Optical intelligent silicagel surface molecularly imprinted microsphere and preparation method thereof

A surface molecular imprinting and molecular imprinting membrane technology, applied in the field of chemical engineering, can solve the problems of molecularly imprinted polymer molecular recognition and selectivity decline, template molecule target molecule processing capacity reduction, irregular shape, etc., to achieve mechanical strength and Good chemical stability, uniform particle size, and complete elution

Inactive Publication Date: 2014-07-02
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In recent years, there have been many research reports on the use of molecularly imprinted polymers in the active ingredients of natural products, but the molecularly imprinted polymer particles prepared by traditional bulk polymerization methods embed the template molecules too deeply or too tightly to be eluted, resulting in the template molecules Carryover affects analysis and molecularly imprinted polymer materials have reduced processing capacity for target molecules
Moreover, the prepared material has the disadvantages of irregular shape and poor dispersion after mechanical collection process, and the molecular recognition and selectivity of molecularly imprinted polymers will also decrease during the grinding process.

Method used

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  • Optical intelligent silicagel surface molecularly imprinted microsphere and preparation method thereof
  • Optical intelligent silicagel surface molecularly imprinted microsphere and preparation method thereof
  • Optical intelligent silicagel surface molecularly imprinted microsphere and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Synthesis of Functional Monomers of Azobenzene Derivatives

[0029]

[0030] 4-Aminoacetophenone and phenol were diazotized to synthesize 4-hydroxy-4'-acetyl azobenzene as raw materials. The specific synthesis steps were as follows: ①Put 2.7g of p-aminoacetophenone into a 100mL double-necked bottle , add 20mL of distilled water, then add 5.4mL of concentrated hydrochloric acid dropwise, and stir in an ice bath (0-5°C) for 10 minutes; dissolve 1.38g of sodium nitrite with 30mL of distilled water, and add dropwise to the double-necked flask Stir in an ice bath to generate diazonium salts. ②Dissolve 1.88g of phenol in 11mL of methanol, add it dropwise into the double-necked flask with a constant pressure separatory funnel, and stir for 2 hours. ③The reaction solution was neutralized to neutral with 5% sodium hydroxide solution, and a yellow solid was observed to form. Suction filtration, recrystallization with ethanol to obtain the product.

[0031] Step 2, p-Hydroxy...

Embodiment 2

[0034] Preparation of Molecularly Imprinted Microspheres on Silica Surface.

[0035] (1) Ethyl orthosilicate was stirred at a constant speed in ethanol solution containing ammonia water for 24 hours to synthesize silicon spheres with a particle size of 500 nm; the silicon spheres were stirred in aqueous nitric acid solution for 12 hours, filtered and washed, and vacuum-dried to constant weight.

[0036] The described ammonia solution concentration is 16.7%, and the nitric acid solution concentration is 50%.

[0037] Said uniform stirring, stirring speed: 500-600rpm; stirring temperature: 25°C.

[0038] For the washing, twice distilled water was used to wash three times.

[0039] The temperature of the vacuum drying is 110°C.

[0040] (2) Azobenzene derivatives are grafted onto the surface of activated silica spheres, and template molecules are added. The template molecules are chlorogenic acid in Eucommia leaves, oleanolic acid in privet leaves or dihydromyricetin in vine tea ...

Embodiment 3

[0048] one. Preparation of molecularly imprinted microspheres on the silica gel surface of chlorogenic acid:

[0049] (1) The molar ratio of chlorogenic acid, AIBN and EDMA is 0.2:0.2:2.5. Under dark conditions, 0.16g grafted silicon spheres, 0.2mmol chlorogenic acid were stirred in 15ml acetonitrile at 25°C for 2h, 0.2mmol AIBN, 2.5mmol EDMA were added to the reaction system, the temperature was raised to 60°C, and the reaction was carried out for 12h. (2) After the reaction, stir in DMSO at 60°C for 30 minutes, wash with 25ml of methanol for 3 times, and wash with 25ml of acetone for 2 times (remove the remaining dispersant, organic matter, etc.), each time for 10 minutes, ultrasonically oscillate during washing, and finally pass methanol : Soxhlet extraction with acetic acid (90:10) to further remove template molecules; (3) Dry the polymer silica gel from which template molecules have been removed to constant weight at 50°C in vacuum to obtain molecularly imprinted microsp...

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Abstract

The invention discloses an optical intelligent silicagel surface molecularly imprinted microsphere and a preparation method thereof. The method comprises the following steps of: arranging a layer of azobenzene derivative molecularly imprinted membrane on the surface of microsphere silicagel through graft polymerization; and grafting the surface of the microsphere silicagel through taking an azobenzene derivative as a functional monomer to obtain a product, adding template molecules and solvents with hydroxyls or carboxyls into the obtained product, and after the obtained mixture is polymerized through an initiator and a crosslinking agent, removing the template molecules through Soxhlet extraction, and drying so as to obtain the final product. Because a microsphere prepared through the graft polymerization in the method disclosed by invention combines the advantages of organic-inorganic materials, the microsphere is good in mechanical strength and chemical stability; and because the template molecules are completely removed, the microsphere is large in handling capacity and uniform in particle size, and can be used as an effective solid-phase extraction material, and therefore, the microsphere has a good application prospect.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a silica gel surface molecularly imprinted microsphere and a preparation method thereof. Background technique [0002] Natural product active ingredients refer to compounds with unique functions and biological activities extracted from renewable resources such as plants, animals, microorganisms, and various natural biomes, forests, grasslands, and aquatic organisms. The material basis of the body. Natural products have always been an important material source for human prevention and treatment of diseases. Not only are the drugs used in various traditional medicines in the world all natural sources, but about half of the chemical drugs widely used in modern medicine are also derived from natural sources. products and their derivatives or analogues. However, the natural product system is complex, and the content of active ingredients is low, so it is difficult to en...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F230/08C08J9/28B01J20/26B01J20/28B01J20/30
Inventor 钟世安李翠娥李晓静
Owner CENT SOUTH UNIV
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