Fu Yuanyuan, Li Zhentao, Li Qiaoyan, Hu Changjun, Liu Yikun, Sun Wenqi, Chen Zilin
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, Hubei Province Engineering and Technology Research Center for Fluorinated Pharmaceuticals, and Wuhan University School of Pharmaceutical Sciences, Wuhan, 430071, China; State Key Laboratory of Transducer Technology, Chinese Academy of Sciences, Beijing 100080, China.
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, Hubei Province Engineering and Technology Research Center for Fluorinated Pharmaceuticals, and Wuhan University School of Pharmaceutical Sciences, Wuhan, 430071, China.
J Chromatogr A. 2021 Jul 19;1649:462239. doi: 10.1016/j.chroma.2021.462239. Epub 2021 May 11.
Covalent organic frameworks (COFs), considered as a series of newly emerging porous organic materials, have been widely utilized in separation fields. Herein, a novel COF (TFPB-BD) was first employed as stationary phase for high-efficiency capillary electrochromatographic separation. Benzidine (BD) and 1,3,5-Tris-(4-formylphenyl)benzene (TFPB) were selected as organic linkers and then introduced into the aldehyde group modified capillary for the in situ growth of TFPB-BD onto the capillary inner wall at room temperature. The morphology and formation of TFPB coated capillary column were confirmed by a variety of tools including Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and energy dispersive X-ray spectrometry (EDS). It's interesting that the TFPB globular crystals with nanoscale were uniformly and densely modified on the capillary inner surface. Hence, the prepared column exhibited prominent separation performance for the test analytes including alkylbenzenes, chlorobenzenes and phenolic compounds with high efficiency and high resolution. The maximum column efficiency can reach about 1.8 × 10 plates•m. Additionally, the high resolutions of anilines, amino acids and parabens were also achieved on the TFPB modified capillary. The precisions (RSDs) of the retention times of alkylbenzenes of intra-day runs (n = 3), inter-day runs (n = 3) and parallel columns (n = 3) were all less than 2.83%. This innovative COF-based stationary phase gives great promise for the chromatographic separation field.
共价有机框架（COFs）作为一系列新兴的多孔有机材料，已在分离领域得到广泛应用。在此，一种新型COF（TFPB-BD）首次被用作高效毛细管电色谱分离的固定相。选择联苯胺（BD）和1,3,5-三（4-甲酰基苯基）苯（TFPB）作为有机连接体，然后将其引入醛基修饰的毛细管中，在室温下使TFPB-BD在毛细管内壁原位生长。通过傅里叶变换红外光谱（FT-IR）、扫描电子显微镜（SEM）和能量色散X射线光谱（EDS）等多种工具证实了TFPB包覆毛细管柱的形态和形成情况。有趣的是，纳米级的TFPB球状晶体均匀且密集地修饰在毛细管内表面。因此，制备的色谱柱对包括烷基苯、氯苯和酚类化合物在内的测试分析物表现出显著的分离性能，具有高效率和高分辨率。最大柱效可达约1.8×10⁴ 塔板•米⁻¹。此外，在TFPB修饰的毛细管上也实现了苯胺、氨基酸和对羟基苯甲酸酯类的高分辨率分离。日内（n = 3）、日间（n = 3）和平行柱（n = 3）运行的烷基苯保留时间的精密度（相对标准偏差，RSDs）均小于2.83%。这种基于创新COF的固定相在色谱分离领域具有广阔的应用前景。
