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Application of multivariate optimization in the development of an ultrasound-assisted extraction procedure for multielemental determination in bean seeds samples using ICP OES

机译:多元优化技术在使用ICP OES进行豆类样品中多元素测定的超声辅助提取方法开发中的应用

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In this paper, multivariate optimization was applied for the development of an ultrasound-assisted multielemental extraction procedure for analysis of bean samples by inductively coupled plasma optical emission spectrometry. For this procedure, powdered samples were treated with an acid mixture and submitted to ultrasound energy for extracting the target elements (Ba, Ca, Cu, Fe, K, Mg, Mn, Sr and Zn). Centroid simplex mixture design was used for optimize the acid proportions (nitric, acetic and chloride acid) and Box Behnken design was applied for optimize the process variables (particle size, final concentration of extracting solution and sonication time) after mixture optimization. Iron had not presented quantitative extractions and it was excluded from final samples analysis, The developed method presents the follow limits of quantification in mu g g(-1): Ba (0.90); Ca (5.2); Cu (4.0); K (0.90); Mg (1.4); Mn (0.22); Sr (0.25) and Zn (4.0). Accuracy was accessed by comparison of determined concentration with the values obtained by the microwave digestion procedure. The proposed method was applied toward the determination of elemental composition in bean samples collected in the country zone from Jequie city located on the Bahia State, Brazil. The trace elements content ranged from 0.21 to 3.04, 3.84 to 10.8, 0.60 to 5.23, 31.0 to 46.5 and 10.8 to 19.6 mu g g(-1) Ba, Cu. Sr, Zn, Mn, respectively. The major elements content ranged from 0.0418 to 0.0877, 0.109 to 0.153 and 1.30 to 1.56% (w/w) Ca, Mg and K, respectively.
机译:在本文中,多变量优化被用于开发超声波辅助的多元素萃取程序,用于通过电感耦合等离子体发射光谱法分析豆样品。对于此程序,将粉末状样品用酸混合物处理,并施加超声能量以提取目标元素(Ba,Ca,Cu,Fe,K,Mg,Mn,Sr和Zn)。质心单纯形混合物设计用于优化酸比例(硝酸,乙酸和氯酸),Box Behnken设计用于优化混合物优化后的工艺变量(粒径,萃取液的最终浓度和超声处理时间)。铁未进行定量提取,因此未从最终样品分析中排除。所开发的方法以μg g(-1)表示定量的以下限制:Ba(0.90); Ca(5.2);铜(4.0); K(0.90);镁(1.4);锰(0.22); Sr(0.25)和Zn(4.0)。通过将确定的浓度与通过微波消解程序获得的值进行比较来获得准确性。所提出的方法用于测定从巴西巴伊亚州杰基市郊外地区收集的豆类样品中的元素成分。微量元素含量范围为0.21至3.04、3.84至10.8、0.60至5.23、31.0至46.5和10.8至19.6μg g(-1)Ba,Cu。分别为Sr,Zn,Mn。主要元素含量分别为0.0418至0.0877、0.109至0.153和1.30至1.56%(w / w)Ca,Mg和K.

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