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In Situ Synthesis of MIL-100(Fe) in the Capillary Column for Capillary Electrochromatographic Separation of Small Organic Molecules

机译:毛细管柱中原位合成MIL-100(Fe)用于小的有机分子的毛细管电色谱分离

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Because of the unusual properties of the structure, the metal organic frameworks (MOFs) have received great interest in separation science. However, the most existing methods for the applications of MOFs in separation science require an off-line procedure to prepare the materials. Here, we report an in situ, layer-by-layer self-assembly approach to fabricate MIL-100(Fe) coated open tubular (OT) capillary columns for capillary electrochromatography. By a controllable manner, the OT capillary columns with a tailored MIL-100(Fe) coating have been successfully synthesized. The results of SEM, XRD, FT-IR, and ICP-AES indicated that MIL-100(Fe) was successfully grafted on the inner wall of the capillary. Some neutral, acidic and basic analytes were used to evaluate the performance of the MIL-100(Fe) coating OT capillary column. Because of the size selectivity of lattice aperture and hydrophobicity of the organic ligands, three types of analytes were well separated with this novel MIL-100(Fe) coating OT capillary column. For three consecutive runs, the intraday relative standard deviations (RSDs) of migration time and peak areas were 0.4-4.6% and 1.2-6.6%, respectively. The interday RSDs of migration time and peak areas were 0.6-8.0% and 2.2-9.5%, respectively. The column-to-column reproducibility of retention time was in range of 0.6-9.2%. Additionally, the 10 cycles OT capillary column (10-LC) could be used for more than 150 runs with no observable changes on the separation efficiency.
机译:由于结构的不同寻常的特性,金属有机骨架(MOF)在分离科学中引起了极大的兴趣。但是,在分离科学中应用MOF的大多数现有方法都需要离线过程来制备材料。在这里,我们报告了一种原位,逐层自组装方法来制造用于毛细管电色谱的MIL-100(Fe)涂层开放管式(OT)毛细管柱。通过可控的方式,已成功合成了具有量身定制的MIL-100(Fe)涂层的OT毛细管柱。 SEM,XRD,FT-IR和ICP-AES的结果表明,MIL-100(Fe)已成功接枝到毛细管的内壁上。一些中性,酸性和碱性分析物用于评估MIL-100(Fe)涂层OT毛细管柱的性能。由于晶格孔径的大小选择性和有机配体的疏水性,使用这种新型的MIL-100(Fe)涂层OT毛细管色谱柱可以很好地分离出三种类型的分析物。对于三个连续运行,迁移时间和峰面积的日内相对标准偏差(RSD)分别为0.4-4.6%和1.2-6.6%。迁移时间和高峰区域的日间相对标准偏差分别为0.6-8.0%和2.2-9.5%。保留时间从色谱柱到色谱柱的重现性在0.6-9.2%的范围内。此外,10个循环OT毛细管柱(10-LC)可以用于150多个运行,而分离效率没有明显变化。

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