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Magnetic restricted-access carbon nanotubes for the extraction/pre-concentration of organophosphates from food samples followed by spectrophotometric determination.
Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy ( IF 4.4 ) Pub Date : 2020-06-20 , DOI: 10.1016/j.saa.2020.118632
Pedro Marcos Frugeri 1 , Marcello Henrique da Silva Cavalcanti 1 , Ayla Campos do Lago 2 , Eduardo Costa Figueiredo 3 , Cesar Ricardo Teixeira Tarley 4 , Célio Wisniewski 5 , Pedro Orival Luccas 1
Affiliation  

In this work, magnetic restricted-access carbon nanotubes (M-RACNTs) were synthesized, characterized and used in the dispersive solid-phase extraction (d-SPE) of organophosphate pesticides (OPPs) from food samples (broccoli, eggplant, cauliflower, and soy milk), followed by spectrophotometric determination in a flow injection analysis system. Fe3O4 nanoparticles were incorporated in the multi-walled carbon nanotubes employing dimethylformamide. The dimethylformamide was used as a solvent in the incorporation process, forming the suspension of both particles.

The resulting M-CNTs were covered with an external bovine serum albumin (BSA) layer, chemically crosslinked. M-RACNTs were able to efficiently capture OPPs, excluding about 95% of the proteins from food matrices. The analyses were carried out in a flow injection analysis system (FIA), with the spectrophotometric detection (at 560 nm) of the complex formed by the reaction between OPPs, N-bromosuccinimide and rhodamine B. A fractional factorial design method was used to optimize the experimental parameters. The addition/recovery test showed results from 95.5% to 108.9%. Accuracies were checked by comparing the results obtained with the proposed and standard HPLC methods, which were in agreement. The proposed method was linear from 5 to 90 μg L−1 of OPPs, with limits of detection and quantification of 0.74 and 5 μg L−1 and precision of 3.67%, expressed as relative standard deviation. The pre-concentration factor was about 164 times.



中文翻译:

磁性限制进入的碳纳米管,用于从食品样品中提取/预浓缩有机磷酸盐,然后进行分光光度法测定。

在这项工作中,合成了磁性受限访问的碳纳米管(M-RACNT),对其进行了表征,并将其用于从食物样品(西兰花,茄子,菜花和菜籽)中有机磷农药(OPP)的分散固相萃取(d-SPE)。豆浆),然后在流动注射分析系统中进行分光光度测定。将Fe 3 O 4纳米颗粒掺入采用二甲基甲酰胺的多壁碳纳米管中。在掺入过程中将二甲基甲酰胺用作溶剂,形成两个颗粒的悬浮液。

所得的M-CNT被化学交联的外部牛血清白蛋白(BSA)层覆盖。M-RACNTs能够有效捕获OPP,从食物基质中排除约95%的蛋白质。分析是在流动注射分析系统(FIA)中进行的,通过分光光度法检测由OPP,N-溴代琥珀酰亚胺和若丹明B之间的反应形成的络合物(在560 nm)。采用分数阶乘设计方法进行了优化实验参数。添加/恢复测试显示结果为95.5%至108.9%。通过比较与拟议方法和标准HPLC方法获得的结果(一致)来检查准确性。所提出的方法在5至90μgL -1之间呈线性OPP的检出限和定量限为0.74和5μgL -1,精度为3.67%,以相对标准偏差表示。预浓缩系数约为164倍。

更新日期:2020-07-07
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