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Rapid microwave synthesis of dioxin-linked covalent organic framework for efficient micro-extraction of perfluorinated alkyl substances from water.
Journal of Hazardous Materials ( IF 12.2 ) Pub Date : 2020-04-22 , DOI: 10.1016/j.jhazmat.2020.122793 Wenhua Ji 1 , Yu-Shuang Guo 1 , Hui-Min Xie 1 , Xiao Wang 2 , Xin Jiang 1 , Dian-Shun Guo 1
Journal of Hazardous Materials ( IF 12.2 ) Pub Date : 2020-04-22 , DOI: 10.1016/j.jhazmat.2020.122793 Wenhua Ji 1 , Yu-Shuang Guo 1 , Hui-Min Xie 1 , Xiao Wang 2 , Xin Jiang 1 , Dian-Shun Guo 1
Affiliation
To synthesize covalent organic framework (COF) via irreversible reactions is more challenging than by reversible ones. In this work, microwave-assisted synthesis is used to facilitate the nucleophilic substitution of 2,3,5,6-tetrafluoro-4-pyridinecarbonitrile with 2,3,6,7,10,11-hexahydroxy triphenylene. The dioxin-linked COF, named TH-COF, was efficiently synthesized with extraordinarily large surface area of 1254 m2 g-1. With its high crystallinity, excellent thermal and chemical stabilities, TH-COF is used as the coating for the solid-phase micro-extraction (SPME) of perfluorinated alkyl substances (PFASs). The adsorptive mechanism was evaluated with adsorption isotherm and kinetic adsorption. Adsorption energies are calculated based on the density functional theory. Following SPME with TH-COF-coated fibers, PFASs were eluted using 1 mL of 0.6% trifluoroacetic acid/methanol and analyzed through the ultra-performance liquid chromatography equipped with triple quadrupole mass spectrometer (UPLC-MS/MS). When applied to spiked real water samples, this method demonstrates good linearity (0.01-1000 ng L-1) with R2 ≥ 0.9945. The TH-COF-SPME-UPLC-MS/MS technique provides low limits of detection (0.0020-0.0045 ng L-1), excellent precision (≤ 7.9%), and good fiber-to-fiber reproducibility (≤ 7.1%). The TH-COF-coated fibers can be reused at least 20 times without the loss of extraction performance. In addition, the relative recoveries from spiked real water samples are 89.5%-105%.
中文翻译:
快速微波合成二恶英连接的共价有机骨架,可从水中高效微萃取全氟烷基物质。
与不可逆反应相比,通过不可逆反应合成共价有机骨架(COF)更具挑战性。在这项工作中,微波辅助合成被用来促进2,3,6,7,10,11-六羟基苯并菲对2,3,5,6-四氟-4-吡啶腈的亲核取代。高效率地合成了二恶英连接的COF,称为TH-COF,表面积非常大,为1254 m2 g-1。TH-COF具有高结晶度,出色的热稳定性和化学稳定性,可作为全氟烷基物质(PFASs)的固相微萃取(SPME)的涂层。通过吸附等温线和动力学吸附评价吸附机理。根据密度泛函理论计算吸附能。用TH-COF涂层的纤维进行SPME处理后,用1 mL的0洗脱PFAS。6%三氟乙酸/甲醇,并通过配备三重四极杆质谱仪(UPLC-MS / MS)的超高效液相色谱进行分析。当应用于加标的真实水样时,该方法表现出良好的线性(0.01-1000 ng L-1),R2≥0.9945。TH-COF-SPME-UPLC-MS / MS技术可提供低检测限(0.0020-0.0045 ng L-1),出色的精密度(≤7.9%)和良好的光纤到光纤重现性(≤7.1%)。TH-COF涂层的纤维可以重复使用至少20次,而不会损失萃取性能。此外,从加标的真实水样中得到的相对回收率为89.5%-105%。该方法显示出良好的线性(0.01-1000 ng L-1),R2≥0.9945。TH-COF-SPME-UPLC-MS / MS技术可提供低检测限(0.0020-0.0045 ng L-1),出色的精密度(≤7.9%)和良好的光纤到光纤重现性(≤7.1%)。TH-COF涂层的纤维可以重复使用至少20次,而不会损失萃取性能。此外,从加标的真实水样中得到的相对回收率为89.5%-105%。该方法显示出良好的线性(0.01-1000 ng L-1),R2≥0.9945。TH-COF-SPME-UPLC-MS / MS技术可提供低检测限(0.0020-0.0045 ng L-1),出色的精密度(≤7.9%)和良好的光纤到光纤重现性(≤7.1%)。TH-COF涂层的纤维可以重复使用至少20次,而不会损失萃取性能。此外,从加标的真实水样中得到的相对回收率为89.5%-105%。
更新日期:2020-04-22
中文翻译:
快速微波合成二恶英连接的共价有机骨架,可从水中高效微萃取全氟烷基物质。
与不可逆反应相比,通过不可逆反应合成共价有机骨架(COF)更具挑战性。在这项工作中,微波辅助合成被用来促进2,3,6,7,10,11-六羟基苯并菲对2,3,5,6-四氟-4-吡啶腈的亲核取代。高效率地合成了二恶英连接的COF,称为TH-COF,表面积非常大,为1254 m2 g-1。TH-COF具有高结晶度,出色的热稳定性和化学稳定性,可作为全氟烷基物质(PFASs)的固相微萃取(SPME)的涂层。通过吸附等温线和动力学吸附评价吸附机理。根据密度泛函理论计算吸附能。用TH-COF涂层的纤维进行SPME处理后,用1 mL的0洗脱PFAS。6%三氟乙酸/甲醇,并通过配备三重四极杆质谱仪(UPLC-MS / MS)的超高效液相色谱进行分析。当应用于加标的真实水样时,该方法表现出良好的线性(0.01-1000 ng L-1),R2≥0.9945。TH-COF-SPME-UPLC-MS / MS技术可提供低检测限(0.0020-0.0045 ng L-1),出色的精密度(≤7.9%)和良好的光纤到光纤重现性(≤7.1%)。TH-COF涂层的纤维可以重复使用至少20次,而不会损失萃取性能。此外,从加标的真实水样中得到的相对回收率为89.5%-105%。该方法显示出良好的线性(0.01-1000 ng L-1),R2≥0.9945。TH-COF-SPME-UPLC-MS / MS技术可提供低检测限(0.0020-0.0045 ng L-1),出色的精密度(≤7.9%)和良好的光纤到光纤重现性(≤7.1%)。TH-COF涂层的纤维可以重复使用至少20次,而不会损失萃取性能。此外,从加标的真实水样中得到的相对回收率为89.5%-105%。该方法显示出良好的线性(0.01-1000 ng L-1),R2≥0.9945。TH-COF-SPME-UPLC-MS / MS技术可提供低检测限(0.0020-0.0045 ng L-1),出色的精密度(≤7.9%)和良好的光纤到光纤重现性(≤7.1%)。TH-COF涂层的纤维可以重复使用至少20次,而不会损失萃取性能。此外,从加标的真实水样中得到的相对回收率为89.5%-105%。