Zhang Li-Shun, Zhao Qing-Li, Li Xin-Xin, Li Xi-Xi, Huang Yan-Ping, Liu Zhao-Sheng
Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics (Theranostics), School of Pharmacy, Tianjin Medical University, Tianjin 300070, China.
Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics (Theranostics), School of Pharmacy, Tianjin Medical University, Tianjin 300070, China.
Talanta. 2016 Dec 1;161:660-667. doi: 10.1016/j.talanta.2016.09.030. Epub 2016 Sep 11.
A hybrid monolith incorporated with mesoporous molecular sieve MCM-41 of uniform pore structure and high surface area was prepared with binary green porogens in the first time. With a mixture of room temperature ionic liquids and deep eutectic solvents as porogens, MCM-41 was modified with 3-(trimethoxysilyl) propyl methacrylate (γ-MPS) and the resulting MCM-41-MPS was incorporated into poly (BMA-co-EDMA) monoliths covalently. Because of good dispersibility of MCM-41-MPS in the green solvent-based polymerization system, high permeability and homogeneity for the resultant hybrid monolithic columns was achieved. The MCM-41-MPS grafted monolith was characterized by scanning electron microscopy, energy dispersive spectrometer area scanning, transmission electron microscopy, FT-IR spectra and nitrogen adsorption tests. Chromatographic performance of MCM-41-MPS grafted monolith was characterized by separating small molecules in capillary electrochromatography, including phenol series, naphthyl substitutes, aniline series and alkyl benzenes. The maximum column efficiency of MCM-41-MPS grafted monolith reached 209,000 plates/m, which was twice higher than the corresponding MCM-41-MPS free monolith. Moreover, successful separation of non-steroidal anti-inflammatory drugs and polycyclic aromatic hydrocarbons demonstrated the capacity in broad-spectrum application of the MCM-41-MPS incorporated monolith. The results indicated that green synthesis using room temperature ionic liquid and deep eutectic solvents is an effective method to prepare molecular sieve-incorporated monolithic column.
首次采用二元绿色致孔剂制备了一种包含具有均匀孔结构和高比表面积的介孔分子筛MCM - 41的混合整体柱。以室温离子液体和低共熔溶剂的混合物为致孔剂，用甲基丙烯酸3 -（三甲氧基硅基）丙酯（γ - MPS）对MCM - 41进行改性，然后将所得的MCM - 41 - MPS共价结合到聚（BMA - co - EDMA）整体柱中。由于MCM - 41 - MPS在基于绿色溶剂的聚合体系中具有良好的分散性，因此所得混合整体柱具有高渗透性和均匀性。通过扫描电子显微镜、能谱仪面积扫描、透射电子显微镜、傅里叶变换红外光谱和氮气吸附测试对MCM - 41 - MPS接枝整体柱进行了表征。通过在毛细管电色谱中分离小分子，包括酚类系列、萘基取代物、苯胺系列和烷基苯，对MCM - 41 - MPS接枝整体柱的色谱性能进行了表征。MCM - 41 - MPS接枝整体柱的最大柱效达到209,000理论塔板数/米，比相应的不含MCM - 41 - MPS的整体柱高出两倍。此外，成功分离非甾体抗炎药和多环芳烃证明了含MCM - 41 - MPS整体柱在广谱应用方面的能力。结果表明，使用室温离子液体和低共熔溶剂进行绿色合成是制备包含分子筛的整体柱的有效方法。
