A kind of hydrophilic hybrid material and its preparation method and application
A hybrid material and hydrophilic technology, which is applied in the field of hydrophilic hybrid materials and its preparation, can solve the problems of insufficient selectivity of hydrophilic matrix, non-glycopeptides cannot be effectively removed, and glycopeptide mass spectrometry response is affected.
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[0039] The invention provides a preparation method of a hydrophilic hybrid material, comprising the following steps:
[0040] The template agent, swelling agent, hydrochloric acid solution and silicon source are mixed, and a hydrolysis polycondensation reaction is carried out to obtain a sol;
[0041] The sol is aged and then calcined 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 to carry out a grafting reaction to obtain vinyl chloride Functionalized hybrid mesoporous silicon material;
[0044] A modification solution containing glutathione, a photoinitiator and a solvent is mixed with the vinyl-functionalized hy...
Embodiment 1
[0074] Mix 30 mL of 2 mol / L hydrochloric acid solution, 0.5 g of template agent F127, 0.7 mL of swelling agent TMB and 2.21 mL of silicon source TEOS, and stir at 14 °C for 24 h to obtain a sol;
[0075] The obtained sol was put into a reaction kettle, aged at 130°C for 72h, filtered, dried and then calcined at 550°C for 5h to obtain mesoporous inorganic silicon material;
[0076] Disperse 0.5 g of the mesoporous inorganic silicon into 30 mL of a hydrochloric acid solution with a concentration of 15% 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, and react for 35 min, then add 0.25 mL of dimethylvinylchlorosilane, 55 The grafting reaction was carried out under magnetic stirring at ℃ for 12 h. After the reaction, the obtained product was washed ...
Embodiment 2
[0082] Mix 30 mL of 2 mol / L hydrochloric acid solution, 0.5 g of template agent F127, 0.7 mL of swelling agent TMB and 2.21 mL of silicon source TEOS, and stir at 14 °C for 24 h to obtain a sol;
[0083] The obtained sol was put into a reaction kettle, aged at 100°C for 24h, filtered, dried and calcined at 550°C for 5h to obtain mesoporous inorganic silicon material;
[0084] Disperse 0.5 g of the mesoporous inorganic silicon into 30 mL of a hydrochloric acid solution with a concentration of 15% 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 it up to 55 °C, add 0.4 mL of triethylamine under stirring, and then add 0.25 mL of dimethylvinylchlorosilane after reacting for 35 min. The grafting reaction was carried out under magnetic stirring at ℃ for 12 h. After the reaction, the obtained product was wash...
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