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Hydrophilic hybrid material, and preparation method and application thereof

A hybrid material and hydrophilic technology, applied in the field of hydrophilic hybrid material and its preparation, can solve the problems of insufficient selectivity of hydrophilic matrix, non-glycopeptide can not be effectively removed, affecting the response of glycopeptide mass spectrometry, etc.

Active Publication Date: 2021-08-31
BEIFANG UNIV OF NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current hydrophilic interaction chromatography still has the disadvantage of insufficient selectivity to the hydrophilic matrix, and non-glycopeptides cannot be effectively removed, which affects the mass spectrometry response of glycopeptides.

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  • Hydrophilic hybrid material, and preparation method and application thereof
  • Hydrophilic hybrid material, and preparation method and application thereof
  • Hydrophilic hybrid material, and preparation method and application thereof

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preparation example Construction

[0039] The invention provides a method for preparing a hydrophilic hybrid material, comprising the following steps:

[0040] Mix template agent, swelling agent, hydrochloric acid solution and silicon source, carry out hydrolysis polycondensation reaction, obtain sol;

[0041] aging and calcining the sol to obtain a mesoporous inorganic silicon material;

[0042] Acidifying the mesoporous inorganic silicon material to obtain an activated mesoporous inorganic silicon material;

[0043] After mixing the activated mesoporous inorganic silicon material with toluene, adding triethylamine to the obtained reaction system for the first heat preservation, adding dimethylvinylchlorosilane to the obtained reaction system for grafting reaction to obtain vinyl Functionalized hybrid mesoporous silicon materials;

[0044] The modifying liquid containing glutathione, photoinitiator and solvent is mixed with the vinyl functionalized hybrid mesoporous silicon material, and a click reaction is ...

Embodiment 1

[0074] Mix 30mL of 2mol / L hydrochloric acid solution, 0.5g of template agent F127, 0.7mL of swelling agent TMB and 2.21mL of silicon source TEOS, and stir at 14°C for 24h to obtain a sol;

[0075] The obtained sol was put into a reaction kettle, aged at 130°C for 72h, filtered, dried and calcined at 550°C for 5h to obtain a mesoporous inorganic silicon material;

[0076] Disperse 0.5 g of the mesoporous inorganic silicon into 30 mL of 15% hydrochloric acid solution by volume, reflux at 110° C. for 5 hours, filter, and wash to obtain an activated mesoporous inorganic silicon material;

[0077] Disperse 500 mg of the activated mesoporous inorganic silicon material in 15 mL of toluene, heat up to 55 ° C, add 0.4 mL of triethylamine under stirring conditions, and react for 35 minutes, then add 0.25 mL of dimethylvinylchlorosilane, 55 ℃ magnetic stirring for 12 hours to carry out the grafting reaction, after the reaction, the product obtained was washed with methanol to obtain a vi...

Embodiment 2

[0082] Mix 30mL of 2mol / L hydrochloric acid solution, 0.5g of template agent F127, 0.7mL of swelling agent TMB and 2.21mL of silicon source TEOS, and stir at 14°C for 24h to obtain a sol;

[0083] The obtained sol was put into a reaction kettle, aged at 100°C for 24 hours, filtered, dried and calcined at 550°C for 5 hours to obtain a mesoporous inorganic silicon material;

[0084] Disperse 0.5 g of the mesoporous inorganic silicon into 30 mL of 15% hydrochloric acid solution by volume, reflux at 110° C. for 5 hours, filter, and wash to obtain an activated mesoporous inorganic silicon material;

[0085] Disperse 500 mg of the activated mesoporous inorganic silicon material in 15 mL of toluene, heat up to 55 ° C, add 0.4 mL of triethylamine under stirring conditions, and react for 35 minutes, then add 0.25 mL of dimethylvinylchlorosilane, 55 ℃ magnetic stirring for 12 hours to carry out the grafting reaction, after the reaction, the product obtained was washed with methanol to o...

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Abstract

The invention belongs to the technical field of chromatographic stationary phase materials, and particularly relates to a hydrophilic hybrid material, and a preparation method and application thereof. The provided preparation method of the hydrophilic hybrid material comprises the following steps: firstly, synthesizing a mesoporous inorganic silicon material by adopting a template, a swelling agent and a silicon source through sol-gel reaction, acidifying, and then carrying out vinyl modification to obtain a vinyl functionalized hybrid mesoporous silicon material; and finally, bonding glutathione to the surface of the vinyl functionalized hybrid mesoporous silicon material by adopting a photo-initiated sulfydryl-alkene click reaction to obtain the hydrophilic hybrid material. The preparation method provided by the invention is simple to operate and easy to master, and large-scale expanded production can be realized; and the obtained hydrophilic hybrid material has excellent glycopeptide enrichment performance.

Description

technical field [0001] The invention belongs to the technical field of chromatographic stationary phase materials, in particular to a hydrophilic hybrid material and its preparation method and application. Background technique [0002] Protein glycosylation is a very important post-translational modification of proteins, and the glycoproteins formed by it are involved in many important life processes, such as immune response, information transmission, cell migration, etc. At present, the glycosylation analysis of proteins is usually realized by the combination of high-performance liquid chromatography (HPLC) and mass spectrometry (Massspectrometry, MS). Due to the coexistence of non-glycosylated peptides in proteins, the signal of glycopeptides is suppressed by non-glycosylated peptides during MS analysis. Therefore, prior to MS analysis, glycopeptides should be enriched. At present, the commonly used glycopeptide enrichment methods mainly include hydrazine chemical reacti...

Claims

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Application Information

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IPC IPC(8): B01D15/26G01N27/626G01N30/02
CPCB01D15/26G01N27/62G01N30/02
Inventor 龚波林田央
Owner BEIFANG UNIV OF NATITIES
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