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Molecularly imprinted monolithic column with high monomer content and preparation method

A technology of molecular imprinting and monomer content, applied in chemical instruments and methods, material separation, analysis of materials, etc., can solve the problems of high performance liquid chromatography and high negative pressure of the column, and achieve obvious imprinting effect, high column efficiency, and column efficiency high effect

Inactive Publication Date: 2015-01-07
TIANJIN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the common porogens commonly used at present, such as toluene / iso-octane mixed system, often produce monolithic columns with extremely high column negative pressure, which cannot be applied to conventional high-performance liquid chromatography at all.

Method used

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  • Molecularly imprinted monolithic column with high monomer content and preparation method
  • Molecularly imprinted monolithic column with high monomer content and preparation method
  • Molecularly imprinted monolithic column with high monomer content and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Preparation and chromatogram of high monomer content molecularly imprinted monolithic column using ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate as porogen and naproxen as template.

[0039] Naproxen high monomer content molecularly imprinted monolithic column was synthesized by in-situ polymerization, and the chromatograms of the imprinted column and blank column were obtained after suitable chromatographic conditions. The synthesis reaction conditions and chromatographic conditions are as follows:

[0040] Preparation of high monomer content imprinted monolithic columns by in situ polymerization:

[0041] a. The mass percentage template naproxen 2.44%, auxiliary monomer methyl methacrylate 3.39%, functional monomer 4-vinylpyridine 4.48%, initiator azobisisobutyronitrile 0.32%, crosslinking agent dimethyl Ethylene glycol acrylate 67.80%, dissolved in the mixed porogen solution of porogen 1-butyl-3-methylimidazolium tetrafluoroborate 16.91%, dimethyl sulfox...

Embodiment 2

[0047] In order to demonstrate the permeability of the molecularly imprinted monolithic column with high monomer content, we prepared a high monomer content column and a low monomer content column (40% monomer content) with the same chemical composition but different ratios of monomer and porogen. And carried out mercury intrusion analysis, the specific operation steps are as follows:

[0048] Synthesis method of low monomer content column:

[0049] a. template naproxen 2.31% (both mass percent), auxiliary monomer methyl methacrylate 1.61%, functional monomer 4-vinylpyridine 2.13%, initiator azobisisobutyronitrile 0.30%, cross Joint agent ethylene glycol dimethacrylate 32.20%, dissolved in the mixed porogen solution of 48.17% 1-butyl-3-methylimidazolium tetrafluoroborate and 13.27% dimethyl sulfoxide as porogen Medium; Ultrasonic dissolution for 30 min to dissolve and clarify, remove oxygen in the liquid, then inject the prepolymer into a stainless steel column (100 × 4.6 mm ...

Embodiment 3

[0055] The present invention simultaneously synthesizes a high-monomer content molecularly imprinted monolithic column using ketoprofen as an imprinting template, and the specific operation steps are as follows:

[0056] With template ketoprofen 3.82% (both mass percent), auxiliary monomer methyl methacrylate 3.35%, functional monomer 4-vinylpyridine 4.37%, initiator azobisisobutyronitrile 0.31%, linking agent Ethylene glycol dimethacrylate 66.89%, dissolved in a porogen solution of 16.67% 1-butyl-3-methylimidazolium tetrafluoroborate and 4.59% dimethyl sulfoxide; Ultrasonic dissolution was performed for 30 min to dissolve and clarify the liquid, and the oxygen in the liquid was removed, and then the prepolymer was injected into a stainless steel column (100 × 4.6 mm I.D.), both ends were sealed, and reacted in a water bath at 60 °C for 1.5 h. After the polymerization is completed, the column is washed with the same method as in Example 1.

[0057] High monomer content monoli...

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Abstract

The invention relates to a molecularly imprinted monolithic column with high monomer content and a preparation method. The molecularly imprinted monolithic column comprises the following materials in percent by weight: 1.96-3.82% of naproxen or ketoprofen, 2-5.22% of methyl methacrylate, 4.37-4.48% of 4-vinylpyridine, 0.32% of azodiisobutyronitrile, 67.8% of ethylene glycol dimethacrylate, 14.89-19.18% of 1-butyl-3-methylimidazole tetrafluoroborate and 2.56-6.54% of dimethyl sulfoxide. The molecularly imprinted monolithic column has the beneficial effects that by a formula design of a pore-forming agent, the content of monomers such as a functional monomer, a crosslinking agent and the like is up to 80%, and the content of the pore-forming agent is not more than 20%. The ion liquid (1-butyl-3-methylimidazole tetrafluoroborate) is used as a main pore-forming agent, and the monolithic column with short synthesis time (shorter than 1.5 hours), specific imprinting effect and high column efficiency (N=11680platesm<-1>) is prepared. The molecularly imprinted monolithic column has the average diameter with the size from submicron to micron and is good in permeability. The molecularly imprinted monolithic column has the advantages that the environmental friendliness is better, the consumption of the pore-forming agent can be reduced by 2-3 times, the preparation method is simple and convenient, the permeability is good, the back pressure is low, the mechanical strength is good, and the molecular recognition effect is good.

Description

technical field [0001] The invention relates to a molecularly imprinted monolithic column with high monomer content and a preparation method. Background technique [0002] Molecular imprinting technique (MIT), also known as molecular imprinting technique, is a technique developed on the basis of simulating the interaction of enzyme-substrate and receptor-antibody in nature to synthesize a preselective stationary phase. MIT has three characteristics: pre-determinedness, specific recognition and wide applicability. Monolithic column, also known as monolithic stationary phase, continuous bed or continuous rod, is a continuous bed stationary phase that is polymerized in the chromatographic column by organic or inorganic polymerization method, and is a high-performance liquid chromatography monolithic column prepared by in-situ polymerization. It is one of them, which has better porosity and permeability than conventionally packed chromatographic columns, and has the characteri...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/30G01N30/60G01N30/56
CPCB01J20/285B01J2220/62G01N30/56G01N30/60
Inventor 刘照胜黄艳萍李秀媛陈秀秀钟丹丹
Owner TIANJIN MEDICAL UNIV