Organo-silica hybrid monolithic column modified with 4,5-imidazoledicarboxylic acid and its application
A hybrid technology of imidazole dicarboxylic acid and silica gel is applied in the field of chromatographic fillers, which can solve the problems of complex preparation methods, inability to achieve good separation of polar compounds, and unenvironmental protection, and achieve the effects of simple preparation methods and green preparation methods.
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Embodiment 1
[0031] Example 1 Preparation and Application of 4,5-Imidazoledicarboxylic Acid Modified Organic Silica-Hybrid Monolithic Column
[0032] Proceed as follows:
[0033] ①Pretreatment of the capillary: Take a fused silica capillary with a length of 40 cm, wash it with methanol and water for 20 min, and then wash it with 1 mol / L NaOH solution, water, and 1 mol / L hydrochloric acid for 2.0 h, respectively. 0.5 h, 1.5 h, and then rinse the capillary with water for 20 min until the pH of the flushed liquid is neutral, and finally rinse with methanol for 20 min, and dry it with nitrogen at 120 °C for use;
[0034] ② Dissolve 240 mg polyethylene glycol (PEG, M=10 000) in a glass bottle filled with 2.5 mL 0.01 M acetic acid aqueous solution, and then slowly add 0.9 mL tetramethoxysilane (TMOS) and 0.3 mL Chloropropyltrimethoxysilane (CPTMS), the mixed solution was reacted for 4 h under ice-water bath conditions until a uniform and transparent sol was formed, and then the sol was ultrason...
Embodiment 2
[0037] Example 2 Preparation and application of 4,5-imidazoledicarboxylic acid modified organo-silica hybrid monolithic column
[0038] Proceed as follows:
[0039] ①Pretreatment of the capillary: Take a fused silica capillary with a length of 45 cm, wash it with methanol and water for 20 min, and then wash it with 1 mol / L NaOH solution, water, and 1 mol / L hydrochloric acid for 2.0 h, respectively. 0.5 h, 1.5 h, and then rinse the capillary with water for 20 min until the pH of the flushed liquid is neutral, and finally rinse with methanol for 20 min, and dry it with nitrogen at 120 °C for use;
[0040] ② Dissolve 240 mg polyethylene glycol (PEG, M=10 000) in a glass bottle filled with 2.5 mL 0.01 M acetic acid aqueous solution, and then slowly add 0.9 mL tetramethoxysilane (TMOS) and 0.3 mL Chloropropyltrimethoxysilane (CPTMS), the mixed solution was reacted for 4 h under ice-water bath conditions until a uniform and transparent sol was formed, and then the sol was ultrasoni...
Embodiment 3
[0043] Example 3 Preparation and application of organo-silica hybrid monolithic column modified with 4,5-imidazoledicarboxylic acid
[0044] Proceed as follows:
[0045] ①Pretreatment of the capillary: Take a fused silica capillary with a length of 50 cm, wash it with methanol and water for 20 min, and then wash it with 1 mol / L NaOH solution, water, and 1 mol / L hydrochloric acid for 2.0 h, respectively. 0.5 h, 1.5 h, and then rinse the capillary with water for 20 min until the pH of the flushed liquid is neutral, and finally rinse with methanol for 20 min, and dry it with nitrogen at 120 °C for use;
[0046] ② Dissolve 240 mg polyethylene glycol (PEG, M=10 000) in a glass bottle filled with 2.5 mL 0.01 M acetic acid aqueous solution, and then slowly add 0.9 mL tetramethoxysilane (TMOS) and 0.3 mL Chloropropyltrimethoxysilane (CPTMS), the mixed solution was reacted for 4 h under ice-water bath conditions until a uniform and transparent sol was formed, and then the sol was ultr...
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