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

Inactive Publication Date: 2012-06-13
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, there have been related research reports on the modification of inorganic nanoparticles and electrodes by dendritic polymers, but there are still few reports on the combination of MIPs, and they are mainly limited to bulk polymerization on non-support surfaces. Based on dendritic nanostructures on the surface of magnetic nanoparticle materials MIPs research has not been reported

Method used

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  • Preparation method of magnetic beads of dendritic molecular imprinting polymer on surface of estrogenic nano silica gel
  • Preparation method of magnetic beads of dendritic molecular imprinting polymer on surface of estrogenic nano silica gel
  • Preparation method of magnetic beads of dendritic molecular imprinting polymer on surface of estrogenic nano silica gel

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a preparation method of magnetic beads of dendritic molecular imprinting polymer on a surface of estrogenic nano silica gel. The preparation method comprises the following steps of: carrying out cross-over study on a magnetic nano material and dendritic polymer study technology, a dummy template technology and a surface molecular-imprinted technology and then carrying out dendritic molecular imprinting design of the surface of the magnetic nano silica gel on low-abundance environmental estrogens; by means of the advantage of nano construction with rich functional groups provided by the dendritic molecules, preparing a controllable, ordered and dense molecular imprinting nuclear shell on the surface of a carrier material and synthesizing a new molecular imprinting material with high efficiency and strong magnetism. According to the preparation method, the problem of low efficiency of surface molecular imprinting is solved and the fast and sensitive detection of residual estrogens in foods and environments is realized.

Description

technical field [0001] The invention belongs to the technical field of new materials, and in particular relates to a preparation method of dendritic molecular imprinted polymer magnetic beads on the surface of estrogen nano-silica gel. Background technique [0002] At present, food safety has become a global focus, especially in my country. Such as the abuse of adrenergic receptor agonists, estrogens and antibiotics in the breeding industry, and the abuse of pesticides in the agricultural industry, the problem of harmful residues in food has become increasingly serious. Since humans are at the top of the food chain, they have become a gathering place for pollutants. Many residual drugs are extremely harmful to human health and ecological environment at very low levels. For example, environmental estrogens (EES) mostly at ppt-ppb or lower levels will have a great impact on organisms. The International Codex Alimentarius Commission (CAC), the European Union, the United State...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30
Inventor 周学敏王舒王若禹文婷婷薛诚汪洋洪俊丽李飞
Owner NANJING MEDICAL UNIV
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