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Preparation method of carbaryl molecularly imprinted polymer

A technology of molecular imprinting and polymers, applied in chemical instruments and methods, other chemical processes, etc., can solve rare and large specific surface area problems, achieve low detection limit, good selective adsorption, and good popularization and use

Active Publication Date: 2019-01-08
SICHUAN AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a new type of polymer material, metal nanomaterials have the characteristics of large specific surface area, surface modification and easy separation from complex matrices under the action of an external magnetic field. At present, nanomaterials are used to prepare carbaryl molecularly imprinted polymers. The method is rarely reported

Method used

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  • Preparation method of carbaryl molecularly imprinted polymer
  • Preparation method of carbaryl molecularly imprinted polymer
  • Preparation method of carbaryl molecularly imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Preparation of Fe 3 o 4 Nanoparticles:

[0040] 2.7802g FeSO 4 ·7H 2 O (0.01mol) and 5.4058g FeCl 3 ·6H 2 O (0.02mol) was successively dissolved in 100mL ultrapure water, and after being completely dissolved, it was transferred to a separatory funnel; then the prepared mixed iron solution was slowly added dropwise to a 45mL 2.0mol·L -1 NaOH and 8mL 0.2mol·L -1 In the three-necked flask of the sodium citrate mixed solution (deoxygenated with nitrogen, the flask was placed in a water bath at 80°C), during the dropwise addition, the reaction temperature was kept constant at 80°C and oxygen was isolated, and stirring was continued. After the dropwise addition was completed, the stirring reaction was continued for 1 h, and nitrogen gas was introduced throughout the whole process to prevent oxygen from entering; finally, the nanoparticles were separated by a magnetic field, washed with ultrapure water until neutral, and a uniform magnetic fluid Fe containing magneti...

Embodiment 2

[0044] (2) Preparation of modified nanoparticles:

[0045] Take 100mg of the magnetic nanomaterial prepared in Example 1 and disperse it in 100mL of ethanol-water (V:V=8:2) solution, oscillate and mix well, ultrasonicate for 15min, add 1mL of tetraethyl orthosilicate, 25% Ammonia water 2mL, then sonicated for 10min, followed by deoxygenation operation (nitrogen gas for 1min), and finally shaken in a water bath at 30°C for 6h to obtain Fe 3 o 4 @SiO 2 .

[0046] Wash Fe with ethanol 3 o 4 @SiO 2 After several times, the particles were dispersed in 100mL ethanol solution, and 2mL KH570 was added to it, ultrasonicated for 10min, filled with nitrogen for 1min to deoxygenate, and then placed in a water bath shaker at 60°C for 24h to obtain double bond modified Fe 3 o 4 @SiO 2 Nanoparticles.

Embodiment 3

[0048] (3) Preparation of Molecularly Imprinted Polymers MMIPs / MNIPs

[0049] Wash the double bond modified Fe with acetonitrile 3 o 4 @SiO 2 Magnetic nanoparticles several times, the double bond modified magnetic nanoparticles and sequentially added 0.1g template molecule (carbaryl), 0.345mL functional monomer (methacrylic acid), 30μL ionic liquid (1-butyl-3- Methylimidazole hexafluorophosphate) was mixed with 50 mL of acetonitrile solution and ultrasonicated for 10 min. Dissolve 0.1g of PVP dispersant in 50mL of acetonitrile, add it into the magnetic material mixed solution, then add 1.585mL of crosslinking agent (ethylene glycol dimethacrylate), after ultrasonication for 10min, add 25mg of initiator (coupling Nitrobutyronitrile), ultrasonication for 1 min, deoxygenation treatment (nitrogen gas filling for 1 min), and shaking in a water bath at 60°C for 24 h to obtain MMIPs. The preparation of MNIPs is the same as that of MMIPs except that template molecules are not adde...

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Abstract

The invention provides a preparation method of a carbaryl molecularly imprinted polymer, and belongs to the technical field of preparation of an adsorbent in detection of pesticide residues. The preparation method provided by the invention comprises the following steps of (1) preparing nanoparticles; (2) modifying the prepared nanoparticles; (3) synthetizing the molecularly imprinted polymer; and(4) preparing the carbaryl molecularly imprinted polymer. The prepared carbaryl molecularly imprinted polymer can perform fast detection and treatment on a trace quantity of carbaryl agricultural chemicals in foods or fruits and vegetables, is good in selective adsorption properties on the carbaryl, has high recovery rate, low detection limit and high precision when being applied to actual sampledetection as a solid phase extraction agent, and is high in detection sensitivity and suitable for actual detection application.

Description

technical field [0001] The invention belongs to the technical field of molecular imprinting, and in particular relates to a method for preparing a carbaryl molecular imprinting polymer, which can be well used for detecting and treating trace residues of the pesticide carbaryl in grains, fruits and vegetables. Background technique [0002] Carbaryl is a 1-naphthyl-N-methylcarbamate insecticide. It entered the pesticide market in the middle of the 20th century. Due to its high efficiency and broad spectrum, it is widely used in fruits, vegetables, grains and economic crops, etc. pest control. Carbaryl is moderately toxic and can enter organisms through the skin, digestive system, and respiratory system. Lighter poisoning manifests as headache, nausea, vomiting, miosis, etc.; severe cases coma, convulsions, pulmonary edema and even death. Its residual time is long, and its long-term effect on the human body will interfere with human endocrine, such as inhibiting the synthesis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F220/06C08K9/06C08K3/22C08K3/36C08J9/26B01J20/26B01J20/30
CPCB01J20/268C08F222/1006C08F222/102C08J9/26C08J2335/02C08K3/22C08K3/36C08K9/06C08K2003/2275C08K2201/01C08K2201/011C08F220/06
Inventor 陈姝娟付珍珍付静霞邹立扣何利杨勇周康刘书亮敖晓琳申光辉
Owner SICHUAN AGRI UNIV