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碳纳米角在甲基丙烯酸酯整体毛细管柱的自由基聚合中的作用及其作为萃取相的应用。

Effect of carbon nanohorns in the radical polymerization of methacrylate monolithic capillary columns and their application as extractant phases.

机构信息

Departamento de Química Analítica, Instituto Universitario de Investigación en Química Fina y Nanoquímica IUNAN, Universidad de Córdoba, Campus de Rabanales, Edificio Marie Curie, E-14071 Córdoba, Spain.

Departamento de Química Analítica, Instituto Universitario de Investigación en Química Fina y Nanoquímica IUNAN, Universidad de Córdoba, Campus de Rabanales, Edificio Marie Curie, E-14071 Córdoba, Spain.

出版信息

Talanta. 2019 Jan 1;191:149-155. doi: 10.1016/j.talanta.2018.08.054. Epub 2018 Aug 22.

Abstract

A successful copolymerization of the single-walled carbon nanohorns (SWNHs) with methacrylate monomers was achieved via thermal initiated free-radical polymerization because of the high reactivity of the SWNHs in comparison with other carbon nanostructures. The hybrid solids were deeply characterized in terms of morphology, by scanning electron microscopy (SEM). The effect of the incorporation of the bare or oxidized (o-SWNHs) carbon nanoparticles at different percentages (0-0.5 wt%) in polymerization mixtures to obtain hybrid monolithic capillary columns has been evaluated. In addition, their impact both in the polymerization step and in the extraction capacity was deeply studied. Final hybrid monoliths were applied for the extraction of polycyclic aromatic hydrocarbons and nonsteroidal anti-inflammatory drugs in water and biological samples, respectively. The precision was calculated both intra- and inter-capillaries obtaining satisfactory RSD values of less than 19.1%, which indicated the high robust reproducibility of the extraction procedure and the synthesis method. The accuracy of the method was also evaluated through a recovery study giving good recovery values, which varied between 78% and 112% for PAHs in waters, and 90-114% for NSAIDs in human urine samples.

摘要

通过热引发自由基聚合,成功地将单壁碳纳米角(SWNHs)与甲基丙烯酸酯单体共聚,这是由于 SWNHs 与其他碳纳米结构相比具有更高的反应性。通过扫描电子显微镜(SEM)对混合固体的形貌进行了深入的表征。评估了在聚合混合物中以不同百分比(0-0.5wt%)掺入未处理或氧化(o-SWNHs)碳纳米粒子对获得混合整体毛细管柱的影响。此外,还深入研究了它们在聚合步骤和萃取能力方面的影响。最终的混合整体柱分别用于水和生物样品中多环芳烃和非甾体抗炎药的萃取。通过在毛细管内和毛细管间进行精度计算,得到了令人满意的小于 19.1%的 RSD 值,这表明萃取过程和合成方法具有很高的稳健重现性。通过回收率研究评估了该方法的准确性,给出了良好的回收率值,对于水中的 PAHs 回收率在 78%至 112%之间,对于人尿样中的 NSAIDs 回收率在 90%至 114%之间。

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