Chitosan oligosaccharide hydrophilic interaction chromatography stationary phase and preparation method thereof
A technology of hydrophilic chromatography and chitosan oligosaccharides, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve problems affecting separation, irreversible adsorption of silica gel columns, etc., and achieve high-efficiency separation, simple structure, and high selectivity and the effect
A technology of hydrophilic chromatography and chitosan oligosaccharides, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve problems affecting separation, irreversible adsorption of silica gel columns, etc., and achieve high-efficiency separation, simple structure, and high selectivity and the effect
CN101757897AInactive
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[0048] An embodiment comprises the following steps:
[0049] (1) Preparation of Azidesulfonylimidazole Hydrochloride
[0050] Add 50mmol sulfonyl chloride (about 4mL) dropwise to 50mmol NaN in an ice-water bath 3 (about 3.2 g) in 100 mL of anhydrous MeCN suspension, the mixture was stirred overnight at room temperature;
[0051] Slowly add 100mmol imidazole (about 6.8g) into the above system under an ice-water bath, and stir the obtained emulsion at room temperature overnight;
[0052] Add 75mL of ethyl acetate to the mixture to dilute, successively wash with 2×75mL H 2 O, 2 x 120mL saturated NaHCO 3 The solution was extracted, and the organic phase was added with anhydrous Na 2 SO 4 Drying, suction filtration, and salt formation: Add HCl in EtOH solution (5.4mL acetyl chloride was added dropwise to 19mL EtOH under ice-water bath) to the above organic phase, a white solid was precipitated, suction filtration, washing with ethyl acetate, Obtain solid azidesulfonylimidazol...
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Abstract
The invention relates to a preparation method for a chitosan oligosaccharide hydrophilic interaction chromatography stationary phase. The click chemistry is adopted as a bonding reaction method for bonding chitosan oligosaccharide, firstly, terminal alkynyl is introduced on the surface of silica gel, secondly, the following solvents of water and methanol or the mixture of the solvents is taken as the reaction solvent, and then the chitosan oligosaccharide modified with azido group is bonded to the surface of the silica gel to obtain the chitosan oligosaccharide hydrophilic interaction chromatography stationary phase; the chitosan oligosaccharide is adopted as the polarity functional group with simple structure, and the chitosan oligosaccharide taken as the polarity stationary phase can realize the highly effective separation to the strongly polar compounds under the hydrophilic interaction liquid chromatogram mode; the chitosan oligosaccharide taken as the functional group has stable property, the surface structure does not change due to the change of pH, and the chitosan oligosaccharide is not liable to react with the solute molecule; and the click chemistry is adopted as the bonding reaction method, therefore, the purpose of immobilization with high selectivity and high transformation ratio can be achieved under the mild conditions.
Description
【Technical field】 [0001] The invention relates to liquid chromatography stationary phase technology, specifically, a method for preparing a hydrophilic chromatography stationary phase using "link chemistry" (click chemistry) as a bonding method to bond chitosan oligosaccharides. 【technical background】 [0002] Hydrophilic Interaction Chromatography (HILIC for short) is a chromatographic technique developed in recent years for the separation of strongly polar components. The chromatographic mode with low-concentration aqueous solution as the mobile phase solves the problem that traditional reversed-phase chromatography hydrophobic stationary phases, such as C18, C8, etc., have weak retention of strong polar compounds, such as oligosaccharides, glycosides, and strong polar oligopeptides. Even unreserved questions. Hydrophilic interaction chromatography has been used to separate polar compounds such as amino acids, peptides and sugars, which have been reported in the literatur...
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- IPC
- B01J20/288
- CPC
- B01D15/305
- Inventors
- 梁鑫淼; 黄洪雪