Preparation method of magnetic beads of dendritic molecular imprinting polymer on surface of estrogenic nano silica gel
A nano-silica gel and molecular imprinting technology, applied in chemical instruments and methods, other chemical processes, etc., to achieve the effects of expanding adsorption capacity, improving imprinting efficiency, and effective separation and enrichment
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Embodiment 1
[0030] Example 1: Preparation of Fe 3 O 4 SiO 2 Nanoparticles
[0031] In a 250ml three-neck bottle, add 80ml deoxygenated deionized water, and add FeCl under nitrogen protection 3 ·6H 2 O (4.72g) and FeCl 2 ·4H 2 O (1.98g), stirring at 800rmp / min, 15ml of concentrated ammonia water and 1ml of oleic acid were added dropwise at 85°C, reacted for 1h, and black Fe was obtained by magnetic separation 3 O 4 Nanoparticles, washed with deionized water until neutral for later use;
[0032] Take 0.3gFe 3 O 4 Nanoparticles, uniformly dispersed in 30ml isopropanol and 2ml deionized water, keep stirring at 200rmp / min, add 2ml concentrated ammonia water and 5ml tetraethyl orthosilicate (TEOS), react at room temperature for 12h, magnetically separate Fe 3 O 4 SiO 2 Nanoparticles, washed with deionized water until neutral, and dried for later use;
Embodiment 2
[0034] a) Preparation of dendrimer-modified magnetic nanoparticles
[0035] (1): 0.3g Fe 3 O 4 SiO 2 The nanoparticles were dispersed in toluene, added with silane coupling agent, heated at 120 °C for 24 h under nitrogen protection, and subjected to conventional magnetic separation to obtain amino-terminated magnetic nanoparticles (MNPs-NH 2 ), the volume ratio of the silane coupling agent to toluene is 0.05:1 ml / ml;
[0036] (2): 0.3g MNPs-NH 2 The nanoparticles were dispersed in methanol, added with methyl acrylate (MA), heated at 50 °C for 30 h under nitrogen protection, and subjected to conventional magnetic separation to obtain end-ester modified dendritic magnetic nanoparticles (MNPs-OCH). 3 ), the molar ratio of the MA and the silane coupling agent added in (1) is 4:1;
[0037] (3): 0.3g MNPs-OCH 3 Nanoparticles were dispersed in N,N-dimethylformamide (DMF), and serinol and an appropriate amount of potassium carbonate were added at the same time. The reaction was ...
Embodiment 3
[0043] a) Preparation of dendrimer-modified magnetic nanoparticles
[0044] (1): the Fe prepared according to the method of Example 1 3 O 4 SiO 2 The nanoparticles were dispersed in toluene, added with silane coupling agent, heated at 140 °C for 18 h under nitrogen protection, and subjected to conventional magnetic separation to obtain magnetic nanoparticles modified with terminal amino groups (Magnetic Nanoparticles-NH). 2 , MNPs-NH 2 ), the volume ratio of the silane coupling agent and toluene is 0.06:1;
[0045] (2): 0.3g MNPs-NH 2 The nanoparticles were dispersed in methanol, added with methyl acrylate (MA), heated at 60 °C for 24 h under nitrogen protection, and subjected to conventional magnetic separation to obtain terminal ester modified dendritic magnetic nanoparticles (Magnetic Nanoparticles-OCH). 3 , MNPs-OCH 3 ), the molar ratio of the MA and the silane coupling agent added in (1) is 2:1; (3): MNPs-OCH 3 Nanoparticles were dispersed in N,N-dimethylformamide ...
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