Department of Orthopedics Trauma and Microsurgery, Zhongnan Hospital of Wuhan University, School of Pharmaceutical Sciences, Wuhan University, Wuhan 430072, China; Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, Hubei Province Engineering and Technology Research Center for Fluorinated Pharmaceuticals, Wuhan 430071, China.
Department of Orthopedics Trauma and Microsurgery, Zhongnan Hospital of Wuhan University, School of Pharmaceutical Sciences, Wuhan University, Wuhan 430072, China; Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, Hubei Province Engineering and Technology Research Center for Fluorinated Pharmaceuticals, Wuhan 430071, China.
J Chromatogr A. 2022 Jun 21;1673:463070. doi: 10.1016/j.chroma.2022.463070. Epub 2022 Apr 30.
The development of novel stationary phases to achieve high-efficiency separation is still an important topic in separation sciences. Covalent organic frameworks (COFs) with the advantages of large specific surface areas, high porosity and stability have attracted great attention in chromatographic field. Here, a novel crystalline covalent organic framework (TzDa-V) was designed and synthesized by condensation reaction between 4,4',4″-(1,3,5-Triazine-2,4,6-triyl)trianiline (Tz) and 2,5-diallyloxyterephthalaldehyde (Da-V) for open-tubular capillary electrochromatography (OT-CEC). Thanks to the regular shape, strong hydrophobicity and microporous structure of COF TzDa-V, the TzDa-V modified capillary column exhibited excellent efficiency for the separation of several groups of small molecules, including alkylbenzenes, chlorobenzenes, sulfonamides and so on. The maximum column efficiency can reach about 2.0 × 10 plates•m (for chlorobenzene). Besides, the prepared COF TzDa-V modified OT-column can afford methylbenzene loading capacity of 127.72 pmol. Also, the OT-columns were considerably stable and reproducible. The RSDs of intra-day (n = 3), inter-day (n = 3) and three batches runs for the retention times of four benzenes were all below 1.89%. Our successful work indicates the great potential of COF TzDa-V in CEC for high-efficiency separation.
新型固定相的发展以实现高效分离仍然是分离科学的一个重要课题。具有大比表面积、高孔隙率和稳定性的共价有机骨架（COFs）在色谱领域引起了极大的关注。在这里，通过 4,4',4″-(1,3,5-三嗪-2,4,6-三基)三苯胺（Tz）和 2,5-二烯丙氧基对苯二甲醛（Da-V）之间的缩合反应设计并合成了一种新型结晶共价有机骨架（TzDa-V），用于开管毛细管电色谱（OT-CEC）。由于 COF TzDa-V 的规则形状、强疏水性和微孔结构，TzDa-V 修饰的毛细管柱对包括烷基苯、氯苯、磺胺类等几类小分子的分离表现出优异的效率。最大柱效可达到约 2.0×10 块•m（用于氯苯）。此外，所制备的 COF TzDa-V 修饰的 OT 柱可以提供 127.72 pmol 的甲苯负载能力。此外，OT 柱非常稳定且重现性好。四种苯的保留时间的日内（n=3）、日间（n=3）和三批运行的 RSD 均低于 1.89%。我们的成功工作表明 COF TzDa-V 在 CEC 中具有高效分离的巨大潜力。
