Barbosa Marta O, Ribeiro Rui S, Ribeiro Ana R L, Pereira M Fernando R, Silva Adrián M T
Laboratory of Separation and Reaction Engineering-Laboratory of Catalysis and Materials (LSRE-LCM), Faculdade de Engenharia, Universidade do Porto, Rua Dr. Roberto Frias s/n, 4200-465, Porto, Portugal.
Sci Rep. 2021 Jul 5;11(1):13817. doi: 10.1038/s41598-021-93163-2.
Carbon xerogels (CXs) were synthesized by polycondensation of resorcinol and formaldehyde, followed by thermal annealing, and subjected to hydrothermal oxidation. Solid-phase extraction (SPE) cartridges were filled with CXs and tested for extraction of metaflumizone and other seven environmental micropollutants (acetamiprid, atrazine, isoproturon, methiocarb, carbamazepine, diclofenac, and perfluorooctanesulfonic acid) before chromatographic analysis. The recoveries obtained with the pristine CX were low for most analytes, except for metaflumizone (69 ± 5%). Moreover, it was concluded that the adsorption/desorption process of the micropollutants performed better on CXs with a less acidic surface (i.e., pristine CX). Thus, cartridges were prepared with pristine CX and multi-walled carbon nanotubes (MWCNTs) in a multi-layer configuration. This reusable cartridge was able to simultaneously extract the eight micropollutants and was used to validate an analytical methodology based on SPE followed by ultra-high performance liquid chromatography-tandem mass spectrometry. A widespread occurrence of 6/8 target compounds was observed in surface water collected in rivers supplying three drinking water treatment plants and in the resulting drinking water at the endpoint of each distribution system. Therefore, the first study employing CXs and MWCNTs as sorbent in multi-layer SPE cartridges is herein reported as a proof of concept for determination of multi-class water micropollutants.
通过间苯二酚和甲醛的缩聚反应合成碳干凝胶(CXs),随后进行热退火,并进行水热氧化。在色谱分析之前,将CXs填充到固相萃取(SPE)小柱中,并测试其对甲氟虫脲和其他七种环境微污染物(啶虫脒、阿特拉津、异丙隆、灭虫威、卡马西平、双氯芬酸和全氟辛烷磺酸)的萃取效果。对于大多数分析物,除甲氟虫脲(69±5%)外,原始CX获得的回收率较低。此外,得出的结论是,微污染物在表面酸性较低的CXs(即原始CX)上的吸附/解吸过程表现更好。因此,制备了具有原始CX和多层配置的多壁碳纳米管(MWCNT)的小柱。这种可重复使用的小柱能够同时萃取八种微污染物,并用于验证基于SPE随后进行超高效液相色谱-串联质谱的分析方法。在为三个饮用水处理厂供水的河流中采集的地表水以及每个分配系统终点处的饮用水中,观察到6/8种目标化合物广泛存在。因此,本文报道了首次使用CXs和MWCNT作为多层SPE小柱中的吸附剂来测定多类水中微污染物的概念验证研究。