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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Multi-response optimization of magnetic solid phase extraction based on carbon coated Fe _3O _4 nanoparticles using desirability function approach for the determination of the organophosphorus pesticides in aquatic samples by HPLC-UV
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Multi-response optimization of magnetic solid phase extraction based on carbon coated Fe _3O _4 nanoparticles using desirability function approach for the determination of the organophosphorus pesticides in aquatic samples by HPLC-UV

机译:基于期望函数法的碳包覆Fe _3O _4纳米颗粒磁性固相萃取多响应优化测定水样中有机磷农药的研究

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摘要

The present study investigates the application of carbon coated Fe _3O _4 (Fe _3O _4/C) magnetic nanoparticles as an adsorbent for magnetic solid phase extraction (MSPE) of trace amounts of organophosphorus pesticides (OPPs) from environmental water samples and their determination using high performance liquid chromatography with ultraviolet detection (HPLC-UV). The Fe _3O _4/C magnetic nanoparticles were synthesized by a simple hydrothermal reaction and the resultant material was characterized by X-ray powder diffraction, field emission scanning electron microscopy and Fourier transform infrared. Central composite design combined with desirability function (DF) was applied to find the experimental conditions providing the highest global extraction efficiency. These conditions were found in correspondence with a solution pH of 9.16, 97.4 mg Fe _3O _4/C and 10 mmol L ~(-1) NaCl added to samples. Under the optimal conditions, the proposed method was evaluated, and applied to the analysis of OPPs in water samples. The results demonstrated that our proposed method had wide dynamic linear range (0.05-400 ng mL ~(-1)) with a good linearity (R ~2>0.9949) and low detection limits (4.3-47.4 pg mL ~(-1)). High enrichment factors were achieved ranging from 330-1200. The established MSPE-HPLC-UV method has been successfully applied for the determination of the OPPs in spiked water samples (well, tap, river and mineral). Satisfactory recovery results showed that the matrices under consideration do not significantly affect the extraction process.
机译:本研究研究了碳包覆的Fe _3O _4(Fe _3O _4 / C)磁性纳米粒子作为吸附剂的应用,该吸附剂用于磁性固相萃取(MSPE)从环境水样品中分离出痕量有机磷农药(OPP),并通过高浓度测定紫外检测高效液相色谱(HPLC-UV)。通过简单的水热反应合成Fe _3O _4 / C磁性纳米粒子,并通过X射线粉末衍射,场发射扫描电子显微镜和傅立叶变换红外对所得材料进行表征。采用中央复合设计与合意功能(DF)相结合的方法,以找到提供最高整体萃取效率的实验条件。发现这些条件对应于溶液的pH为9.16,向样品中添加了97.4 mg Fe _3O _4 / C和10 mmol L〜(-1)NaCl。在最佳条件下,对提出的方法进行了评估,并应用于水样中的OPPs分析。结果表明,我们提出的方法具有宽动态线性范围(0.05-400 ng mL〜(-1)),良好的线性度(R〜2> 0.9949)和低检测限(4.3-47.4 pg mL〜(-1) )。获得的高富集因子范围为330-1200。建立的MSPE-HPLC-UV方法已成功用于测定加标水样(井,水龙头,河流和矿物质)中的OPP。令人满意的回收率结果表明,所考虑的基质对提取过程没有明显影响。

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