Method for preparing magnetic molecule mark polymer for detecting PDE-5 inhibitor
A PDE-5, imprinting polymer technology, applied in the field of preparation of specific magnetic molecular imprinting polymers, can solve the problems of application limitation of magnetic nanoparticles, loss of magnetic properties of magnetic nanoparticles, etc., achieve easy surface functional design, prevent particles The effect of reunion and simple operation
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[0031] A preparation method of magnetic molecularly imprinted polymer for detecting PDE-5 inhibitor, comprising preparing Fe by conventional method 3 O 4 @SiO 2 Nanoparticles, the preparation steps are:
[0032] (1) Preparation of surface-grafted magnetic nanoparticles: Fe 3 O 4 @SiO 2 The nanoparticles are dispersed in toluene, a silane coupling agent is added, nitrogen is protected, the reaction is carried out at 120 ° C for 12-24 hours, and the product is ultrasonically washed to obtain magnetic nanoparticles grafted on the surface. The mass-volume ratio of the silane coupling agent to toluene is 0.06. ~0.09:1 mg / ml, the Fe 3 O 4 @SiO 2 The dosage of nanoparticles is 300mg;
[0033] (2) Preparation of core-shell magnetic nanoparticles / PDE-5 inhibitor composite spheres: Dissolve the surface-grafted magnetic nanoparticles obtained in step (1) together with functional monomers and PDE-5 inhibitor template molecules in toluene , the prepolymerization was carried out at...
Embodiment 1
[0042] Example 1: Preparation of Fe 3 O 4 @SiO 2 Nanoparticles
[0043] In a 250ml three-neck flask, add 80ml deoxygenated deionized water, keep the stirring speed at 800rmp / min, and add FeCl under nitrogen protection 2 ·4H 2 O (1.72 g) and FeCl 3 ·6H 2 O (4.72 g), 10 ml of concentrated ammonia water was added dropwise at 85°C, and reacted for 1 h to obtain Fe 3 O 4 Magnetic nanoparticles, washed with deionized water until neutral for later use;
[0044] Take 0.3gFe 3 O 4 Magnetic nanoparticles, dispersed in 50ml of isopropanol and 2ml of deionized water, kept stirring at 200rmp / min, added 2ml of ammonia water, added 5ml of TEOS at a speed of 20μl / min, reacted at room temperature for 12h to obtain Fe 3 O 4 @SiO 2 Nanoparticles; washed with deionized water until neutral for later use;
Embodiment 2
[0045] Example 2: Preparation of Sildenafil Fe 3 O 4 @SiO 2 -MIPs 1
[0046] like figure 1 As shown, 300 mg of the above Fe 3 O 4 @SiO 2 The nanoparticles were dispersed in 50 ml of toluene, 6 ml of γ-methacryloyloxytrimethoxysilane was added, and the reaction was carried out at 120 °C for 12 h under nitrogen protection. magnetic nanoparticles;
[0047] Disperse 40 mg of surface-grafted magnetic nanoparticles, template molecule sildenafil and functional monomer TFMAA in 50 ml of toluene, stir at room temperature for 1 h, then add crosslinking agent TMPTMA and initiator AIBN to make the above functional monomer, template molecule The molar concentrations of sildenafil, cross-linking agent TMPTMA and initiator AIBN in toluene were 20 mmol / L, 2 mmol / L, 20 mmol / L and 1 mmol / L, respectively, under nitrogen protection, the reaction was carried out at 50 °C for 6 h and 60 °C for 24 h. Finally, the temperature was raised to 85 °C for 6 h. Magnetic nanoparticles / sildenafil co...
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