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A "mercapto-gold" modified silica gel surface Sudan red molecular imprinting material, preparation method and application

A technology of molecular imprinting and imprinting materials, which is applied in the field of separation and analysis to achieve the effects of short elution time, simple adsorption operation, and favorable adsorption and elution.

Active Publication Date: 2018-07-17
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are no published patents and literature reports on the synthesis of Sudan red molecularly imprinted adsorption materials using "mercapto-gold" modified silica gel as a support.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Preparation of gold nanoparticles: sodium citrate reduction method, 100mL of 1mM HAuCl 4 The aqueous solution was heated to reflux until it boiled, and 10mL of 38.8mM sodium citrate aqueous solution was quickly added under vigorous stirring. After two minutes, the color of the solution changed from light yellow to wine red, kept boiling for 15 minutes, stopped heating, continued to stir to room temperature, and obtained Au nano Particles were stored at 4°C for later use.

[0048] (2) Silica gel activation treatment: put 4g of silica gel into a 100mL round bottom flask, then add 40mL of water and 40mL of concentrated hydrochloric acid, stir at a constant temperature of 105°C, condense and reflux for 24h. Finally, wash with deionized water until neutral, then wash with absolute ethanol 3-4 times, and dry in the air.

[0049] (3) Surface modification of silica gel: In a 25 mL three-neck round bottom flask, add 1 g of activated silica gel, disperse it in 10 mL of xylen...

Embodiment 2

[0056] (1) The preparation of gold nanoparticles is the same as in Example 1

[0057] (2) silica gel activation treatment is the same as embodiment 1

[0058] (3) Surface modification of silica gel: In a 25 mL three-neck round bottom flask, add 1.5 g of activated silica gel, disperse in 15 mL of xylene solution, and then add about 1 mL of silane coupling agent 3-mercaptopropane Trimethoxysilane (TMMPS) and 1 mL of 3-(methacryloyloxy)propyltrimethoxysilane (MPS) in N 2 Under the protection of magnetic stirring for reaction, reflux at 140°C for 12 hours, after cooling to room temperature, wash with toluene and ethanol in turn, and vacuum dry overnight at 60°C for later use, to obtain surface-modified silica gel. (4) Preparation of "mercapto-gold"@silica gel: Dilute the prepared gold sol to 210mL, take 210mg of the surface-modified silica colloid particles, add them to the gold sol one by one under magnetic stirring, and continue stirring 12h. The prepared "mercapto-gold"@sili...

Embodiment 3

[0064] (1) The preparation of gold nanoparticles is the same as in Example 1

[0065] (2) silica gel activation treatment is the same as embodiment 1

[0066] (3) Surface modification of silica gel: In a 25 mL three-neck round bottom flask, add 1 g of activated silica gel, disperse it in 10 mL of xylene solution, and then add about 1.5 mL of silane coupling agent 3-mercaptopropane Trimethoxysilane (TMMPS) and 1.5 mL of 3-(methacryloyloxy)propyltrimethoxysilane (MPS) in N 2 Under the protection of magnetic stirring for reaction, reflux at 140°C for 12 hours, after cooling to room temperature, wash with toluene and ethanol in turn, and vacuum dry overnight at 60°C for later use, to obtain surface-modified silica gel.

[0067] (4) Preparation of "mercapto-gold"@silica gel: Dilute the prepared gold sol to 250mL, take 250mg of the above-mentioned surface-modified silica colloid particles, add them to the gold sol one by one under magnetic stirring, and continue stirring 12h. The...

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Abstract

The invention discloses a 'mercapto-gold' modified silica-gel surface sudan molecularly imprinted material as well as a preparation method and application thereof. The preparation method comprises the following steps: performing surface modification on silica gel, so that the silica-gel surface contains mercapto groups; performing coordination bonding on gold nanoparticles and the mercapto groups so as to connect the gold nanoparticles and silica gel through the mercapto groups, consequently, forming 'mercapto-gold' @silica gel; taking sudan as a template molecule, adding the 'mercapto-gold' @silica gel, a cross-linking agent, an initiator and a pore-foaming agent for carrying out a polymerization reaction, and removing the template molecule, so as to obtain the 'mercapto-gold' modified silica-gel surface sudan molecularly imprinted material. The material prepared by the method has adsorptivity on the sudan molecule, and also has the advantages of high selectivity, specific recognition ability and the like.

Description

technical field [0001] The invention belongs to the technical field of separation and analysis, and relates to a preparation and application technology for molecularly imprinted adsorption materials, in particular to a "sulfhydryl-gold" modified silica gel surface Sudan red molecularly imprinted material, a preparation method and its application in food testing. Application Technology. Background technique [0002] Sudan red dye is often used as an industrial raw material and is widely used in the color enhancement of solvents, oils, waxes, gasoline, shoes, and floors. Sudan red mainly includes Ⅰ, Ⅱ, Ⅲ, and Ⅳ four types of azo oil-soluble industrial pigments. Sudan red B and Sudan red 7B are also often used as dyes and pigments. In 1995, the European Union (EU) and other countries have banned it from being used as a pigment in food. The International Agency for Research on Cancer listed Sudan Red Ⅰ, Ⅱ, Ⅲ and Ⅳ as animal carcinogens. The health supervision department of our ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F222/14C08J9/26B01J20/26B01J20/30B01D15/08G01N30/02
CPCB01D15/08B01J20/0233B01J20/103B01J20/268B01J2220/46C08F292/00C08J9/26C08J2201/0424C08J2351/10G01N30/02C08F222/102
Inventor 纪文华王晓赵恒强段文娟刘伟刘峰耿岩玲
Owner SHANDONG ANALYSIS & TEST CENT
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