Department of Chemistry, Capital Normal University, Beijing, 100048, PR China.
Department of Chemistry, Capital Normal University, Beijing, 100048, PR China.
J Chromatogr A. 2023 Sep 13;1706:464234. doi: 10.1016/j.chroma.2023.464234. Epub 2023 Jul 22.
In this work, a three-dimensional fluorinated covalent organic frameworks (3D FCOFs) JUC-515 was synthesized from tetra(4-aminophenyl)methane (TAM) and 2,3,5,6-tetrafluoroterephthalol (TFA) by an ionic liquid method. JUC-515 was introduced into the capillary column and bonded to the inner wall of the capillary column by chemical bonding. Through a variety of characterization results, JUC-515 was successfully synthesized and introduced into the capillary column. The effects of buffer solution concentration, organic additive content and pH of the buffer solution on the separation of fluoroquinolones (FQs) were investigated in detail. The JUC-515-coated capillary column showed good resolution (>1.5) and reproducibility. The relative standard deviations (RSDs) of the retention time for intraday, interday, column-to-column and interbatch precision were less than 0.88%, 2.45%, 2.74% and 3.32%, respectively. The RSDs of the peak area for intraday, interday, column-to-column and interbatch precision were less than 3.79%, 4.31%, 3.33% and 5.62%, respectively. The JUC-515-coated capillary column could be used no less than 150 times. The results showed that the JUC-515-coated capillary column had good separation performance. In addition, by separating fluorinated β-phenylalanine analogs, β-phenylalanine and trifluoromethyl β-phenylalanine analogs, the separation mechanism based on fluorine interactions was discussed. In conclusion, JUC-515 had good potential as a stationary phase for capillary electrochromatography.
在这项工作中，通过离子液体法，由四(4-氨基苯基)甲烷(TAM)和 2,3,5,6-四氟对苯二甲酸(TFA)合成了三维氟化共价有机骨架(JUC-515)。JUC-515 被引入到毛细管柱中，并通过化学键合到毛细管柱的内壁上。通过多种表征结果，成功合成了 JUC-515 并将其引入到毛细管柱中。详细考察了缓冲溶液浓度、有机添加剂含量和缓冲溶液 pH 值对氟喹诺酮(FQs)分离的影响。JUC-515 涂覆的毛细管柱表现出良好的分离度(>1.5)和重现性。日内、日间、柱间和批间精密度的保留时间的相对标准偏差(RSD)分别小于 0.88%、2.45%、2.74%和 3.32%。日内、日间、柱间和批间精密度的峰面积的 RSD 分别小于 3.79%、4.31%、3.33%和 5.62%。JUC-515 涂覆的毛细管柱可使用不少于 150 次。结果表明，JUC-515 涂覆的毛细管柱具有良好的分离性能。此外，通过分离氟化β-苯丙氨酸类似物、β-苯丙氨酸和三氟甲基β-苯丙氨酸类似物，讨论了基于氟相互作用的分离机制。总之，JUC-515 作为毛细管电色谱的固定相具有良好的应用潜力。
