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方便地制备葡萄干面包夹心结构的磁性石墨烯/介孔硅复合材料,其孔壁用 C18 修饰,用于环境水样中邻苯二甲酸酯的高效富集。

Facile preparation of raisin-bread sandwich-structured magnetic graphene/mesoporous silica composites with C18-modified pore-walls for efficient enrichment of phthalates in environmental water.

机构信息

Department of Chemistry, Fudan University, Shanghai 200433, China.

Department of Chemistry, Fudan University, Shanghai 200433, China.

出版信息

J Chromatogr A. 2014 Jan 17;1325:65-71. doi: 10.1016/j.chroma.2013.12.025. Epub 2013 Dec 15.

Abstract

In this study, novel raisin-bread sandwich-structured magnetic graphene/mesoporous silica composites with C18-modified interior pore-walls (mag-graphene@mSiO2-C18) were synthesized by coating mesoporous silica layers onto each side of magnetic graphene through a surfactant-mediated co-condensation sol-gel process. The prepared functionalized nanocomposites possessed marvelous properties of extended plate-like morphology, fine water dispersibility, high magnetic response, large surface area (315.4cm(2)g(-1)), uniform pore size (3.3nm) and C18-modified interior pore-walls. Several kinds of phthalates were selected as model analytes to systematically evaluate the performance of adsorbents in extracting hydrophobic molecules followed by gas chromatography-mass spectrometry analyses. Various extraction parameters, including pH value of sample solution, amounts of adsorbents, adsorption time, species and volume of eluting solvent, and desorption time were optimized. The anti-interference ability to macromolecular proteins was also investigated. Method validations such as linearity, recovery, reproducibility, and limit of detection were also studied. Finally, mag-graphene@mSiO2-C18 composites were successfully applied to analyzing phthalates in environmental water samples. The results indicated that this novel approach offered an attractive alternative for rapid, convenient, efficient and selective magnetic solid-phase extraction for targeted hydrophobic compounds.

摘要

在这项研究中,通过表面活性剂介导的共缩合溶胶-凝胶过程,在磁性石墨烯的每一侧涂覆介孔硅层,合成了具有 C18 修饰的内部孔壁的新型葡萄干面包夹心结构的磁性石墨烯/介孔硅复合材料(mag-graphene@mSiO2-C18)。所制备的功能化纳米复合材料具有扩展的片状形态、良好的水分散性、高磁响应性、大表面积(315.4cm2g-1)、均匀的孔径(3.3nm)和 C18 修饰的内部孔壁等优异性能。选择几种邻苯二甲酸酯作为模型分析物,系统地评估了吸附剂在提取疏水分子方面的性能,随后进行气相色谱-质谱分析。优化了各种提取参数,包括样品溶液的 pH 值、吸附剂的用量、吸附时间、洗脱溶剂的种类和体积以及解吸时间。还研究了对高分子蛋白质的抗干扰能力。还研究了方法验证,如线性、回收率、重现性和检测限。最后,成功地将 mag-graphene@mSiO2-C18 复合材料应用于环境水样中邻苯二甲酸酯的分析。结果表明,这种新方法为快速、方便、高效和选择性的磁性固相萃取提供了一种有吸引力的替代方法,用于目标疏水性化合物。

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