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Preparation method of cyhalothrin molecularly imprinted polymer and use thereof

A technology of cyhalothrin and molecular imprinting, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of poor imprinting efficiency, large difference in MIP performance, large molecular structure, etc., and achieve good regeneration performance and improve specificity. Adsorption capacity, kinetics combined with fast effect

Inactive Publication Date: 2011-03-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for specific template molecules, the preparation of corresponding MIP using cyclodextrin as a functional monomer still needs to be carried out one by one; this is because the performance of MIP obtained by different template molecules participating in the imprinting reaction is quite different
At present, there is no research report on the preparation of cyhalothrin MIP and its application using cyclodextrin as a functional monomer abroad.
In addition, compared with other pesticides, cyhalothrin has a large molecular structure and few polar groups, so it is difficult to generate strong intermolecular forces with conventional functional monomers, resulting in poor imprinting efficiency, resulting in the loss of the obtained MIP. The specific binding performance is not ideal, so it is necessary to find more suitable functional monomers to prepare MIP

Method used

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  • Preparation method of cyhalothrin molecularly imprinted polymer and use thereof
  • Preparation method of cyhalothrin molecularly imprinted polymer and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Weigh 1.5mmol of dry β-cyclodextrin and dissolve it in 20ml of anhydrous dimethyl sulfoxide (DMSO), add 0.5mmol of cyhalothrin (as a template molecule), stir at room temperature (15-35°C) for 1h, and then Slowly add 9mmol of 1,6-hexamethylene diisocyanate (HMDI) dropwise, and react with magnetic stirring at 65°C for 24h; Frequency: 40KHz) to remove template molecules and unreacted β-cyclodextrin, cross-linking agent (1,6-hexamethylene diisocyanate) and DMSO, until no template molecules (cyhalothrin) were detected in the wash supernatant. A GC method can be used to detect whether cyhalothrin as a template molecule is contained in the wash supernatant. After centrifugation, suction filtration and drying, the blocky polymer is ground into fine particles to obtain HMDI-crosslinked cyhalothrin MIP (namely MIP-HMDI), which is stored in a dry container at room temperature.

[0023] Using a non-imprinted polymer (NIP) as a blank control, the synthesis method of the non-imprint...

Embodiment 2

[0038] Weigh 1.5mmol of dry β-cyclodextrin and dissolve it in 20mL of anhydrous DMSO, add 0.5mmol of cyhalothrin (template molecule), stir at room temperature (15-35°C) for 1h, then slowly add 9mmol of toluene-2 , 4-diisocyanate (TDI), magnetic stirring reaction under 65 ℃ for 24h; The flocculent precipitate was then ultrasonically extracted with hot water-ethanol-acetone solvents in order to remove unreacted β-cyclodextrin, cross-linking agent, template molecule and DMSO until no template molecule was detected in the supernatant of the washing solution (using GC detection); after centrifugation, suction filtration, and drying, the massive polymer was ground into fine particles to obtain TDI-crosslinked cyhalothrin MIP (ie MIP-TDI), which was stored in a dry container at room temperature.

[0039] Using NIP as a blank control, the synthesis method is the same as the above-mentioned preparation method of cyhalothrin MIP except that no template molecule is added to obtain NIP-TD...

Embodiment 3

[0053] Weigh 2 mmol of dry β-cyclodextrin and dissolve it in 25 mL of anhydrous DMSO, add 0.5 mmol of cyhalothrin template molecule, stir at room temperature (15-35°C) for 1 hour, then slowly add 10 mmol of naphthalene diisocyanate (NDI) dropwise , and reacted with magnetic stirring at 65°C for 24 hours; after the reaction, the white slurry was taken out and ultrasonically extracted with acetone-hot water-ethanol in order to remove template molecules and unreacted β-cyclodextrin, cross-linking agent (NDI) and DMSO until no template molecules were detected in the supernatant of the washing liquid (detected by GC); after centrifugation, suction filtration, and drying, the blocky polymer was ground into fine particles to obtain NDI-crosslinked cyhalothrin MIP (ie, MIP- NDI), stored in a desiccated container at room temperature.

[0054] Using NIP as a blank control, the synthesis method is the same as the above-mentioned preparation method of cyhalothrin MIP except that no templa...

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Abstract

The invention discloses a preparation method of cyhalothrin molecularly imprinted polymer, orderly including the following steps: 1) dissolving a beta-cyclodextrin as functional monomers in a solvent, and then, adding a cyhalothrin as molecular templates for stirred reaction at room temperature; 2) adding a isocyanate compound as a cross-linking agent in a mixed liquor obtained from the step 1) for reaction with magnetic stirring; 3) washing the reaction products of the step 2) with an ultrasonic extraction method to remove the cyhalothrin, the un-reacted beta-cyclodextrin, the isocyanate compound and the solvent; 4) processing products of the step 3) with centrifugation, vacuum filtering and drying, and milling the obtained blocky high polymers into grains which are the cyhalothrin molecularly imprinted polymers. The cyhalothrin molecularly imprinted polymers can be used for High-selectivity enrichment and separation and purification of trace amount of the cyhalothrin in environmental samples or plant samples.

Description

technical field [0001] The invention relates to a cyhalothrin molecularly imprinted polymer based on host-guest inclusion complexation, and the polymer is suitable for highly selective enrichment and separation and purification of trace amounts of cyhalothrin in environment and plant samples. Background technique [0002] Cyhalothrin (trade name: Kungfu Chrysin, lambda-cyhalothrin) is (S)-alcohol-(Z)-1R-cis-acid and (R)-alcohol-(Z)-1S-cis-acid[1: 1] The mixture, as a typical second-generation pyrethroid pesticide, has the characteristics of fast insecticidal effect, long-lasting effect, high efficiency, low toxicity and low residue. One of the main varieties. It is mainly used for contact killing and stomach poisoning. It has permeability but no systemic effect. It can effectively control Lepidoptera, Hemiptera, Coleoptera and mites, but it is highly effective against aquatic animals such as fish and shrimp, silkworms and bees. poison. So far, there have been some reports...

Claims

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Application Information

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IPC IPC(8): C08G18/64C08J9/26B01J20/285B01J20/30
Inventor 桂文君郭逸蓉梁晓王阳阳刘毅华朱国念
Owner ZHEJIANG UNIV
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