Bao Tao, Zhang Juan, Zhang Wenpeng, Chen Zilin
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, and Wuhan University School of Pharmaceutical Sciences, Wuhan 430071, China; State Key Laboratory of Transducer Technology, Chinese Academy of Sciences, Beijing 10080, China.
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, and Wuhan University School of Pharmaceutical Sciences, Wuhan 430071, China.
J Chromatogr A. 2015 Feb 13;1381:239-46. doi: 10.1016/j.chroma.2015.01.005. Epub 2015 Jan 12.
Much attention is being paid to applying metal-organic frameworks (MOFs) as stationary phases in chromatography because of their fascinating properties, such as large surface-to-volume ratios, high levels of porosity, and selective adsorption. HKUST-1 is one of the best-studied face-centered-cubic MOF containing nano-sized channels and side pockets for film growth. However, growth of HKUST-1 framework inside capillary column as stationary phase for capillary electrochromatography is a challenge work. In this work, we carry out the growth of HKUST-1 on the inner wall of capillary by using liquid-phase epitaxy process at room temperature. The fabricated HKUST-1@capillary can be successfully used for the separation of substituted benzene including methylbenzene, ethylbenzene, styrene, chlorobenzene, bromobenzene, o-dichlorobenzene, benzene series, phenolic acids, and benzoic acids derivates. High column efficiency of 1.5×10(5) N/m for methylbenzene was achieved. The formation of HKUST-1 grown in the capillary was confirmed and characterized by scanning electron microscopy images, Fourier transform infrared spectra and X-ray diffraction. The column showed long lifetime and excellent stability. The relative standard deviations for intra-day and inter-day repeatability of the HKUST-1@capillary were lower than 7%.
由于金属有机框架材料（MOFs）具有诸如大的比表面积、高孔隙率和选择性吸附等迷人特性，其作为色谱固定相正受到广泛关注。HKUST-1是研究最为深入的面心立方MOF之一，它含有纳米尺寸的通道和用于薄膜生长的侧袋。然而，在毛细管柱内生长HKUST-1框架作为毛细管电色谱的固定相是一项具有挑战性的工作。在这项工作中，我们通过在室温下使用液相外延法在毛细管内壁上生长HKUST-1。所制备的HKUST-1@毛细管可成功用于分离包括甲苯、乙苯、苯乙烯、氯苯、溴苯、邻二氯苯、苯系物、酚酸和苯甲酸衍生物在内的取代苯。对于甲苯，实现了1.5×10(5) N/m的高柱效。通过扫描电子显微镜图像、傅里叶变换红外光谱和X射线衍射对在毛细管中生长的HKUST-1的形成进行了确认和表征。该柱显示出长寿命和优异的稳定性。HKUST-1@毛细管日内和日间重复性的相对标准偏差低于7%。
