Citation: LIANG Qian, ZHOU Yuhong, ZHANG Zhilun, HUANG Mingxian. Preparation of a versatile polyethylene glycol-bonded stationary phase based on silica monolith particles and its application in multi-modal separation in high performance liquid chromatography[J]. Chinese Journal of Chromatography, ;2020, 38(8): 937-944. doi: 10.3724/SP.J.1123.2020.03036 shu

Preparation of a versatile polyethylene glycol-bonded stationary phase based on silica monolith particles and its application in multi-modal separation in high performance liquid chromatography

College of Science, University of Shanghai for Science and Technology, Shanghai 200093, China

Corresponding author: HUANG Mingxian, hmx@usst.edu.cn
Received Date: 31 March 2020

Fund Project: the Foundation of Hujiang (No. D15011).Science and Technology Commission of Shanghai Municipality (No. 14440502300)

Silica monolith particles with sizes of 2-5 μm and pore sizes of 20-60 nm were obtained by grinding, flotation, pseudomorphic transformation, and hydrothermal treatment of the silica monolith prepared by the sol-gel method. The pseudomorphic transformation was performed with a dual micellar templating system consisting of Capstone FS-66, a partially fluorinated anion surfactant, and cetyltrimethylammonium bromide (CTAB), a commonly used cation surfactant. Hydrothermal treatment with a sodium carbonate solution was adopted to further expand the pore size. Scanning electron microscopy (SEM) images and N₂ adsorption-desorption isotherm measurement results of the silica monolith particles before and after the treatments clearly demonstrated the changes in morphology caused by these treatments. Afterward, a long-chain polyethylene glycol (PEG) containing silane was bonded on the surface of the as-prepared particles, and the resulting products were characterized by elemental analysis and FT-IR spectroscopy analysis, and evaluated by high performance liquid chromatography (HPLC). Elemental analysis and thermogravimetric analysis (TGA) of the bonded stationary phase revealed that the bonding amount of PEG on the silica surface is about 8%. It has been shown that silica monolith particles can be treated and modified for the separation of proteins in size exclusion chromatography mode. It is also demonstrated that the bonded stationary phase can be used for the separation of ribonuclease A and lysozyme in hydrophobic interaction chromatography mode, and for the separation of highly polar compounds (picolinic acid, levodopa, melamine, and catechol) in hydrophilic interaction chromatography mode. The results indicate the versatility of the PEG-bonded stationary phase and its promising application to multi-modal separation in HPLC.
- high performance liquid chromatography (HPLC),
- pseudomorphic transformation,
- protein separation,
- multi-modal stationary phase,
- silica monolith particles
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