Hollow molecularly imprinted polymers and solid phase extraction column and preparation method and application thereof
A solid-phase extraction column and molecularly imprinted technology, which is applied in the field of preparation of hollow molecularly imprinted solid-phase extraction columns, can solve the problems of uneven distribution of imprinted sites, unfavorable elution, and too deep "embedding" to improve adsorption Efficiency, obvious adsorption effect, obvious enrichment effect
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Embodiment 1
[0038] Preparation of a Boron Affinity Hollow Molecularly Imprinted Solid Phase Extraction Column
[0039] Weigh 1.00 mmol of monomeric methacrylic acid and 1.00 mmol of 3-aminophenylboronic acid respectively, mix the two evenly, and then dissolve them in 40 mL of acetonitrile, and stir at room temperature for 12 hours to obtain methacrylic acid surface-modified with nucleoside Phenylboronic acid structure with boron affinity;
[0040] Add template uridine to the above phenylboronic acid structure in an amount of 0.25mmol, and let stand at 0°C for 4h; add 5.00mmol of cross-linking agent ethylene glycol dimethacrylate, and then add initiator azobisisobutyronitrile 0.457mmol, through N2 10min, stirred at 40°C for 1h; then, added 200mg of mesoporous molecular sieve MCM-48 to the system, ultrasonicated for 15min, and passed through N 2 Seal, stir at 40°C for 2h, at 65°C for 18h, and at 80°C for 6h to prepare polymer microspheres;
[0041] After the polymer microspheres prepared ...
Embodiment 2
[0054] Preparation of a Boron Affinity Hollow Molecularly Imprinted Solid Phase Extraction Column
[0055] Weigh 1.00mmol of monomeric methacrylic acid and 2.00mmol of 3-aminophenylboronic acid, mix the two evenly, and then dissolve them in 50mL of acetonitrile, stir at room temperature for 16h, and obtain methacrylic acid surface-modified with nucleoside Phenylboronic acid structure with boron affinity;
[0056] Add template uridine to the above phenylboronic acid structure, the addition amount is 0.4mmol, and stand at 20°C for 4h; add 4mmol of crosslinking agent ethylene glycol dimethacrylate, and then add initiator azobisisobutyronitrile 0.061 mmol, thru N 2 20min, stirring at 60°C for 2h; after that, add 400mg of mesoporous molecular sieve MCM-48 to the system, sonicate for 20min, pass N 2 Seal, stir at 60°C for 3h, at 80°C for 20h, and at 100°C for 6h to prepare polymer microspheres;
[0057] After the polymer microspheres prepared above were washed with ethanol by suc...
Embodiment 3
[0070] Preparation of a Boron Affinity Hollow Molecularly Imprinted Solid Phase Extraction Column
[0071] Weigh 1.00mmol of monomeric methacrylic acid and 3.00mmol of 3-aminophenylboronic acid, mix the two evenly, and then dissolve them in 60mL of acetonitrile, stir at room temperature for 18h, and obtain methacrylic acid surface-modified with nucleoside Phenylboronic acid structure with boron affinity;
[0072] Add template uridine to the above phenylboronic acid structure in an amount of 0.25 mmol, and let it stand at 30°C for 6 hours; add 10 mmol of crosslinking agent ethylene glycol dimethacrylate, and then add 0.12 mmol of initiator azobisisobutyronitrile , through N 2 30min, stirring at 80°C for 1h; after that, add 600mg of mesoporous molecular sieve MCM-48 to the system, ultrasonic for 30min, pass N 2 Seal, stir at 70°C for 4h, at 80°C for 20h, and at 90°C for 8h to prepare polymer microspheres;
[0073] After the polymer microspheres prepared above were washed with...
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