Citation: LI Qiang, LI Yuan-Yuan, ZHU Nan, GAO Zhu-Xian, LI Tian-Jun, ZHOU Tong, MA Yu-Long. Preparation of Cyclodextrin Type Stationary Phase Based on Graphene Oxide and Its Application in Enantioseparation and Hydrophilic Chromatography. Chinese Journal of Analytical Chemistry, 2018, 46(9): 1455-1463. doi: 10.11895/j.issn.0253-3820.181337 [复制]
Preparation of Cyclodextrin Type Stationary Phase Based on Graphene Oxide and Its Application in Enantioseparation and Hydrophilic Chromatography
Graphene oxide (GO) was covalently coupled to the surface of amino silica gel by amide bond. β-Cyclodextrin (β-CD) was further chemically bonded to GO to prepare a novel chiral stationary phase. The resulting material was characterized by Fourier transform-infrared (FT-IR) spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), elemental analysis and thermogravimetric analysis (TGA). The separation of seven enantiomers was improved in varying degrees. At the same time, the stationary phase showed typical characteristics of hydrophilic interaction chromatography (HILIC), and four small nucleoside molecules were separated when the mobile phase was methanol-acetonitrile-water (45:45:10, V/V) in HILIC mode. In addition, the separation mechanism of the stationary phase was further explored by studying the effects of mobile phase composition, temperature, and pH on the analyte retention. The low temperature was conducive to the separation of analytes at 20-60℃. The addition of protonated solvent methanol significantly decreased retention time of the four analytes. The pH affected the degree of protonation of the analyte, the interaction among analytes and stationary phase, and retention time of analytes. The results showed that GO and β-CD played a synergistic effect in the chiral resolution of the chromatographic stationary phase. The retention of analytes in HILIC was attributed to their mixed-mode retention mechanisms including hydrophilic interactions, electrostatic interactions, hydrogen bonding, π-π stacking and so on.
Haginaka J. J. Chromatogr. B, 208, 875(1): 12-19
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