Cyano-modified molecular cage silica gel stationary phase: Multi-functional chromatographic performance by high-performance liquid chromatography

IF 3.8 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS
Zhen Li , Zixia Tang , Junxiang Cao , Xingyu Yao , Jia Chen , Kang Xu , Ruixue Sun , Xiaoyi Shao , Mei Lv , Litao Wang
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Abstract

This study successfully prepared different loading levels of cyano-functionalized RCC3 molecular cage silica gel stationary phase (RCC3-CN@SiO2) through aldehyde-amine condensation reaction and subsequent modification strategies. Fourier transform infrared spectroscopy, thermogravimetric analysis, nitrogen adsorption-desorption, and scanning electron microscopy confirmed the successful synthesis of RCC3-CN@SiO2 chromatographic stationary phase. The research demonstrates that due to hydrophobic/hydrophilic interactions, π-π interactions, hydrogen bonding, and size-selective porous structure, the stationary phase effectively separates moderately polar and weakly polar compounds in reversed-phase liquid chromatography (RPLC) mode, exhibiting hydrophobic selectivity comparable to the commercial DaisoC18-RP columns. Additionally, the tertiary amine and cyanogen groups on the molecular cage surface enhance the interaction with polar compounds, successfully separating nucleosides, sulfonamides, amino acids, and sugars in hydrophilic interaction chromatography (HILIC) mode. Further applications in the separation analysis of acidic drugs, alkaline drugs, cinnamic acid natural products, and chiral compounds demonstrate the multifunctional chromatographic capabilities for diverse compound types. Compared to Unitary Diol commercial columns, the prepared stationary phase showed significant advantages in wide polarity range separation performance. Moreover, through nucleoside compound separation mode switching analysis, RCC3-CN@SiO2 stationary phase further validates its favorable performance in both RPLC and HILIC modes, demonstrating extensive potential applications in the field of analytical chemistry. Importantly, the stationary phase exhibits efficient separation of nucleoside compounds in pure water systems, aligning with the principles of green analysis.
氰基改性分子笼硅胶固定相:高效液相色谱的多功能色谱性能
本研究通过醛胺缩合反应及后续改性策略,成功制备了不同负载水平的氰基功能化 RCC3 分子笼硅胶固定相(RCC3-CN@SiO2)。傅立叶变换红外光谱、热重分析、氮吸附-解吸和扫描电子显微镜证实了 RCC3-CN@SiO2 色谱固定相的成功合成。研究表明,由于疏水/亲水相互作用、π-π相互作用、氢键和尺寸选择性多孔结构,该固定相在反相液相色谱(RPLC)模式下可有效分离中等极性和弱极性化合物,其疏水选择性与商用 DaisoC18-RP 色谱柱相当。此外,分子笼表面的叔胺和氰基还能增强与极性化合物的相互作用,从而在亲水相互作用色谱(HILIC)模式下成功分离核苷、磺胺、氨基酸和糖类。在酸性药物、碱性药物、肉桂酸天然产品和手性化合物的分离分析中的进一步应用,证明了该色谱柱具有针对不同化合物类型的多功能色谱能力。与 Unitary Diol 商用色谱柱相比,制备的固定相在宽极性范围分离性能方面具有显著优势。此外,通过核苷化合物分离模式切换分析,RCC3-CN@SiO2 固定相进一步验证了其在 RPLC 和 HILIC 两种模式下的良好性能,展示了其在分析化学领域的广泛应用潜力。重要的是,该固定相能在纯水体系中高效分离核苷化合物,符合绿色分析的原则。
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来源期刊
Journal of Chromatography A
Journal of Chromatography A 化学-分析化学
CiteScore
7.90
自引率
14.60%
发文量
742
审稿时长
45 days
期刊介绍: The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.
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