Ning Weijie, Xiang Yuhong, Zhang Lu, Ye Nengsheng
Department of Chemistry, Capital Normal University, Beijing, 100048, China.
Department of Chemistry, Capital Normal University, Beijing, 100048, China.
Anal Chim Acta. 2024 Oct 16;1326:343148. doi: 10.1016/j.aca.2024.343148. Epub 2024 Aug 22.
Capillary electrochromatography (CEC) stationary phases have always been the focus of attention. The selection of excellent stationary phases are the key to realize separate of different compounds. Hydrogen-bonded organic frameworks (HOFs) are porous materials connected by hydrogen bonds between molecules, which have the advantages of renewable, high specific surface area and mild synthesis conditions. At present, HOFs are used in gas adsorption and storage, catalysis and drug delivery. Because of its unique advantages, HOFs have a bright future as CEC stationary phases.
Using melamine (MA) and 1,3,6,8-tetra (4-carboxylphenyl)pyrene (HTBAPy) as reaction monomers, a HOFs named MA/PFC-1 was synthesized by solvent evaporation at room temperature. The inner wall of the capillary column was coated with MA/PFC-1 by chemical bonding. Sulfonamides were used as the target analytes. The effects of pH, phosphate buffer solution concentration, organic additive content and applied voltage on sulfonamides separation were investigated. The MA/PFC-1-coated capillary column had good resolution (>1.5) and reproducibility. The intra-day, inter-day, column-to-column, and inter-batch precision of the retention times were 0.03%-0.09%, 0.04%-0.09%, 0.03%-0.14% and 0.06%-0.09%, respectively. The intra-day, inter-day, column-to-column, and inter-batch precision of the peak areas were 0.11%-0.25%, 0.13%-0.20%, 0.12%-0.15% and 0.08%-0.15%, respectively. The MA/PFC-1-coated capillary column was run 150 consecutive times, and the results showed no noticeable change, which proved that this method had good stability.
This work applied HOFs to CEC. The results show the that MA/PFC-1-coated capillary column has good separation performance. The MA/PFC-1-coated capillary column has been successfully applied to the determination of sulfamethoxazole in tablets, which has practical application value. To open up the application of HOFs in CEC and provide a new idea for developing new CEC stationary phases.
毛细管电色谱(CEC)固定相一直是人们关注的焦点。选择优良的固定相是实现不同化合物分离的关键。氢键有机骨架(HOFs)是分子间通过氢键连接的多孔材料,具有可再生、比表面积高、合成条件温和等优点。目前,HOFs已应用于气体吸附与存储、催化和药物递送等领域。由于其独特的优势,HOFs作为CEC固定相具有广阔的前景。
以三聚氰胺(MA)和1,3,6,8-四(4-羧基苯基)芘(HTBAPy)为反应单体,通过室温溶剂挥发法合成了一种名为MA/PFC-1的HOFs。采用化学键合的方法将MA/PFC-1涂覆在毛细管柱内壁。以磺胺类药物为目标分析物,考察了pH值、磷酸盐缓冲溶液浓度、有机添加剂含量和施加电压对磺胺类药物分离的影响。MA/PFC-1涂覆的毛细管柱具有良好的分离度(>1.5)和重现性。保留时间的日内、日间、柱间和批间精密度分别为0.03%-0.09%、0.04%-0.09%、0.03%-0.14%和0.06%-0.09%。峰面积的日内、日间、柱间和批间精密度分别为0.11%-0.25%、0.13%-0.20%、0.12%-0.15%和0.08%-0.15%。MA/PFC-1涂覆的毛细管柱连续运行150次,结果显示无明显变化,证明该方法具有良好的稳定性。
本工作将HOFs应用于CEC。结果表明,MA/PFC-1涂覆的毛细管柱具有良好的分离性能。MA/PFC-1涂覆的毛细管柱已成功应用于片剂中磺胺甲恶唑的测定,具有实际应用价值。为开拓HOFs在CEC中的应用并为开发新型CEC固定相提供新思路。