Pellicer-Castell Enric, Belenguer-Sapiña Carolina, El Haskouri Jamal, Amorós Pedro, Herrero-Martínez José Manuel, Mauri-Aucejo Adela R
Department of Analytical Chemistry, Faculty of Chemistry, Universitat de València, Dr. Moliner 50, 46100 Burjassot, Valencia, Spain.
Institute of Material Science (ICMUV), Universitat de València, Catedrático José Beltrán 2, 46980 Paterna, Valencia, Spain.
Nanomaterials (Basel). 2022 Apr 23;12(9):1441. doi: 10.3390/nano12091441.
In this work, sorbets based on UVM-7 mesoporous silica doped with Fe were synthesized and applied to solid-phase extraction of perfluoroalkyl substances from environmental water samples. These emerging pollutants were then determined by liquid chromatography coupled with a mass spectrometry detector. Thus, Fe-UVM-7 mesoporous silica materials with different contents of iron, as well as different pore sizes (by using alkyltrimethilamonium bromide surfactants with different organic tail lengths) were synthesized, and their structure was confirmed for the first time by transmission electron microscopy, nitrogen adsorption-desorption, X-ray diffraction, and Raman spectroscopy. After comparison, Fe50-UVM-7-C was selected as the best material for analyte retention, and several extraction parameters were optimized regarding the loading and elution step. Once the method was developed and applied to real matrices, extraction efficiencies in the range of 61-110% were obtained for analytes with C-C chain length, both perfluoroalkyl carboxylates, and perfluoroalkyl sulfonates. Likewise, limits of detection in the range of 3.0-8.1 ng L were obtained for all target analytes. In the analysis of real well-water samples, no target compounds were detected. Spiked samples were analyzed in comparison to Oasis WAX cartridges, and statistically comparable results were achieved.
在本研究中，合成了基于掺杂铁的UVM-7介孔二氧化硅的冰糕，并将其应用于从环境水样中固相萃取全氟烷基物质。然后通过液相色谱与质谱检测器联用测定这些新兴污染物。因此，合成了具有不同铁含量以及不同孔径（通过使用具有不同有机尾链长度的烷基三甲基溴化铵表面活性剂）的Fe-UVM-7介孔二氧化硅材料，并首次通过透射电子显微镜、氮吸附-脱附、X射线衍射和拉曼光谱对其结构进行了确认。经过比较，选择Fe50-UVM-7-C作为分析物保留的最佳材料，并对加载和洗脱步骤的几个萃取参数进行了优化。该方法开发并应用于实际基质后，对于具有C-C链长度的分析物，全氟烷基羧酸盐和全氟烷基磺酸盐的萃取效率在61-110%范围内。同样，所有目标分析物的检测限在3.0-8.1 ng/L范围内。在实际井水样品分析中，未检测到目标化合物。与Oasis WAX柱相比，对加标样品进行了分析，并获得了具有统计学可比性的结果。
