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Preparation method of molecularly imprinted open tubular column

A molecular imprinting and open-column technology, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc. Improved selective identification, increased sensitivity, and reduced matrix interference

Active Publication Date: 2019-10-08
WUHAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional solid-phase extraction column lacks the specific selection ability for the target substance and cannot remove impurities well, which has a great impact on the subsequent analysis and determination.
Moreover, many insoluble, high-viscosity substances and fine particles contained in personal care products are easy to clog the solid-phase extraction column, resulting in a decrease in column efficiency.

Method used

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  • Preparation method of molecularly imprinted open tubular column
  • Preparation method of molecularly imprinted open tubular column
  • Preparation method of molecularly imprinted open tubular column

Examples

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preparation example Construction

[0046] see figure 1 In an embodiment of the preparation method of the molecularly imprinted open-tubular column, the preparation method of the molecularly imprinted open-tubular column comprises the following steps:

[0047] Step S100 , preparing a molecularly imprinted polymer with paraben as a template molecule and modifying the molecularly imprinted polymer with epoxy groups to obtain an epoxy-modified molecularly imprinted polymer.

[0048] Molecular imprinting technology refers to the preparation and application technology of polymers that specifically recognize specific target molecules (template molecules) and their structural analogs. Molecularly imprinted polymers (MIPs) can selectively recognize template molecules in complex systems, and have the advantages of strong resistance to harsh environments, good stability, and long service life, making up for the shortcomings of traditional solid-phase extraction methods. Insufficient, gradually become a research hotspot. ...

Embodiment 1

[0088] Add parabens and functional monomers (a mixture of methacrylic acid and isobutyl vinyl ether) into acetonitrile at a molar ratio of 5:1, prepolymerize at room temperature for 1 min, and then add a crosslinking agent Ethylene glycol dimethacrylate (the molar ratio to the functional monomer is 10:1), the initiator azobisisobutyronitrile 1 mg, nitrogen and oxygen removal for 1 min. Then placed at 50 ° C for 8 hours of polymerization reaction. At the 8th hour of the reaction, 1 mg of initiator azobisisobutyronitrile was added, followed by 20 mL of toluene solution with a mass concentration of 1 (w / w)% glycidyl methacrylate and 1 mg of initiator azobisisobutyronitrile, Continue to react for 4h. After removing the template with an organic solvent, the epoxy-modified molecularly imprinted polymer was obtained.

[0089] Dopamine was dissolved in Tris-HCl buffer solution to obtain a dopamine alkaline solution with a pH of 8.5, which was set aside. Take a polytetrafluoroethyle...

Embodiment 2

[0093] Add parabens and functional monomers (a mixture of methacrylic acid and isobutyl vinyl ether) to acetonitrile at a molar ratio of 10:1, prepolymerize at room temperature for 20 minutes, and then add a crosslinking agent Ethylene glycol dimethacrylate (the molar ratio to the functional monomer is 5:1), 10 mg of initiator azobisisobutyronitrile, nitrogen and oxygen removal for 5 minutes. Then placed at 60 ° C for 12 hours of polymerization reaction. At the 10th hour of the reaction, 3 mg of initiator azobisisobutyronitrile was added, followed by addition of 20 mL of toluene solution with a mass concentration of 8 (w / w)% glycidyl methacrylate and 5 mg of initiator azobisisobutyronitrile, Continue to react for 6h. After removing the template with an organic solvent, the epoxy-modified molecularly imprinted polymer was obtained.

[0094] Dopamine was dissolved in Tris-HCl buffer solution to obtain a dopamine alkaline solution with a pH of 8.5, which was set aside. Take a ...

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Abstract

The invention discloses a preparation method of a molecularly imprinted open tubular column, and relates to the technical field of new materials. The preparation method of the molecularly imprinted open tubular column comprises the following steps: a molecularly imprinted polymer is prepared by taking p-hydroxy-benzoate ester as template molecules and subjected to epoxy group modification, and theepoxy modified molecularly imprinted polymer is obtained; the surface of a capillary tube is subjected to amino modification, and an amino-modified capillary tubular column is obtained; the epoxy modified molecularly imprinted polymer is dispersed in ethyl alcohol to form a mixed solution; and the mixed solution is injected into the amino-modified capillary tubular column, sealing and polymerization are conducted, and the molecularly imprinted open tubular column is formed. The molecularly imprinted open tubular column is prepared, and the molecularly imprinted open tubular column can analyzethe p-hydroxy-benzoate ester in a complex sample.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a preparation method of a molecularly imprinted open-tubular column. Background technique [0002] Parabens (Parabens, PBs) are a class of synthetic esters of p-hydroxybenzoic acid, including methyl p-hydroxybenzoate, ethyl ester, isopropyl ester, propyl ester, isobutyl ester, butyl ester, etc. and their respective The sodium salt is widely used in personal care products, pharmaceuticals and food and other fields. However, related studies have shown that: PBs has a certain endocrine disrupting effect, which can cause an increase in the incidence of female breast cancer and the growth of malignant melanoma, and the relationship between these compounds and immune-related diseases, such as allergies, asthma, diabetes and lupus There is a certain correlation. Generally speaking, personal care products are the main way for the population to expose to PBs, accounting for more t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01J20/26B01J20/286B01J20/30
CPCB01D15/22B01J20/261B01J20/286B01J2220/52B01J2220/54B01J2220/82B01J2220/84
Inventor 方敏沈汪洋宫智勇吴永宁
Owner WUHAN POLYTECHNIC UNIVERSITY
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