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Determination of total arsenic and speciation analysis in Mexican maize tortillas by hydride generation - microwave plasma atomic emission spectrometry and high performance liquid chromatography - inductively coupled plasma - mass spectrometry

机译:氢化物生成测定墨西哥玉米玉米粉体总砷和形态分析 - 微波等离子体原子发射光谱法和高效液相色谱 - 电感耦合等离子体质谱法

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The determination of total arsenic (tAs), inorganic As (iAs = As(III) + As(V)) and As speciation in Mexican maize tortillas has been undertaken for the first time. Hydride generation - microwave plasma atomic emission spectrometry (HG-MP-AES) with tellurium (sodium tellurite Te(IV)) as the internal standard (IS) yielded tAs results in good agreement with those provided by inductively coupled plasma mass spectrometry (ICP-MS). In seven products from local markets, tAs was found in the range of 21.8-192 mu g As kg(-1). Analysis of As(III), As(V), MMAs(V), and DMAs(V) by an established anion exchange liquid chromatography - ICP-MS procedure showed that iAs corresponded to 72.3-98.0% of tAs. A non-chromatographic procedure was envisioned for iAs: diluted tortilla extract or calibration solution (pH 9.0) was loaded on a strong anion exchange cartridge modified with silver chloride, iAs fraction was collected and analyzed by HG-MP-AES with IS. For tAs by HG-MP-AES (with IS) the method quantification limit was 47.6 mu g As kg(-1) whereas for iAs it got worse (95 mu g As kg(-1)) due to the low recovery of this As form in SPE (< 30%). In an attempt to eliminate matrix interference, the lower sample volume was loaded on the cartridge and ICP-MS was used for quantification, yielding an improved percentage recovery of 73.4%. On the other part, the iAs recovery was > 93% while analyzing natural water with off-line quantification by any of the two atomic spectrometry techniques, indicating that the chemical matrix of tortillas was responsible for poor SPE performance. It is concluded that HG-MP-AES with IS is a cost-effective alternative for the determination of tAs that offers improved precision under a nonrigorous protocol; however, efficient separation/preconcentration of iAs by SPE is still a challenge.
机译:首次确定总砷(TAS),无机(IAS = AS(III)+ AS(v))并作为墨西哥玉米玉米饼的形态。作为内标(IS)的碲(碲酸钠TE(IV))的氢化物生成 - 微波等离子体原子发射光谱法(HG-MP-AES)产生的TAS与电感耦合等离子体质谱(ICP-多发性硬化症)。在来自当地市场的七种产品中,TAS被发现在21.8-192 mu g的范围内为kg(-1)。通过已建立的阴离子交换液相色谱 - ICP-MS程序的ICP-MS和DMA(V)分析为(Ⅴ),MMA(V)和DMA(V)表明IAS达到TA的72.3-98.0%。对IAS设想的非色谱程序进行了:稀释饼提取物或校准溶液(pH9.0)在用氯化银改性的强阴离子交换盒上装载,收集IAS级分并通过HG-MP-AES分析。对于HG-MP-AES(用)的TAS,方法量化极限为47.6μg,为kg(-1),而对于IAS而言,由于该恢复,它可能会变得更糟(95μg为kg(-1))作为SPE的形式(<30%)。为了消除基质干扰,将较低样品体积加载到盒上,使用ICP-MS进行定量,得到73.4%的提高百分比恢复。另一方面,IAS回收率> 93%,同时分析了通过任何两个原子光谱法的离线量化分析天然水,表明玉米饼的化学基质对SPE表现不佳负责。得出结论,HG-MP-AES是一种成本效益的替代方案,用于确定在非富集方案下提供改善的精度;然而,SPE的IAS的有效分离/预浓度仍然是一个挑战。

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