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Method for preparing chromatographic stationary phase by using divinyl sulphone as template

A technology of divinyl sulfone and chromatographic stationary phase, which is applied in the field of chromatographic stationary phase, can solve the problems of affecting chromatographic separation performance, non-uniform bonded stationary phase surface, lengthy preparation route, etc., and achieve simple synthesis route and convenient and easy-to-obtain raw materials , the effect of high reaction efficiency

Active Publication Date: 2017-06-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0010] Aiming at the problem that the preparation route of high performance liquid chromatography stationary phase is lengthy and the multi-step reaction causes heterogeneous bonded stationary phase surface, thereby affecting the performance of chromatographic separation, the present invention provides a method for efficiently and simply preparing different types of chromatographic stationary phases , mainly involves divinyl sulfone activated silica gel stationary phase, which undergoes nucleophilic addition reaction with reagents containing sulfhydryl, amino or hydroxyl functional groups to prepare C8, C18, monosaccharides or polysaccharides, amino acids, biomacromolecules (lectin ) and other different types of chromatographic stationary phases;

Method used

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  • Method for preparing chromatographic stationary phase by using divinyl sulphone as template
  • Method for preparing chromatographic stationary phase by using divinyl sulphone as template
  • Method for preparing chromatographic stationary phase by using divinyl sulphone as template

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Embodiment 1

[0028] Under nitrogen protection, take 1.66 g of aminopropyltrimethoxysilane reagent, dissolve it in 20 mL of anhydrous tetrahydrofuran solution, stir it electromagnetically, add 1.027 g of divinyl sulfone reagent, adjust the pH value to 7.5 with triethylamine, stir at room temperature, and Phase chromatographic detection yields a divinylsulfone-bonded silane reagent. Under nitrogen protection, dissolve the dried silica gel (2.5g) in 30mL of anhydrous toluene, add divinylsulfone-bonded silane reagent, and dropwise add pyridine (6mmol, 480uL), heat to reflux, react for 12h, stop the reaction , cooled and suction-filtered, washed with anhydrous toluene, tetrahydrofuran, methanol, water, and methanol successively, dried and solidified at 80°C for 6 hours, and obtained divinyl sulfone-activated silica gel, named as SNDVS material.

[0029] Weigh 2.5g of the above dried SNDVS material, under nitrogen protection, dissolve in 10mL of anhydrous N,N-dimethylamide (DMF), add glucosamine...

Embodiment 2

[0031] With the operation process of embodiment 1, difference is:

[0032] Weigh 2.5g of the above dried SDVS material, under nitrogen protection, dissolve in 10mL of anhydrous methanol solvent, add glutathione (6mmol, 1.84g), triethylamine (6mmol, 840μL) and stir at room temperature for 10h, stop the reaction, reduce Filter under pressure, wash with 30mL methanol, 20mL water, and 20mL methanol successively, dry and solidify at 60°C for 6h to obtain SNDVS-GSH and store at room temperature.

[0033]

Embodiment 3

[0035] Under nitrogen protection, take 1.05 g of mercaptopropyltriethoxysilane reagent, dissolve it in 20 mL of anhydrous tetrahydrofuran solution, stir it electromagnetically, add 1.21 g of divinyl sulfone reagent, adjust the pH value to 7.5 with triethylamine, and stir at room temperature. Liquid chromatographic detection obtained divinyl sulfone modified mercaptosilane reagent. Under nitrogen protection, dissolve the dried silica gel (2.5g) in 30mL of anhydrous toluene, add divinylsulfone-bonded silane reagent, and dropwise add pyridine (6mmol, 480uL), heat to reflux, react for 12h, stop the reaction , cooled and suction-filtered, washed with anhydrous toluene, tetrahydrofuran, methanol, water, and methanol successively, dried and solidified at 80°C for 6 hours, and obtained divinyl sulfone-activated silica gel, which was named SSDVS material.

[0036] Weigh 2.5g of the above-mentioned dry SSDVS material, under nitrogen protection, dissolve in 10mL of anhydrous N, N-dimethy...

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Abstract

The invention relates to the technical field of preparation of silica gel chromatography materials, and discloses a method for preparing chromatographic stationary phase by using divinyl sulphone as a template. The method comprises the following steps: firstly, synthesizing a chemical reagent with divinyl sulphone silane, bonding the chemical reagent with the surface of a matrix, and performing nucleophilic addition with a reagent with sulfydryl, amino and hydroxyl. The method for preparing the chromatographic stationary phase, which is disclosed by the invention, is simple, rapid, gentle in condition, low in cost and high in bonding quantity. Due to adoption of divinyl sulphone, reactive chemical properties of electrons can be easily obtained from an external environment, the surface of silica gel can be modified, and an affine reagent comprises easily added sulfydryl, amino and hydroxyl at one end and amino acid containing C18, glycosyl, carboxyl, amino or zwitter ions simultaneously at the other end, and functional aglucon of biomacromolecules such as protein. The method for preparing a silica gel chromatographic material is concise in step, gentle in condition and high in aglucon bonding efficiency, a diversity of chromatographic materials can be prepared, and can be applied to high performance liquid chromatography separation.

Description

technical field [0001] The invention relates to the technical field of preparation of silica gel chromatographic materials. It is a silica gel-based silanization reagent synthesized with divinyl sulfone modification, which is prepared by nucleophilic addition reaction with reagents containing mercapto, amino and hydroxyl groups. Hydrophilic, zwitterionic, and biocompatible chromatographic stationary phases. Background technique [0002] High performance liquid chromatography is playing an increasingly important role in the field of biomedicine, especially in the effective purification and preparation of compounds and the separation and analysis of biological macromolecules such as peptides and proteins. [0003] There are various preparation methods of HPLC materials, and the types of obtained chromatographic materials have different separation properties due to different preparation methods. But there are also some problems in the preparation of chromatographic materials. ...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30B01D15/08
Inventor 梁鑫淼刘玉洁于龙付冬梅肖远胜薛兴亚
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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