by the low relative standard deviation (~4.3%) in the day-to-day precision for quantifying inorganic As in NIST SRM 1568a on 7 different days.
机译:提出了两种基于氢化物发生原子荧光光谱法的新颖方法,分别在5分钟和2分钟内准确筛选稻米消化物中的总砷和无机砷(As)。总砷的测定是使用在线UV光解,通过碱性过硫酸钾氧化来实现的,该方法将所有有机砷转化为砷酸盐,从而定量生成氢化物。稻谷中无机砷的测定是通过在高酸度(4.8 M HCl)下选择性氢化物生成而完成的,这使砷生成氢化物的效率比稻米中有机砷的普遍形式即二甲基砷酸(DMA)高约50倍。 ,然后使用碘化钾/抗坏血酸将所有无机As还原。 (1)与NIST SRM 1658a中总As的认证值和无机As的文献值极好的一致性,验证了该方法的准确性; (2)完全回收添加了2 ng As g〜(-1)DMA的NIST SRM 1568a中的总As; (3)与ICP-MS和HPLC-ICP-MS测量相比,在80种不同类型,来源和处理(代表不同基质)的样品中,总砷和无机砷值具有极好的一致性; (4)ERM-BC-211和圆粒大米样品中的无机砷回收率达到100%左右,甚至加入DMA达到200 ng As g〜(-1)。此外,在7个不同的日期,NIST SRM 1568a中定量分析无机As的日常精度较低,其相对标准偏差较低(〜4.3%),表明数据分散性较低。

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