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Preparation method of estrogen specific nanometer silica gel surface molecule marking material

A technology of nano-silica gel and molecular imprinting, which is applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., and can solve the problems of decreased specific adsorption capacity of target molecules, morphological changes and movement of recognition sites, and incomplete removal of template molecules and other problems, to achieve the effect of simple and easy-to-obtain experimental equipment, easy to repeat, save time and reagents

Inactive Publication Date: 2010-01-06
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the study of molecularly imprinted polymers, due to the lack of rigidity of the organic cross-linked polymer materials used, the imprinted "holes" are prone to morphological changes and recognition site movement under the action of temperature and solvents, resulting in MIPs' inability to target molecules. Decreased specific adsorption capacity
On the other hand, in the synthesis process of molecularly imprinted polymers, because the template molecules are inside the polymer material, the removal of the template molecules is not complete, and there is generally a problem of 3-5% residues, which not only affects the adsorption capacity of MIPs, but also affects the adsorption capacity of MIPs. Severe interferences in trace analysis

Method used

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  • Preparation method of estrogen specific nanometer silica gel surface molecule marking material
  • Preparation method of estrogen specific nanometer silica gel surface molecule marking material
  • Preparation method of estrogen specific nanometer silica gel surface molecule marking material

Examples

Experimental program
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Effect test

Embodiment 1

[0028]At room temperature, 2ml of mass concentration of 25% ammonia and 2ml of double-distilled water were dissolved in 50ml of absolute ethanol, and 2.5ml of tetraethyl orthosilicate (TEOS) was added dropwise to the above mixture at a rate of 0.025ml. min -1 , 200r·min -1 The reaction was stirred for 24h. The obtained silica sol nanospheres were washed with absolute ethanol until neutral for later use.

[0029] Disperse 100mg of silica sol nanospheres with a particle size of 150nm in 50ml of toluene, add 2ml of γ-methacryloxypropyltrimethoxysilane, and react under nitrogen protection at 120°C for 16 hours. Toluene was washed 4 times by ultrasonic centrifugation at 16500r / min to obtain modified silica sol nanospheres;

[0030] Functional monomer methacrylic acid, template molecule estradiol, crosslinking agent ethylene glycol dimethacrylate and initiator azobisisobutyronitrile are dissolved in 50 milliliters of porogen toluene to make the above functional monomer The molar...

Embodiment 2

[0033] At room temperature, 2ml of mass concentration of 25% ammonia and 2ml of double-distilled water were dissolved in 50ml of absolute ethanol, and 2.5ml of tetraethyl orthosilicate (TEOS) was added dropwise to the above mixture at a rate of 0.025ml. min -1 , 200r·min -1 The reaction was stirred for 24h. The obtained silica sol nanospheres were washed with absolute ethanol until neutral for later use.

[0034] Disperse 50mg of silica sol nanospheres with a particle size of 150nm in 50ml of toluene, add 1ml of γ-methacryloxypropyl trimethoxysilane, and react under nitrogen protection at 120°C for 12 hours. Acetonitrile was ultrasonically washed three times at 16500r / min to obtain modified silica sol nanospheres;

[0035] Dissolve functional monomer methyl methacrylate, template molecule estradiol, crosslinking agent ethylene glycol dimethacrylate and initiator azobisisobutyronitrile in 50 milliliters of porogen acetone to make the above functional The molar concentration...

Embodiment 3

[0038] At room temperature, 2ml of mass concentration of 25% ammonia and 2ml of double-distilled water were dissolved in 50ml of absolute ethanol, and 2.5ml of tetraethyl orthosilicate (TEOS) was added dropwise to the above mixture at a rate of 0.025ml. min -1 , 200r·min -1 The reaction was stirred for 24h. The obtained silica sol nanospheres were washed with absolute ethanol until neutral for later use.

[0039] Disperse 150 mg of silica sol nanospheres with a particle size of 150 nm in 50 ml of toluene, add 2 ml of γ-methacryloxypropyl trimethoxysilane, and react under nitrogen protection at a high temperature of 120 ° C for 12 hours. Acetone was washed 5 times by ultrasonic centrifugation at 16500r / min to obtain modified silica sol nanospheres;

[0040] Functional monomer acrylamide, template molecule estradiol, crosslinking agent ethylene glycol dimethacrylate and initiator azobisisobutyronitrile are dissolved in 50 milliliters of porogen acetonitrile to make the above ...

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Abstract

The invention provides a preparation method of an estrogen specific nanometer silica gel surface molecule marking material, mainly comprising three steps of surface modification of a colloidal silica sol nanosphere, polyreaction and template molecule elution. The preparation method is easy to control, required experimental facilities are simple, and a prepared nanometer colloidal silica gel molecule marking polymer has the advantages of big specific surface, high molecule binding capacity, many recognition sites, favorable molecular recognition performance and the like. An estrogen molecule marking polymer material prepared by the invention not only can be used for various ideal adsorbents or coating materials of a solid-phase extraction technology, but also can be used for preparing molecule marking sensors and chips. The invention adopting the technology is of great importance in analyzing and researching various environmental pollutant residues.

Description

1. Technical field [0001] The invention belongs to the field of new material science, and particularly relates to a preparation method of a core-shell type estrogen-specific nano silica gel surface molecular imprinting material. 2. Background technology [0002] The problem of estrogen (ES) residues is currently the focus of attention and research by governments around the world. With the rapid development of the breeding industry, the abuse of estrogen in agricultural inputs (feed and feed additives, etc.) to promote animal growth is very common. The problem of estrogen residues in aquatic products, meat, eggs and milk is becoming more and more serious. Because ES has strong physiological activity, even at extremely low concentrations (mostly at the ppt-ppb level or lower) it will have a great impact on organisms. They interfere with the normal endocrine function of human beings, change the signal transmission process in the body during development and adulthood, and thus ...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/286B01J20/28B01J20/30B01J13/02C07J1/00
Inventor 周学敏马静袁丽华丁美娟王舒徐金慧吴晓丽李芸
Owner NANJING MEDICAL UNIV
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