State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.
J Chromatogr A. 2012 Sep 28;1257:1-8. doi: 10.1016/j.chroma.2012.08.028. Epub 2012 Aug 16.
In this work, superparamagnetic nanoparticle-decorated graphene (MG) sheets were synthesized and used as support for hemimicelles/admicelles for solid-phase extraction (SPE) of different compounds from environmental water samples for the first time. The MG sheets were facilely synthesized by a one-step, one-pot redox reaction between graphene oxide and Fe(II). Due to the large surface area and unique nanosheet morphology, MG served as an excellent nano-scaled support material for hemimicelles and admicelles, exhibiting higher loading capacity than conventional materials and pure Fe₃O₄ nanoparticles. The MG sheets could be negatively or positively charged depending on solution pH, allowing the extraction to be conducted in different modes. In cationic mode, cetyltrimethylammonium bromide (CTAB) was used as micelle-forming reagent, and perfluoroalkyl and polyfluoroalkyl substances (PFASs) and alkylphenols were used as model analytes. In anionic mode, sodium dodecyl sulfate (SDS) was used as micelle-forming reagent and alkyltrimethylammonium salts were selected as analytes. In both modes, the formation processes of hemimicelles/admicelles on MG sheets were studied and the extraction conditions were optimized. For PFASs, the analytical sensitivity was enhanced by 50-113-fold by the extraction, and the method detection limits (MDLs) ranged from 0.15 to 0.50 ng/L. For alkyltrimethylammonium salts, the MDLs were in the range of 1.4-8.0 ng/L. In both modes, good recoveries (56.3-93.9%) and reproducibility (run-to-run RSDs<9.3%) were obtained. The results from this work show a potential new role of graphene in analytical sample preparation.
在这项工作中,首次合成了超顺磁纳米粒子修饰的石墨烯 (MG) 薄片,并将其用作支持物,用于从环境水样中固相萃取 (SPE) 不同化合物的半胶束/胶束。MG 薄片通过氧化石墨烯和 Fe(II) 之间的一步一锅氧化还原反应简便合成。由于其大的表面积和独特的纳米片形态,MG 薄片作为半胶束和胶束的优异纳米级支撑材料,表现出比传统材料和纯 Fe₃O₄纳米粒子更高的负载能力。MG 薄片的表面电荷可以根据溶液 pH 值而变化,允许在不同模式下进行萃取。在阳离子模式下,十六烷基三甲基溴化铵 (CTAB) 用作胶束形成试剂,全氟烷基和多氟烷基物质 (PFAS) 和烷基酚用作模型分析物。在阴离子模式下,十二烷基硫酸钠 (SDS) 用作胶束形成试剂,选择烷基三甲基铵盐作为分析物。在这两种模式下,都研究了半胶束/胶束在 MG 薄片上的形成过程,并优化了萃取条件。对于 PFAS,萃取将分析灵敏度提高了 50-113 倍,方法检测限 (MDL) 范围为 0.15-0.50ng/L。对于烷基三甲基铵盐,MDL 范围为 1.4-8.0ng/L。在这两种模式下,都获得了良好的回收率 (56.3-93.9%) 和重现性 (运行间 RSDs<9.3%)。这项工作的结果表明了石墨烯在分析样品制备中的一个潜在的新角色。