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Polyhydrogen bond melamine core-shell molecularly imprinted polymer and preparation method thereof

A technology of hydrogen bond melamine and molecular imprinting, applied in the direction of material electrochemical variables, etc., can solve the problems of pretreatment and detection limit not meeting the requirements of melamine detection, cumbersome experimental steps, limited application, etc., to achieve good selection and enrichment The effect of adsorption, improving specific recognition ability, good reproducibility and stability

Active Publication Date: 2016-05-11
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The early industrial detection methods of melamine were gravimetric method and potentiometric titration method. The pretreatment and detection limit of these methods could not meet the national requirements for the detection of melamine in food. At the same time, these methods took a long time and the experimental steps were cumbersome. limit its use

Method used

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  • Polyhydrogen bond melamine core-shell molecularly imprinted polymer and preparation method thereof
  • Polyhydrogen bond melamine core-shell molecularly imprinted polymer and preparation method thereof
  • Polyhydrogen bond melamine core-shell molecularly imprinted polymer and preparation method thereof

Examples

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Effect test

Embodiment 1

[0027] The mixed solution containing 5.4 ml TEOS and 4.6 ml ethanol was added to the mixed solution containing 1 mol / L ammonia water and 5 mol / L water, and reacted for 2 hours under mechanical stirring to obtain monodisperse SiO 2 nanoparticles. Such as figure 2 shown. On this basis, the synthesis of melamine molecularly imprinted core-shell nanoparticles: the resulting SiO 2 Weigh 0.3 grams of nanoparticles and disperse them in anhydrous toluene, add 7 milliliters of 3-aminopropyltriethoxysilane (APTES) to heat and reflux for 12 hours, wash the product with ethanol for 3 times, and redisperse the product to 50 milliliters In ethanol, add 1 milliliter of glutaraldehyde and stir for 12 hours, further modification (the morphology of the product obtained is as follows image 3 shown), then the resulting product was cleaned and dispersed in methanol, weighed 0.168 g of 6-aminouracil, heated and dissolved with 20 ml of dimethyl sulfoxide, added to the above flask, added an appr...

Embodiment 2

[0029] Add the mixed solution containing 6.0 ml TEOS and 4.0 ml ethanol to the mixed solution containing 0.7 mol / L ammonia water and 4 mol / L water, and react under mechanical stirring for 2 hours to obtain monodisperse SiO 2 nanoparticles. On this basis, the synthesis of melamine molecularly imprinted core-shell nanoparticles (specific conditions and amount of materials): Weigh 0.127 grams of 6-aminouracil, heat and dissolve with 20 milliliters of dimethyl sulfoxide, and add it to the flask as a function monomer, then add 50 ml of acetonitrile to the flask, and add 10 mg of melamine as template molecule, 0.4 ml of methacrylic acid, 20 mg of AIBN as initiator and 3.5 ml of EGDMA as cross-linking agent, and carry out polymerization reaction according to the two-step heating method : first react at 55° C. for 4 hours, then react at 70° C. for 18 hours, and age at 90° C. for 8 hours to obtain melamine trihydrogen bond molecularly imprinted core-shell nanoparticles.

Embodiment 3

[0031] Synthesize graphene oxide and reduce it to obtain reduced graphene oxide: mix graphite powder with concentrated sulfuric acid and phosphoric acid for half an hour, oxidize with potassium permanganate, react at 50°C for 12 hours, and cool the sample to room temperature Pour over containing 300 µl HO 2 o 2 Wash the sample in ice water until the color of the solution turns khaki, and prepare a 0.5 mg / ml solution. 5.0 mg of the above suspension was reacted with 4.0 mg of polyvinylpyrrolidone at 50°C for 12 hours. After cooling to room temperature, 3.5 µl of hydrazine and 40.0 µl of ammonia were added, and reacted at 95°C for 1 hour to obtain reduced graphene oxide. Mix 0.5 ml of 1 mg / ml reduced graphene suspension with 0.5 ml of 5.0 μl / ml ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm]BF 4 ) in DMF to make a modifier. Prepare different electrode modifiers: ① DMF solution of ionic liquid; ② DMF mixture of graphene oxide and ionic liquid; ③ Mixture of re...

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Abstract

The invention relates to a multi-hydrogen-bond melamine core-shell molecularly imprinted polymer and a preparation method thereof. The preparation method comprises the following steps: by adopting SiO2 as an inner core, performing modification on the surfaces of SiO2 nano particles by using 3-aminopropyltriethoxysilane and glutaraldehyde, and connecting a functional monomer 6-aminouracil; and performing polymerization reaction on melamine as a template molecule, methacrylic acid, an initiating agent and a crosslinking agent to prepare the multi-hydrogen-bond melamine core-shell molecularly imprinted polymer. The multi-hydrogen-bond melamine core-shell molecularly imprinted polymer disclosed by the invention can be used for exchanging the roles of a functional monomer in a conventional three-hydrogen-bond molecularly imprinted system and the template molecule, adopts the functional monomer in the conventional system as the template molecule, adopts a template molecule in the conventional system as the functional monomer in a system disclosed by the invention, has very high selectivity, has specific binding only aiming at melamine and triazine compounds, and has good selective enrichment and adsorption effects in highly-specific food detection.

Description

technical field [0001] The invention relates to a molecularly imprinted polymer and a preparation method thereof, in particular to a multi-hydrogen bond melamine core-shell molecularly imprinted polymer and a preparation method thereof. Background technique [0002] Multiple hydrogen bonds are an important force in molecularly imprinted systems. Template molecules and functional monomers generate ligand-selective binding sites through multiple hydrogen bonds, and through this force, target molecules are recognized in the molecular imprinting system. Studies on the synthesis and application of molecularly imprinted polymers based on multiple hydrogen bond interactions have been reported. In these studies, 2-(trifluoromethyl)acrylic acid and diaminopyridine derivatives were used as functional monomers, and thymus Compounds containing pyrimidine bases such as pyrimidine and uracil are used as target molecules, and molecularly imprinted polymers are prepared by forming multiple...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/06C08F222/14C08F2/44C08K9/04C08K9/06C08K3/36C08J9/00G01N27/48
Inventor 郝京诚赵珮妮
Owner SHANDONG UNIV
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