Hollow molecularly imprinted polymers and solid phase extraction column and preparation method and application thereof

A solid-phase extraction column and molecularly imprinted technology, which is applied in the field of preparation of hollow molecularly imprinted solid-phase extraction columns, can solve the problems of uneven distribution of imprinted sites, unfavorable elution, and too deep "embedding" to improve adsorption Efficiency, obvious adsorption effect, obvious enrichment effect

Inactive Publication Date: 2017-09-22
HARBIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nevertheless, there are still problems in the preparation process of molecularly imprinted polymers such as uneven distribution of imprinted s...

Method used

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  • Hollow molecularly imprinted polymers and solid phase extraction column and preparation method and application thereof
  • Hollow molecularly imprinted polymers and solid phase extraction column and preparation method and application thereof
  • Hollow molecularly imprinted polymers and solid phase extraction column and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Preparation of a Boron Affinity Hollow Molecularly Imprinted Solid Phase Extraction Column

[0039] Weigh 1.00 mmol of monomeric methacrylic acid and 1.00 mmol of 3-aminophenylboronic acid respectively, mix the two evenly, and then dissolve them in 40 mL of acetonitrile, and stir at room temperature for 12 hours to obtain methacrylic acid surface-modified with nucleoside Phenylboronic acid structure with boron affinity;

[0040] Add template uridine to the above phenylboronic acid structure in an amount of 0.25mmol, and let stand at 0°C for 4h; add 5.00mmol of cross-linking agent ethylene glycol dimethacrylate, and then add initiator azobisisobutyronitrile 0.457mmol, through N2 10min, stirred at 40°C for 1h; then, added 200mg of mesoporous molecular sieve MCM-48 to the system, ultrasonicated for 15min, and passed through N 2 Seal, stir at 40°C for 2h, at 65°C for 18h, and at 80°C for 6h to prepare polymer microspheres;

[0041] After the polymer microspheres prepared ...

Embodiment 2

[0054] Preparation of a Boron Affinity Hollow Molecularly Imprinted Solid Phase Extraction Column

[0055] Weigh 1.00mmol of monomeric methacrylic acid and 2.00mmol of 3-aminophenylboronic acid, mix the two evenly, and then dissolve them in 50mL of acetonitrile, stir at room temperature for 16h, and obtain methacrylic acid surface-modified with nucleoside Phenylboronic acid structure with boron affinity;

[0056] Add template uridine to the above phenylboronic acid structure, the addition amount is 0.4mmol, and stand at 20°C for 4h; add 4mmol of crosslinking agent ethylene glycol dimethacrylate, and then add initiator azobisisobutyronitrile 0.061 mmol, thru N 2 20min, stirring at 60°C for 2h; after that, add 400mg of mesoporous molecular sieve MCM-48 to the system, sonicate for 20min, pass N 2 Seal, stir at 60°C for 3h, at 80°C for 20h, and at 100°C for 6h to prepare polymer microspheres;

[0057] After the polymer microspheres prepared above were washed with ethanol by suc...

Embodiment 3

[0070] Preparation of a Boron Affinity Hollow Molecularly Imprinted Solid Phase Extraction Column

[0071] Weigh 1.00mmol of monomeric methacrylic acid and 3.00mmol of 3-aminophenylboronic acid, mix the two evenly, and then dissolve them in 60mL of acetonitrile, stir at room temperature for 18h, and obtain methacrylic acid surface-modified with nucleoside Phenylboronic acid structure with boron affinity;

[0072] Add template uridine to the above phenylboronic acid structure in an amount of 0.25 mmol, and let it stand at 30°C for 6 hours; add 10 mmol of crosslinking agent ethylene glycol dimethacrylate, and then add 0.12 mmol of initiator azobisisobutyronitrile , through N 2 30min, stirring at 80°C for 1h; after that, add 600mg of mesoporous molecular sieve MCM-48 to the system, ultrasonic for 30min, pass N 2 Seal, stir at 70°C for 4h, at 80°C for 20h, and at 90°C for 8h to prepare polymer microspheres;

[0073] After the polymer microspheres prepared above were washed with...

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Abstract

The invention provides hollow molecularly imprinted polymers which are modified by phenylboronic acid and an extraction column which is made by adopting the polymers. According to the synthetic method of the polymers, 3-aminophenylboronic acid is used as a modifying agent to conduct chemical modification on methacrylic acid monomers, uridine is used as a template, the modified methacrylic acid is used as functional monomers, matrixes, crosslinking agents and initiating agents are added to prepare molecularly imprinted materials, the prepared molecularly imprinted materials are subjected to template elution, the matrixes are corroded by adopting hydrofluoric acid, and the hollow molecularly imprinted polymers are obtained. The provided boron affinity hollow molecularly imprinted solid phase column has obvious enrichment effects on nucleoside type materials mainly due to the fact that molecular imprints conduct preferential adsorption on template molecules and structural analogues, and most binding sites of the hollow molecular imprints are distributed on surfaces of carrier matrix materials and in the hollow cavities and thus the adsorption efficiency is improved; furthermore, boric acid groups can carry out reversible adsorption and dissociation on the nucleoside type materials of a cis-diol structure, and therefore the boron affinity hollow molecularly imprinted solid phase column has obvious enrichment effects on the nucleoside type materials.

Description

technical field [0001] The invention belongs to the technical field of solid phase extraction, in particular to a method for preparing and using a hollow molecularly imprinted solid phase extraction column modified by phenylboronic acid, which is combined with a high performance liquid chromatography method for selective separation, enrichment and detection of drugs content of nucleosides in Background technique [0002] Molecular imprinting technology refers to the artificial method of preparing polymers that have specific binding effects on specific molecules in terms of spatial structure and binding sites. Molecularly imprinted polymers (MIPs) are a kind of "acceptor" with a three-dimensional spatial structure synthesized through the interaction between template molecules, functional monomers and cross-linking agents. "Memory" function, thus showing special affinity, high selectivity and excellent molecular recognition ability. Nevertheless, there are still some problem...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F230/06C08J9/26B01D15/22G01N30/60
CPCB01D15/22C08F222/1006C08F222/102C08J9/26C08J2201/0424C08J2335/02G01N30/60C08F230/06
Inventor 田苗苗胡月黄玮佟育奎夏琴飞
Owner HARBIN NORMAL UNIVERSITY
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