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Nitric Acid-based Partial-digestion Method for Selective Determination of Inorganic Arsenic in Hijiki and Application to Soaked Hijiki

机译:硝酸部分消化法选择性测定土Hi中的无机砷及其在浸泡土Hi中的应用

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Because there is a great difference between the toxicity of inorganic arsenic (As) and organic As in food, the JECFA has set a PTWI value for inorganic As (iAs) rather than for total As. The difference in As toxicity makes it necessary to extract iAs completely from food samples for toxicological analysis, but complete extraction of As from most foods including seaweed has not been achieved to date. We developed a partial-digestion method that uses nitric acid as a solvent in order to extract almost all arsenicals from the solid matrix of hijiki (Hizikia fusiforme, a brown alga) samples. In this method, organic As species were not converted into iAs. HPLC/ICP-MS was then used to determine the concentration of iAs. Total As was measured by hydride generation-atomic absorption spectrometry. The adopted conditions for 0.1 g of ground fine powder sample were: 2 mL of 0.3 mol/L nitric acid; heating, 80℃ for 1 hr. Intra-laboratory validation of the method showed good precision and accuracy. The repeatability and intermediate precision for iAs were 1.5% and 1.5%, respectively. The LOD and LOQ for iAs were 0.14 and 0.46 mg/kg dry weight, respectively. Recovery studies performed by spiking 0.5 mg/kg dry weight as the LOQ level and by spiking 3 mg/kg dry weight as the iAs concentration of an un-spiked hijiki sample showed good accuracy. The method was applied to hijiki samples after a water soaking process and a water soaking and simmering process. The results suggested that the As concentration in hijiki after both processes was lower than that before the treatments and that the water soaking and simmering process reduced the iAs concentration much more effectively than the water soaking process.
机译:由于食品中无机砷(As)和有机砷的毒性之间存在很大差异,因此JECFA设定了无机砷(iAs)而不是总砷的PTWI值。砷毒性的差异使得有必要从食品样本中完全提取iAs进行毒理学分析,但是迄今为止,尚未从包括海藻在内的大多数食品中完全提取iAs。我们开发了一种使用硝酸作为溶剂的部分消化方法,以便从hijiki(Hizikia fusiforme,褐藻)样品的固体基质中提取几乎所有的砷。在这种方法中,有机砷物种没有转化为iAs。然后使用HPLC / ICP-MS测定iAs的浓度。通过氢化物发生原子吸收光谱法测量总砷。 0.1g研磨细粉样品的采用条件为:2 mL 0.3 mol / L硝酸; 80℃加热1小时。该方法在实验室内的验证显示出良好的准确性和准确性。 iAs的重复性和中间精度分别为1.5%和1.5%。 iAs的LOD和LOQ分别为0.14和0.46 mg / kg干重。通过掺加0.5 mg / kg干重作为LOQ水平和掺加3 mg / kg干重作为未掺入的hijiki样品的iAs浓度进行的恢复研究显示出良好的准确性。该方法在经过水浸泡过程和水浸泡和煮过程之后被应用于hijiki样品。结果表明,两个工艺后的hijiki中的As浓度均低于处理前的水平,并且浸水和煮过程比浸水过程更有效地降低了iAs浓度。

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