Boron affinity monolithic column based on atom transfer radical polymerization and preparation method thereof

An atom transfer and monolithic column technology, applied in the field of boron affinity monolithic column and its preparation, can solve the problem of low adsorption capacity of boron affinity monolithic column, and achieve the effect of high affinity, stable physical and chemical properties, and easy operation.

Inactive Publication Date: 2018-02-02
TIANJIN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a boron-affinity monolithic column for atom transfer radical polymerization and its preparation method, which can overcome the disadvantage of low adsorption capacity of the existing boron-affinity monolithic column

Method used

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  • Boron affinity monolithic column based on atom transfer radical polymerization and preparation method thereof
  • Boron affinity monolithic column based on atom transfer radical polymerization and preparation method thereof
  • Boron affinity monolithic column based on atom transfer radical polymerization and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] First, the basic porous polymer monolithic column was prepared by ATRP reaction, and then the boron-affinity polymer chain was grafted on the base column by ATRP reaction to prepare the boron-affinity monolithic column, and the basic porous polymer monolithic column and boron-affinic Carry out scanning electron microscopy analysis and characterization, infrared characterization and nitrogen adsorption analysis with the monolithic column. The specific operation steps are as follows:

[0038] Preparation method of boron affinity monolithic column based on two-step ATRP reaction:

[0039] The first step: 0.53% of cuprous bromide (both mass fractions) and 41.4% of ethylene glycol dimethacrylate are dissolved in a mixture of methanol and 26.0% n-hexane with a mass fraction of 31.2%, and ultrasonic at room temperature (Ultrasonic electric power 150 watts) until the cuprous bromide is evenly distributed, add 0.23% ethyl 2-bromopropionate, and after nitrogen gas for 10 minutes,...

Embodiment 2

[0051] Small molecule separation experiment to study the specific adsorption performance of boron-affinity monolithic column based on two-step ATRP reaction on cis-dihydroxy small molecule substances. The specific operation steps are as follows:

[0052] The boron affinity monolithic column based on the two-step ATRP reaction was synthesized with the above method (Example 1) for the separation of cis-dihydroxy small molecular substances.

[0053] Prepare mobile phase: mobile phase one is acetic acid-ammonia solution (pH=8.5) with 0.4% (v / v) acetic acid concentration, mobile phase two is acetic acid solution (pH=3.1) with 0.4% (v / v) concentration .

[0054] Use mobile phase 1 to prepare a mixed solution of ferulic acid-rutin, ferulic acid-rosmarinic acid, epinephrine-phenylephrine at a concentration of 1 ppm. The boron affinity monolithic column was used as a chromatographic column, and the above solution was chromatographically separated by HPLC-UV.

[0055] The chromatogra...

Embodiment 3

[0058] Glycoprotein separation experiment to study the specific adsorption performance of the boron affinity monolithic column based on the two-step ATRP reaction for proteins containing cis-dihydroxyl groups. The specific operation steps are as follows:

[0059] The same method as above (Example 1) was used to synthesize a boron affinity monolithic column based on ATRP reaction for separating cis-dihydroxy-like proteins.

[0060] Prepare mobile phase: mobile phase one is acetic acid-ammonia solution (pH=8.5) with 0.4% (v / v) acetic acid concentration, mobile phase two is acetic acid solution (pH=3.1) with 0.4% (v / v) concentration .

[0061] Use mobile phase one to prepare a mixed solution of lysozyme-horseradish peroxidase, lysozyme-DNase B, and lysozyme-transferrin at a concentration of 10 ppm. The boron affinity monolithic column was used as a chromatographic column, and the above solution was chromatographically separated by HPLC-UV.

[0062] The chromatographic conditio...

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Abstract

The invention relates to a boron affinity monolithic column based on atom transfer radical polymerization and a preparation method thereof. The raw materials for preparation of a basic porous polymermonolithic column include, by mass, 0.34-0.68% of cuprous bromide, 41-46% of ethylene glycol dimethacrylate, 26-36% of methanol, 20-30% of n-hexane, 0.14-0.28% of ethyl 2-bromopropionate, and 0.42-0.84% of pentamethyldiethylenetriamine. Then a boron affinity polymer chain is grafted to the basic porous polymer monolithic column by atom transfer radical polymerization to prepare a boron affinity monolithic column, and the raw materials include, by mass, 3.3-6.4% of 4-vinylbenzeneboronic acid, 0.23-0.45% of pentamethyldiethylenetriamine, 12-20% of double distilled water, 75-84% of isopropanol, 0.45-0.86% of hydrazine hydrate (80%), and copper bromide 0.19-0.28% of cuprous bromide. The boron affinity monolithic column provided by the invention has the advantages of simple preparation method,specific adsorption capacity to cis-dihydroxyl substance, high affinity and high capacity, and has broad application prospect.

Description

technical field [0001] The invention relates to a boron affinity monolithic column based on atom transfer radical polymerization and a preparation method thereof. Specifically, a porous monolithic column base column containing a surface initiator is firstly prepared based on atom transfer radical polymerization, and then atom transfer radical polymerization is used to A boron-affinity polymer chain is grafted on the inner surface of a porous monolithic column base to prepare a boron-affinity monolithic column. The monolithic column has specific adsorption capacity for compounds containing cis-dihydroxy groups, such as catechol, adenosine, rosmarinic acid, epinephrine, glycoprotein, etc. Background technique [0002] Atom Transfer Radical Polymerization (ATRP) is one of the living / controllable radical polymerization methods with the most industrial prospects. diverse. Surface-initiated ATRP (SI-ATRP) is especially suitable for grafting polymers on the surface of solid mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/285B01D15/38B01D15/22C08F122/10C08F267/06C08F230/06C07K1/22
CPCB01D15/22B01D15/3804B01J20/264B01J20/28052B01J20/285B01J2220/4812B01J2220/52B01J2220/82C07K1/22C08F122/1006C08F267/06C08F230/06
Inventor 王涎桦董乾池帅帅邓习燕
Owner TIANJIN MEDICAL UNIV
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