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Pseudo template magnetic molecule imprinted polymer for pesticide residue detection of waterborne sample and application

A magnetic molecular imprinting and pseudo-template technology, applied in the preparation of test samples, other chemical processes, chemical instruments and methods, etc., can solve the problem of high price of solid-phase extraction cartridges, environmental and analyst hazards, and easy precipitation to agglomerate. and other problems, to achieve good selective adsorption characteristics, avoid agglomeration and agglomeration, and avoid template leakage.

Inactive Publication Date: 2015-11-18
HUNAN AGRICULTURAL UNIV
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AI Technical Summary

Problems solved by technology

The SPE method mainly has the following problems: 1. It is complicated and time-consuming, generally takes 3.0-3.5 hours; 2. The cost is high. One-time use; 3. Toxic and harmful organic solvents are consumed more (80-120 ml) in the pretreatment process, causing harm to the environment and analysts
However, Fe 3 o 4 Nanoparticles have high specific surface energy, Fe prepared under alkaline conditions 3 o 4 The surface contains more active groups (-OH), and the dipole moment between the particles is easy to agglomerate and has poor dispersion. The black Fe obtained by the co-precipitation method 3 o 4 Precipitation is very easy to agglomerate, and it is difficult to form dispersed particles. It is difficult to be used as the "core" for molecular imprinted polymerization in practical applications.
[0006] In addition, molecular imprinting technology generally has a technical bottleneck of "template leakage", which may cause high pesticide residue detection results or even false positive results in instrument detection
In addition, currently more mature molecularly imprinted polymers are mostly suitable for synthesis in organic solvents, and the selective adsorption effect on pesticide targets in aqueous solution is not good. As a solvent, it is more environmentally friendly than organic solvent extraction

Method used

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  • Pseudo template magnetic molecule imprinted polymer for pesticide residue detection of waterborne sample and application
  • Pseudo template magnetic molecule imprinted polymer for pesticide residue detection of waterborne sample and application

Examples

Experimental program
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Effect test

Embodiment 1 3

[0021] Example 1 Dicofol Pesticide Pseudo-template Magnetic Molecularly Imprinted Polymer Particles (Fe 3 o 4 Preparation of MIPs)

[0022] Fe coated with oleic acid 3 o 4 Preparation of nanoparticles: 0.02mol of FeCl 2 4H 2 O with 0.03mol FeCl 3 ·6H 2 O was dissolved in 100 mL of degassed ultrapure water, 2 mL of oleic acid was added, ultrasonic water bath was used for 20 min, and nitrogen was blown and stirred at 600 r / min, and 15 mL of NH was added dropwise when the temperature rose to 60 °C. 3 ·H 2 O, after reacting for 30 minutes, add 2 mL of oleic acid dropwise while stirring, react at 80°C for 1 hour, separate the precipitate with a magnet, wash the precipitate with distilled water and ethanol in turn, and finally dry it in vacuum at 50°C for 24 hours.

[0023] Preparation of particles: Take 3.0 g of polyvinylpyrrolidone (PVP) and add it to 120 mL of water, stir at 600 r / min until the polyvinylpyrrolidone is completely dissolved to obtain an aqueous solution of ...

Embodiment 2

[0024] Example 2 Cypermethrin Pesticide Pseudo-template Magnetic Molecularly Imprinted Polymer Particles (Fe 3 o 4 Preparation of MIPs)

[0025] Fe coated with oleic acid 3 o 4 Preparation of nanoparticles: 0.02mol of FeCl 2 4H 2 O with 0.03mol FeCl 3 ·6H 2 O was dissolved in 100 mL of degassed ultrapure water, 2 mL of oleic acid was added, ultrasonic water bath was used for 20 min, and nitrogen was blown and stirred at 600 r / min, and 15 mL of NH was added dropwise when the temperature rose to 60 °C. 3 ·H 2 O, after reacting for 30 minutes, add 2 mL of oleic acid dropwise while stirring, react at 80°C for 1 hour, separate the precipitate with a magnet, wash the precipitate with distilled water and ethanol in turn, and finally dry it in vacuum at 50°C for 24 hours.

[0026] Preparation of particles: Take 3.0g of polyvinylpyrrolidone (PVP) and add it to 120mL of water, stir at 600r / min until completely dissolved to obtain an aqueous solution of polyvinylpyrrolidone; take...

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Abstract

The invention provides a pseudo template magnetic molecule imprinted polymer for pesticide residue detection of a waterborne sample. The polymer Fe3O4@MIPs is prepared by comprising the steps that oleic acid-coated Fe3O4 nanoparticles, pseudo template molecules and functional monomers MAA are added into pore-forming agents, and after self-assembly is performed, cross-linking agents EGDMA and initiating agents AIBN are added in the mixture; after the cross-linking agents EGDMA and the initiating agents AIBN are completely dissolved, the mixture is dropwise added into polyvinyl pyrrolidone water solutions to complete a polymerization reaction; after Fe3O4@MIPs containing the pseudo template molecules is separated through an external magnetic field, the pseudo template molecules are removed, vacuum drying is performed, and the polymer is prepared. According to the polymer, the Fe3O4 nanoparticles are coated with oleic acid, and therefore the agglomeration phenomenon in the Fe3O4 preparation process is effectively avoided; a molecular imprinting polymerization reaction is performed by taking a compound of which the structure is similar to that of target pesticide as the pseudo template molecules, and therefore the phenomenon that a high result or a false positive result caused by the template leakage problem is effectively avoided; the target pesticide is easily and quickly separated from and brought away from the liquid sample through the magnetism of the polymer; the polymer is high in selectivity, little in interference, easy to operate, capable of being reused after being eluted, suitable for being used in the waterborne sample and good in effect.

Description

technical field [0001] The invention belongs to the field of pretreatment of pesticide residue detection samples, in particular to a pseudo-template magnetic molecularly imprinted polymer particle Fe that can be used for the detection of pesticide residues in aqueous samples 3 o 4 MIPs selectively adsorb the pesticide residues in the sample, so as to facilitate the detection of pesticide residues in the sample. Background technique [0002] The detection method of pesticide residues mainly includes four steps: extraction, purification, concentration, and determination, among which extraction and purification are the main technical cores of current sample pretreatment. The current national standard method, industry standard method and local standard method currently formulated, the sample pretreatment operation mainly recommends solvent extraction followed by solid-phase extraction (Solid-PhaseExtraction, SPE) purification and pre-separation. The SPE method mainly has the f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/06C08F222/14C08F2/44C08J9/28C08K9/10C08K3/22B01J20/26B01J20/30G01N1/34
Inventor 谭君刘仲华
Owner HUNAN AGRICULTURAL UNIV
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