Preparation method of glibenclamide magnetic nano silica gel surface polyamide-amide dendritic molecular imprinting polymer

A magnetic nano, amine dendritic technology, applied in the direction of chemical instruments and methods, other chemical processes, etc., can solve problems such as no breakthrough progress, and achieve the effect of economical preparation and application, simple synthesis method, and high effective utilization rate

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

[0005] With the continuous deepening of the research on MIPs on the surface of nanomaterials, the deep-seated issue of the imprinting efficiency of the core-shell layer of MIPs ha

Method used

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  • Preparation method of glibenclamide magnetic nano silica gel surface polyamide-amide dendritic molecular imprinting polymer
  • Preparation method of glibenclamide magnetic nano silica gel surface polyamide-amide dendritic molecular imprinting polymer
  • Preparation method of glibenclamide magnetic nano silica gel surface polyamide-amide dendritic molecular imprinting polymer

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Experimental program
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Effect test

Embodiment 1

[0029] Preparation of Fe 3 o 4 SiO 2 Nanoparticles

[0030] In a 250mL three-necked bottle, add 80mL deoxygenated deionized water, add FeCl under nitrogen protection 3 ·6H 2 O (4.72g) and FeCl 2 4H 2 O (1.98g), stirred 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;

[0031] Take 0.3g Fe 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, and magnetically separate Fe 3 o 4 SiO 2 Nanoparticles, washed with deionized water until neutral, dried for later use;

Embodiment 2

[0033] 1. Fe 3 o 4 SiO 2 Nanoparticle functionalized grafting:

[0034] Get 0.1g Fe that prepares according to embodiment 1 method 3 o 4 SiO 2 Nanoparticles, dispersed in 50mL toluene, add 1mL γ-aminopropyltriethoxysilane and 1mL γ-methacryloxypropyltrimethoxysilane, heat and reflux at 60°C for 24-36h under nitrogen, magnetically separate, and then Wash with toluene and methanol, and dry in vacuum to obtain functionalized Fe 3 o 4 SiO 2 Nanoparticles;

[0035] 2. Preparation of polyamide-amine dendrimers on the surface of magnetic nano-silica gel:

[0036] Fe 3 o 4 SiO 2 Nanoparticles, add 50mL methanol and 0.75mL methyl acrylate (MA), under the protection of nitrogen, heat and reflux for 24 ~ 36h, magnetically separate, wash with methanol, and dry in vacuum; then, add 50mL methanol and 0.60mL ethylenediamine ( EDA), under the protection of nitrogen, heated to reflux for 24 to 36 hours, magnetically separated, washed with methanol, dried in vacuum, repeated the ab...

Embodiment 3

[0043] 1. Fe 3 o 4 SiO 2 Nanoparticle functionalized grafting:

[0044] Get 0.1g Fe that prepares according to embodiment 1 method 3 o 4 SiO 2 Nanoparticles, dispersed in 50mL of toluene, add 1mL of γ-aminopropyltriethoxysilane and 3mL of γ-methacryloxypropyltrimethoxysilane, heat and reflux at 50°C under nitrogen for 24-36h, magnetically separate, sequentially Wash with toluene and methanol, and dry in vacuum to obtain functionalized Fe 3 o 4 SiO 2 Nanoparticles;

[0045] 2. Preparation of polyamide-amine dendrimers on the surface of magnetic nano-silica gel:

[0046] Fe 3 o 4 SiO 2 Nanoparticles, add 50mL methanol and 0.75mL methyl acrylate (MA), under the protection of nitrogen, heat and reflux for 24 ~ 36h, magnetically separate, wash with methanol, and dry in vacuum; then, add 50mL methanol and 0.60mL ethylenediamine ( EDA), under the protection of nitrogen, heated to reflux for 24 to 36 hours, magnetically separated, washed with methanol, and vacuum-dried to...

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Abstract

The invention discloses a preparation method of a glibenclamide magnetic nano silica gel surface polyamide-amide (PAMAM) dendritical molecular imprinting polymer, which comprises the following steps of: (1) dendritically and functionally grafting Fe3O4@SiO2; (2) placing a template molecule, a functional monomer and the functionally grafted Fe3O4@SiO2 in a porogenic agent for prepolymerization, adding a cross-linking agent and an initiating agent, and polymerizing the materials under the reflux of nitrogen; and (3) eluting the polymer to remove a template molecule using a methanol hydrochloricacid solution. The glibenclamide magnetic nano silica gel surface polyamide-amide dendritical molecular imprinting polymer prepared in the invention has specific recognition capability on glibenclamide and drugs with similar structure thereof. The glibenclamide magnetic nano silica gel surface polyamide-amide dendritical molecular imprinting polymer is used together with chromatography and can beused for the fast separation, enrichment and measurement of glibenclamide illegally added into health foods and drugs.

Description

technical field [0001] The invention belongs to the technical field of new materials, and in particular relates to a preparation method of a polyamide-amine dendritic molecule imprinted polymer on the surface of glibenclamide magnetic nano silica gel. Background technique [0002] At present, food and drug safety has become a global focus. In particular, the illegal act of adding chemical drugs to health food and traditional Chinese medicine preparations to increase their efficacy has aroused great concern from the whole society because of its more concealed, deceptive and harmful effects. Liburide, Glimepiride, and Glipizide. [0003] Diabetes is one of the most common diseases in the world. There are many hypoglycemic drugs used to treat diabetes in the market, among which Glibenclamide (also known as glibenclamide) is the second generation of sulfonylurea oral hypoglycemic drugs, and its curative effect is characterized by strong hypoglycemic effect, Effects appear in ...

Claims

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Application Information

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IPC IPC(8): B01J20/283B01J20/30
Inventor 周学敏王若禹王舒文婷婷汪洋薛诚洪俊丽
Owner NANJING MEDICAL UNIV
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