Preparation method of liquid chromatographic stationary phrase and glycosyl-bonded stationary phrase

A liquid chromatography and stationary phase technology, applied in the field of glycosyl-bonded stationary phase and its preparation, can solve the problem that the glycosyl stationary phase has not been reported in literature, and achieves good hydrophilic and thiophilic properties, novel structure, and preparation. Simple and reliable process

Inactive Publication Date: 2016-07-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, glycosyl stationary phases based on thiol-alkene click chemistry have not been reported in the literature

Method used

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  • Preparation method of liquid chromatographic stationary phrase and glycosyl-bonded stationary phrase
  • Preparation method of liquid chromatographic stationary phrase and glycosyl-bonded stationary phrase
  • Preparation method of liquid chromatographic stationary phrase and glycosyl-bonded stationary phrase

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Weigh 10g spherical silica gel (particle size is 5μm, pore size is 10nm, specific surface area is 300m 2 / g), placed in a 250mL glass flask, added 150mL of 5% hydrochloric acid solution, heated to reflux for 12 hours, cooled to room temperature, filtered, washed with water until neutral, and dried at 150°C for 24 hours.

[0035] Put the dried silica gel in a 100mL three-neck glass bottle, add 50mL of toluene to the silica gel under the condition of passing dry nitrogen, stir evenly, then add 6mL of mercaptopropyltriethoxysilane dropwise, at 115°C The reaction was stirred at reflux for 16 hours. The reaction system was filtered, washed successively with methanol, water, tetrahydrofuran and methanol, and the product was dried at 80°C for 12 hours to obtain mercaptopropyl silica gel.

[0036] Put the dried mercaptopropyl silica gel in a 100mL three-neck glass bottle, add 30mL methanol and 30mL water, then add 10g alkenyl maltose and 0.4g azobisisobutyronitrile, stir at 65...

Embodiment 2

[0038] The difference from Example 1 is that glucose is used instead of maltose, and the glucose-bonded stationary phase can be obtained according to the synthesis steps of Example 1.

Embodiment 3

[0040] The difference from Example 1 is that mannose is used instead of maltose, and the mannose-bonded stationary phase can be obtained according to the synthesis steps of Example 1.

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Abstract

The invention relates to a liquid chromatographic stationary phrase, specifically to a preparation method of a liquid chromatographic stationary phrase and a glycosyl-bonded stationary phrase. A glycosyl-bonded silica gel stationary phase is prepared through a sulfydryl-alkene click chemical reaction free of heavy-metal catalysis. According to the method, sulfydryl groups are introduced on the surface of silica gel to prepare a sulfydryl silica gel intermediate; and through an addition reaction of sulfydryl groups and alkenyl groups, alkenyl saccharide molecules are bonded to the surface of silica gel. The method is free of heavy-metal catalysis, and therefore, the final product is free of heavy-metal residues, and adverse effects of heavy metals on performance of the product can be totally avoided. The preparation method is simple and reliable in process, mild in reaction condition, quite easy for massive preparation, and wide in application range. The glycosyl-bonded stationary phrase can be used as a separating material for hydrophilic interaction liquid chromatography, and is widely applied to selective separation of polar compounds, such as oligosaccharide, glycopeptide, glycoprotein, polypeptide, and nucleoside.

Description

technical field [0001] The invention relates to a liquid chromatography stationary phase, specifically a glycosyl bonded stationary phase and a preparation method thereof. Background technique [0002] Reverse-phase chromatography is currently the most widely used chromatographic separation mode. However, reversed-phase chromatography mainly relies on hydrophobic interactions to achieve sample retention and separation, and the retention of polar compounds is short and selectivity is insufficient. How to improve the retention and polar selectivity of polar compounds has become an important problem to be solved in the research and application of HPLC. Hydrophilic Interaction Chromatography (HILIC) is a polar stationary phase, acetonitrile / water is the mobile phase, and water is the strong elution solvent [Alpert, A.J.J.Chromatogr.1990,499,177]. In HILIC mode, the more polar the sample molecules, the longer the retention time. Therefore, HILIC can be used as a supplement to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30
Inventor 梁鑫淼郭志谋金高娃杨铎闫竞宇
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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