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Chrysanthemum ester molecularly imprinted polymer preparing method

A technology of molecular imprinting and polymers, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems that the particle size and uniformity of polymer powder particles are greatly affected by grinding technology, cumbersome operation, and many steps. The effect of low preparation cost, simple preparation process and high enrichment degree

Inactive Publication Date: 2015-11-04
福州市产品质量检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The molecularly imprinted polymers of pyrethroid pesticides prepared by the existing reported methods are generally blocky and require further grinding, but the particle size and uniformity of the polymer powder after grinding are greatly affected by the grinding technology, resulting in process instability , also affects the effect of polymer extraction of pesticides
In addition, the existing preparation method has many steps, cumbersome operation and harsh process conditions

Method used

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  • Chrysanthemum ester molecularly imprinted polymer preparing method
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  • Chrysanthemum ester molecularly imprinted polymer preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 Preparation of Phenothrin Imprinted Polymer Powder

[0031] Take 37.5mL of absolute ethanol, 12.5mL of styrene, 1.0ml of EDMA, 1.0ml of chloroform, 35mg of phenothrin, 0.15g of AIBN, and 0.375g of PVP K-30 in a ground-mouth flask, mix them uniformly by ultrasonic, and aerate with nitrogen 15min, heated and stirred in an oil bath at 70°C with nitrogen gas for 24h, after the reaction was completed, let stand to separate layers, centrifuged to remove the supernatant, and eluted the imprinted polymer of phenothrin with acetic acid / methanol (V / V=1:1) , until no template molecule could be detected in the supernatant, the obtained phenothrin imprinted polymer powder was vacuum-dried at 60°C, and scanned with an electron microscope after drying. Scanned images from the electron microscope, attached figure 1 It can be seen that the phenothrin-imprinted polymer is in the shape of microspheres, and the surface pores are obvious.

Embodiment 2

[0032] Example 2 Preparation of polypermethrin imprinted polymer powder

[0033] Take 37.5mL of absolute ethanol, 12.5mL of styrene, 1.0ml of EDMA, 0.75ml of chloroform, 100ug of permethrin, 0.15g of AIBN, and 0.375g of PVP K-30 in a ground-mouth flask, mix them uniformly by ultrasonic, and blow nitrogen Aerate for 15 minutes, heat and stir in an oil bath at 70°C with nitrogen for 24 hours. After the reaction is over, let stand to separate layers, centrifuge to remove the supernatant, and elute the polypermethrin blot with formic acid / ethanol (V / V=1:1) polymer, combined eluents, and the obtained polypermethrin-imprinted polymer powder was vacuum-dried at 60°C. The supernatant after the polymerization reaction is taken, and the content of polypermethrin template molecules in the supernatant is detected by gas chromatography, and the eluate is taken to detect the content of polypermethrin template molecules by gas chromatography. diagram 2-1 It is the gas chromatographic detec...

Embodiment 3

[0034] Example 3 Solid Phase Extraction of Pesticide Residues in Tea with Polymer Powder

[0035] Take by weighing 5g pulverized tea negative sample and add standard solution, add 50mL acetonitrile and shake for 30min to extract, extract with 30000rpm centrifugation for 15min, transfer supernatant, add 0.1g polymer powder (prepared by embodiment 1 or embodiment 2) in the supernatant ), shaken for 30 minutes and mixed well, centrifuged at 3000rpm for 15 minutes, discarded the supernatant, eluted the polymer powder with acetic acid / methanol (V / V=1:1), combined the eluent, concentrated to near dryness with nitrogen blowing, and used petroleum Dilute the volume of ether to 1mL for gas chromatography (GC) detection, and the standard addition recovery rate can reach more than 90%.

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Abstract

The invention discloses a chrysanthemum ester molecularly imprinted polymer preparing method and relates to a molecularly imprinted polymer preparing method. The chrysanthemum ester molecularly imprinted polymer preparing method includes the following steps that firstly, chrysanthemum ester type template molecules, styrene, halomethane, a cross-linking agent, a stabilizing agent and an initiating agent are evenly mixed and are stirred at the temperature of 50-80 DEG C after nitrogen leading and aerating; secondly, after a reaction is over, standing and layering are conducted, supernatant is removed, a lower-layer solid is eluted through a carboxylic acid and alcohol mixing solution, and chrysanthemum ester molecularly imprinted polymer powder is obtained. The preparing chrysanthemum ester molecularly imprinted polymer is in a powder form, powder-form polymers are in a microsphere shape, surface hole forming is obvious, the powder-form polymers can be directly used for extracting chrysanthemum ester pesticide residues from food media without being ground, and the recovery rate can reach more than 90 percent. According to the chrysanthemum ester molecularly imprinted polymer preparing method, processing does not need to be conducted again, the preparing process is simple, the technology is stable, and the preparing cost is low.

Description

technical field [0001] The invention relates to a method for preparing molecularly imprinted polymers, in particular to a method for preparing pyrethroid molecularly imprinted polymers. Background technique [0002] Pyrethroid pesticides are broad-spectrum insecticides with quick-acting, high-efficiency, low toxicity, low residue, and safety to crops. In addition to having special effects on more than 140 kinds of pests, some pyrethroid pesticides are also effective on underground pests and Acarid pests have a good control effect, therefore, pyrethroid pesticides are widely used in the agricultural field, and pyrethroid pesticide residues are a major problem in today's food health. [0003] Molecular Imprinting Technology (MIT) is a new technology for the preparation of polymer materials with recognition function that has emerged in recent years. It can obtain molecularly imprinted polymers (molecularly imprinted polymers, MIPs), this technology has been applied to the prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F222/14C08J9/26B01J20/26B01J20/30
Inventor 许艳军应松陈熔林清荷王勍陈亮翁贵凤
Owner 福州市产品质量检验所
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