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Molecular imprinting polymer as well as preparation method and application thereof

A technology of molecular imprinting and polymers, applied in chemical instruments and methods, other chemical processes, etc., can solve problems that hinder the accurate analysis of target analytes, and achieve the effect of widening the detection range

Inactive Publication Date: 2010-06-09
CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for molecularly imprinted polymers prepared directly with target analytes as templates, the leakage of trace template molecules will hinder the precise analysis of target analytes.

Method used

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  • Molecular imprinting polymer as well as preparation method and application thereof
  • Molecular imprinting polymer as well as preparation method and application thereof
  • Molecular imprinting polymer as well as preparation method and application thereof

Examples

Experimental program
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preparation example Construction

[0034] Preparation I of the molecularly imprinted polymer of embodiment 1DEP

[0035] (1) Synthesis of DEP

[0036] Weigh 10g of methylurea and 40mL of absolute ethanol into a 250mL round bottom flask, stir at room temperature for 5min, slowly add 20mL of benzaldehyde into the flask with a dropping funnel, and then add 1.0mL of boron trifluoride diethyl ether BF 3 .Et 2 O, stirred at room temperature for 1.5h, and a white solid precipitated out, that is, Schiff base 1-benzylidene-3-methylurea ((E)-1-benzylidene-3-methylurea, abbreviated as BMU). Schiff base BMU was recrystallized with ethanol / water solution with a volume ratio of 1:3, and dried under infrared light to obtain pure Schiff base BMU with a yield of 85%. Weigh 10g of Schiff's base BMU and 30mL of toluene in a 250mL round bottom flask, add 6.5mL of diethyl phosphite dropwise with a dropping funnel, and reflux under stirring for 20h (track the reaction process with TLC) to obtain a colorless liquid. The colorless ...

Embodiment 2

[0040] Preparation II of the molecularly imprinted polymer of embodiment 2DEP

[0041] (1) Synthesis of DEP

[0042] Weigh 10g of methyl urea and 40mL of absolute ethanol in a 250mL round bottom flask, stir at room temperature for 5min, slowly add 35mL of benzaldehyde into it with a dropping funnel, and then add 1.0mL of boron trifluoride diethyl ether BF 3 .Et 2 O, stirred at room temperature for 1.5h, and a white solid precipitated out, that is, Schiff base 1-benzylidene-3-methylurea ((E)-1-benzylidene-3-methylurea, abbreviated as BMU). Schiff base BMU was recrystallized with ethanol / water solution with a volume ratio of 1:3, and dried under infrared light to obtain pure Schiff base BMU with a yield of 80%. Weigh 10g of Schiff's base BMU and 30mL of toluene in a 250mL round-bottomed flask, add 10mL of diethyl phosphite dropwise with a dropping funnel, and reflux for 24 hours under stirring (track the reaction process with TLC) to obtain a colorless liquid. The colored liq...

Embodiment 3

[0046] Preparation III of the molecularly imprinted polymer of embodiment 3DEP

[0047] (1) Synthesis of DEP

[0048] Weigh 10g of methylurea and 40mL of absolute ethanol in a 250mL round bottom flask, stir at room temperature for 5min, slowly add 50mL of benzaldehyde into the flask with a dropping funnel, then add 1.0mL of boron trifluoride diethyl ether BF 3 .Et 2 O, stirred at room temperature for 1.5h, and a white solid precipitated out, that is, Schiff base 1-benzylidene-3-methylurea ((E)-1-benzylidene-3-methylurea, abbreviated as BMU). Schiff base BMU was recrystallized with ethanol / water solution with a volume ratio of 1:3, and dried under infrared light to obtain pure Schiff base BMU with a yield of 82%. Weigh 10g of Schiff's base BMU and 40mL of toluene in a 250mL round bottom flask, add 12mL of diethyl phosphite dropwise with a dropping funnel, and reflux under stirring for 16h (track the reaction process with TLC) to obtain a colorless liquid. The colored liquid ...

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Abstract

The invention discloses molecular imprinting polymer which belongs to the technical field of pesticide molecular imprinting and preparation method thereof. The molecular imprinting polymer is prepared by the following steps of: mixing a polymerization reaction monomer, a cross-linking agent, a hole inducing agent, an initiating agent and an imprinting molecule diethyl(3-methyluren)(phenyl)methyl phosphonate, carrying out in-situ polymerization reaction under the condition of thermal initiation and / or photo-initiation to obtain a polymer containing diethyl(3-methyluren)(phenyl)methyl phosphonate; washing the polymer till an imprinting molecule is not detected; and then washing by an organic solvent to neutrality and drying in vacuum to obtain the molecular imprinting polymer. The invention also discloses applications of the molecular imprinting polymer in aspects of separating, purifying and detecting organophosphorus pesticide in a sample. The applications of the polymer prevent the influence of target analyte template leakage on a following adsorption experiment, can simultaneously detect various target molecules and widen the detecting range of the target molecules.

Description

technical field [0001] The invention relates to a molecularly imprinted polymer, a preparation method and application thereof. Specifically, it is an organophosphorus insecticide analog diethyl (3-methylurea) (phenyl) methyl phosphate diethyl (3-methylureido) (phen-yl) methylphosphonate (DEP) as The molecularly imprinted polymer of the template and its preparation method, as well as the application of the molecularly imprinted polymer for separation, purification and determination of organophosphorus pesticides in biological or environmental samples. Background technique [0002] The structure of my country's pesticide products is seriously unsuitable for the standardized production of agricultural products, which is concentrated in three 70%: insecticides account for 70%, organophosphorus pesticides account for 70% of insecticides, and highly toxic pesticides account for 70% of organophosphorus pesticides. Organophosphorus is currently the most widely used pesticide with t...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/30
Inventor 潘灿平徐云康澍
Owner CHINA AGRI UNIV
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