Preparation method of Clenbuterol surface molecularly imprinted material
A surface molecular imprinting and drying technology, which is applied in the preparation of surface molecular imprinting materials that can detect clenbuterol residues, and in the application field of surface molecular imprinting materials, can solve the problem of deep embedding of template molecules, low mechanical properties, and irregular shapes and other problems, to achieve the effect of short adsorption equilibrium time, short elution time and simple preparation process
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Embodiment 1
[0029] Weigh 30 g of silica gel (particle size 5 μm), add 150 mL of 10% methanesulfonic acid aqueous solution, stir at reflux temperature for 8 h, wash with distilled water until neutral, and dry at 65 °C for 12 h to obtain activated silica gel. Add 10g of activated silica gel to 400mL of water, add 10mL of 3-(methacryloyloxy)propyltrimethoxysilane, stir and react at 50°C for 24h, wash the product with water and ethanol, and dry at 65°C for 12h to obtain a double bond Composite silicone. Add 200mL of water and 3g of double-bonded silica gel into the flask, stir for 1h, then add 10mL of methacrylic acid, in N 2 Stir for 1 h under protection, add 1 mL of 20% ammonium persulfate solution, raise the temperature to 70°C, stir for graft polymerization, and obtain grafted particles after 24 h. Soxhlet extraction with ethanol for 24 hours, and then dried at 65°C for 12 hours before use. Take 50mL concentration as 1000mg·L -1 Clenbuterol aqueous solution, add 1g grafted particles PM...
Embodiment 2
[0036] Weigh 30 g of silica gel (particle size 40 μm), add 150 mL of 10% methanesulfonic acid aqueous solution, stir at reflux temperature for 8 h, wash with distilled water until neutral, and dry at 65 °C for 12 h to obtain activated silica gel. Add 5g of activated silica gel to 200mL of water, add 5mL of 3-(methacryloyloxy)propyltrimethoxysilane, stir and react at 40°C for 24h, wash the product with water and ethanol, and dry at 65°C for 12h to obtain a double bond Composite silicone. Add 200mL of water and 3g of double-bonded silica gel into the flask, stir for 1h, then add 10mL of methacrylic acid, in N 2 Stir for 1 h under protection, add 1 mL of 10% ammonium persulfate solution, raise the temperature to 70 ° C, stir for graft polymerization, and obtain grafted particles after 24 h. Soxhlet extraction with ethanol for 24 hours, and then dried at 65°C for 12 hours before use. Take 50mL concentration as 1000mg·L -1 Clenbuterol aqueous solution, add 1g grafted particles P...
Embodiment 3
[0038] Weigh 30g of silica gel (particle size 120μm), add 150mL of 20% hydrochloric acid aqueous solution, stir at reflux temperature for 8h, wash with distilled water until neutral, dry at 65°C for 12h to obtain activated silica gel. Add 5g of activated silica gel to 200mL of water, add 5mL of 3-(methacryloyloxy)propyltrimethoxysilane, stir and react at 60°C for 24h, wash the product with water and ethanol, and dry at 65°C for 12h to obtain a double bond Composite silicone. Add 200mL of water and 3g of double-bonded silica gel to the flask, stir for 1h, then add 10mL of methacrylic acid, stir for 1h under the protection of N2, add 1mL of 10% ammonium persulfate solution, heat up to 70°C, stir for graft polymerization After 24 hours of reaction, grafted particles were obtained. Soxhlet extraction with ethanol for 24 hours, and then dried at 65°C for 12 hours before use. Take 50mL of clenbuterol aqueous solution with a concentration of 500mg L-1, add 1g of grafted micropartic...
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