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一种用于混合模式液相色谱的复合水凝胶改性硅胶固定相。

A composite hydrogel modified silica stationary phase for mixed‑mode liquid chromatography.

机构信息

Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China; University of Chinese Academy of Sciences, Beijing 100049, China.

Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China.

出版信息

J Chromatogr A. 2023 Sep 27;1707:464300. doi: 10.1016/j.chroma.2023.464300. Epub 2023 Aug 14.

Abstract

A novel composite hydrogel functionalized silica core-shell stationary phase was prepared by the surface modification of silica sphere. The successful synthesis of the new stationary phase (T-Sil@PAM/SA/UiO-66-NH) was proven by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD), etc. Due to the coexistence of amide, hydroxyl, long carbon chain and UiO-66-NH in composite hydrogel shell, the obtained stationary phase can be used in hydrophilic/reversed-phase liquid chromatography with multiple retention mechanisms, such as hydrophilic, hydrophobic and π - π interactions. The chromatographic retention behavior of T-Sil@PAM/SA/UiO-66-NH demonstrated that the new stationary phase showed excellent separation performance for both polar analytes (such as alkaloids, saccharides, etc.) and nonpolar analytes (such as substituted benzene and polycyclic aromatic hydrocarbon (PAHs), etc.). Furthermore, compared with NH column and commercial C18 column, the T-Sil@PAM/SA/UiO-66-NH exhibited a certain superiority. Moreover, the relative standard deviation (RSD) of PAHs' retention time with eight replicates consecutive elution was found to range from 0.03% to 0.17%. Therefore, the successful use of T-Sil@PAM/SA/UiO-66-NH in mixed‑mode liquid chromatography expanded the potential applications of hydrogels in the field of separation.

摘要

一种新型复合水凝胶功能化硅球核壳固定相通过硅球表面改性合成。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X 射线光电子能谱(XPS)和 X 射线衍射(XRD)等手段证明了新固定相(T-Sil@PAM/SA/UiO-66-NH)的成功合成。由于复合水凝胶壳中存在酰胺、羟基、长碳链和 UiO-66-NH,所得固定相可用作亲水/反相液相色谱,具有多种保留机制,如亲水、疏水和π-π相互作用。T-Sil@PAM/SA/UiO-66-NH 的色谱保留行为表明,新固定相对极性分析物(如生物碱、糖等)和非极性分析物(如取代苯和多环芳烃(PAHs)等)均表现出优异的分离性能。此外,与 NH 柱和商业 C18 柱相比,T-Sil@PAM/SA/UiO-66-NH 具有一定的优势。此外,8 次连续洗脱时 PAHs 保留时间的相对标准偏差(RSD)范围为 0.03%至 0.17%。因此,T-Sil@PAM/SA/UiO-66-NH 在混合模式液相色谱中的成功应用扩展了水凝胶在分离领域的潜在应用。

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