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Method for preparing bisphenol A nanometer silicon gel carrier surface molecule print solid phase extraction filling

A nano-silica gel and carrier surface technology, applied in chemical instruments and methods, and other chemical processes, can solve problems such as memory residue and template elution difficulties, and achieve many imprinting sites, easy chemical structure modification and design, and high rigidity and stability effects

Inactive Publication Date: 2009-09-09
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the shortcomings of difficult template elution and memory residue in the prior art, the present invention provides a preparation method for molecularly imprinted solid-phase extraction filler on the surface of bisphenol A nano-silica gel carrier, which has the advantages of easy binding of template molecules, easy elution, and difficult Leakage has the advantages of high selectivity and high extraction efficiency for the phenolic environmental hormone BPA

Method used

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  • Method for preparing bisphenol A nanometer silicon gel carrier surface molecule print solid phase extraction filling
  • Method for preparing bisphenol A nanometer silicon gel carrier surface molecule print solid phase extraction filling
  • Method for preparing bisphenol A nanometer silicon gel carrier surface molecule print solid phase extraction filling

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preparation example Construction

[0022] Preparation of nanoscale silica:

[0023] Preparation of 100nm silica

[0024] Add 100ml of absolute ethanol to a 250ml round bottom flask, then add 3.85ml of concentrated ammonia water and 1.8ml of distilled water, stir at 500r / min for 3min, then add 3.6ml of tetraethyl orthosilicate dropwise for 15-20h, then centrifuge at 10000r / min , discard the supernatant, and add absolute ethanol to ultrasonically wash three times to obtain 100nm silica pellets.

[0025] Preparation of 200nm silica

[0026] Add 88ml of absolute ethanol to a 250ml round bottom flask, then add 11.9ml of concentrated ammonia water, stir at 500r / min for 3min, then add 3.6ml of tetraethyl orthosilicate drop by drop, react for 15-20h, centrifuge at 10000r / min, discard After cleaning with anhydrous ethanol and ultrasonic cleaning three times, 200nm silica pellets were obtained.

[0027] Preparation of 400nm silica

[0028] Add 44ml of absolute ethanol to a 100ml round bottom flask, then add 5.95ml of...

Embodiment 1

[0030] Disperse 0.1g of silica pellets with a particle size of 100nm in 20ml of toluene, add 6.6mmol of vinyltrimethoxysilane, catalyze the reaction with 1ml of concentrated ammonia water for 16h, centrifuge at 10000r / min, and wash the lower solid with toluene for 2 times, surface-grafted nano-silica spheres were obtained. Then disperse the surface-grafted nano-silica spheres in 20ml of toluene, then add 0.25mmol template molecule tetrabromobisphenol A and 2mmol functional monomer 4-vinylpyridine, after ultrasonication for 3 minutes, add 13.2mmol cross-linked Combine vinyltrimethoxysilane and 80mg initiator azobisisobutyronitrile, ultrasonically dissolve and disperse for 1min, vacuumize and fill with nitrogen, and react with stirring at 500r / min in an oil bath at 70°C for 24h. After the reaction is completed, centrifuge, and stir and wash the lower layer of solids with a mixture of methanol and acetic acid at a volume ratio of 9:1 for 12 hours, then centrifuge it, discard the ...

Embodiment 2

[0032] Disperse 0.2g of silica pellets with a particle size of 200nm in 40ml of toluene, add 13.2mmol of vinyltrimethoxysilane, catalyze the reaction with 2ml of concentrated ammonia water for 20h, centrifuge at 10,000r / min, and wash the lower solid with toluene for 3 times, surface-grafted nano-silica spheres were obtained. Then disperse the surface-grafted nano-silica spheres in 20ml toluene, then add 0.5mmol template molecule tetrabromobisphenol A and 4mmol functional monomer 4-vinylpyridine, after ultrasonication for 3 minutes, add 26.4mmol cross-linked Combine vinyltrimethoxysilane and 80 mg initiator azobisisobutyronitrile, ultrasonicate for 1 min, vacuumize and fill with nitrogen, and react with stirring at a speed of 500 r / min for 24 h in an oil bath at 70°C. After the reaction is completed, centrifuge, and stir and wash the lower layer of solids with a mixture of methanol and acetic acid at a volume ratio of 9:1 for 12 hours, then centrifuge it, discard the supernatan...

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Abstract

The invention discloses a method for preparing bisphenol A nanometer silicon gel carrier surface molecule print solid phase extraction filling. Firstly, silanizing agent containing double bonds is grafted on the surfaces of nanometer silicon dioxide beads; secondly, template molecules, functional monomers and crosslinking agents are added into toluene solution containing proper grafted nanometer silicon and catalytic amount evocating agent according to a certain proportion and stirred for polyreaction at temperature of 60 to 70 DEG C and for 15 to 24 hours to generate light-yellow powdery polymer; and finally, templates are eluted from the polymer, and the bisphenol A nanometer silicon gel carrier surface molecule print solid phase extraction filling which has high special selectivity to bisphenol A is obtained. Because the invention adopts the tetrabromobisphenol A and biphenyl diphenol which are analogues of target molecule BPA of as templates, the problem of template leakage is solved. The prepared bisphenol A nanometer silicon gel carrier surface molecule print solid phase extraction filling has high special selectivity to bisphenol A, can collect bisphenol A molecules in trace amount of water sample, and has high recovery ratio and good reproducibility.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, and specifically synthesizes a macromolecular material with a specific recognition ability for bisphenol A molecules by using the surface molecular imprinting technology of nano silica gel carrier. Background technique [0002] Bisphenol A (BPA) is an environmental hormone, also known as an extrinsic endocrine disrupting chemical substance, which is a trace chemical substance released into the environment due to human production and activities. They usually enter organisms through the food chain, mimic or block the effects of endogenous estrogen, interfere with the synthesis and metabolism of endogenous hormones or their receptors, cause endocrine disorders, endanger the reproductive function of organisms or cause malignant tumors. Therefore, bisphenol A research is related to the healthy reproduction, survival and development of human beings. Since most bisphenol A samples have complex m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/30C08F292/00C08J9/26
Inventor 胡琴赵文慧魏芳弟朱荣蔡政李飞
Owner NANJING MEDICAL UNIV
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