Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia, Burjassot, Valencia, Spain.
Department of Chemistry, Faculty of Science, Suez University, Suez, Egypt.
J Sep Sci. 2019 Feb;42(4):834-842. doi: 10.1002/jssc.201801135. Epub 2019 Jan 4.
Metal-organic frameworks consisting of amino-modified MIL-101(M: Cr, Al, and Fe) crystals have been synthesized and subsequently incorporated to glycidyl methacrylate monoliths to develop novel stationary phases for nano-liquid chromatography. Two incorporation approaches of these materials in monoliths were explored. The metal-organic framework materials were firstly attached to the pore surface through reaction of epoxy groups present in the parent glycidyl methacrylate-based monolith. Alternatively, NH -MIL-101(M) were admixed in the polymerization mixture. Using short time UV-initiated polymerization, monolithic beds with homogenously dispersed metal-organic frameworks were obtained. The chromatographic performance of embedded UV-initiated composites was demonstrated with separations of polycyclic aromatic hydrocarbons and non-steroidal anti-inflammatory drugs as test solutes. In particular, the incorporation of the NH -MIL-101(Al) into the organic polymer monoliths led to an increase in the retention of all the analytes compared to the parent monolith. The hybrid monolithic columns also exhibited satisfactory run-to-run and column-to-column reproducibility.
合成了由氨基修饰的 MIL-101（M：Cr、Al 和 Fe）晶体组成的金属有机骨架，并将其随后掺入到甲基丙烯酸缩水甘油酯单体中，以开发用于纳流液相色谱的新型固定相。探索了这两种材料在单体中的两种掺入方法。首先，通过存在于母体甲基丙烯酸缩水甘油酯基单体中的环氧基团的反应，将金属有机骨架材料附着到孔表面上。或者，将 NH-MIL-101（M）混合在聚合混合物中。使用短时间的 UV 引发聚合，获得了均匀分散有金属有机骨架的整体床。嵌入的 UV 引发复合材料的色谱性能通过多环芳烃和非甾体抗炎药作为测试溶质的分离来证明。特别是，与母体单体相比，将 NH-MIL-101（Al）掺入有机聚合物单体中导致所有分析物的保留增加。杂化整体柱还表现出令人满意的运行间和柱间重现性。
