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Molecular imprinted polymer, preparation method and application thereof

A technology of ursodeoxycholic acid and porous silica gel, which is applied in the field of molecularly imprinted polymers to achieve the effects of large specific surface area, stable chemical properties and excellent stability

Active Publication Date: 2012-07-04
ZHONGSHAN BAILING BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For various types of bile acid compounds with similar structures, the traditional separation methods are not satisfactory, and it is of great practical significance to seek a cost-effective and effective UDCA separation and purification method

Method used

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  • Molecular imprinted polymer, preparation method and application thereof
  • Molecular imprinted polymer, preparation method and application thereof
  • Molecular imprinted polymer, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1 Preparation of ursodeoxycholic acid molecularly imprinted polymers on porous silica surface by initiating polymerization in solution

[0040] (1) Activation of silica gel

[0041] Weigh about 50g of coarse-porous microsphere silica gel (80-100 mesh) into a 500ml round bottom flask, add 200ml of nitric acid aqueous solution with a volume ratio of 1:1 and soak for 24h, or condense and reflux on a heating mantle for 8h to increase the amount of silica gel The number of surface hydroxyl groups. Stand overnight, remove the acid solution by suction filtration with a sand core funnel, then wash with deionized water until the pH is neutral, then wash the silica gel with methanol to remove organic impurities in the silica gel, and then collect the silica gel in a vacuum oven at 60°C for drying Finally, place the dried silica gel in an infrared electric oven and activate it at 110°C for 12 hours to remove the physical water on the silica gel surface. The scanning el...

Embodiment 2

[0048] Example 2 Preparation of ursodeoxycholic acid molecularly imprinted polymer on porous silica surface by initiating polymerization on silica gel surface

[0049] (1) Activation of silica gel: with embodiment 1 (1).

[0050] (2) Functional modification of silica gel surface

[0051] Weigh 12g of activated silica gel, add it to a 250mL Erlenmeyer flask with a stopper, add 100ml of toluene, 20mmol of γ-glycidyl ether propyl trimethoxysilane (GPS) and 1ml of triethylamine, and oscillate ultrasonically for 5min in an ultrasonic cleaner , so that the solution system is fully mixed, and the silica gel is fully dispersed in the solution. The system was ventilated with nitrogen for 10 minutes, then sealed, placed in a water-bath shaker at 80° C., and reacted at 280 rpm for 24 hours. After the reaction was completed, the reaction solution was removed by suction filtration with a sand core funnel, washed with toluene, ether, and acetone several times in sequence to remove resid...

Embodiment 3

[0056] Example 3 Adsorption kinetics test

[0057] Prepare a solution of UDCA in acetone with a concentration of 1 mg / ml. Weigh 0.5g of the imprinted polymers prepared in Example 1 and Example 2 respectively and place them in a 100ml conical flask with a stopper, add 40ml of prepared UDCA acetone solution respectively, place them in a 150rpm air bath shaker at room temperature to vibrate and adsorb, and The supernatant was taken to measure the concentration of UDCA, and the adsorption amount of the imprinted polymer to the template molecule was calculated at different times. The imprinted polymer prepared by the present invention can reach adsorption equilibrium after adsorption for 12 hours.

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Abstract

The invention relates to a porous silica gel silicon face ursodesoxycholic acid molecular imprinted polymer which is prepared by the steps of carrying out polymerization to obtain a polymer in an inert solvent under the action of a cross-linking agent by using ursodesoxycholic acid as a template molecule and acrylamide as a functional monomer in the presence of a functionalized porous silica particle modified with a coupling agent on the surface and an initiating agent or a functionalized porous silica gel particle grafted with the initiating agent through the coupling and removing the ursodesoxycholic acid in the polymer. The invention also relates to a preparation method comprising the steps of initiating the polymerization in a solution and initiating polymerization on the surface of silica gel. The invention also relates to relevant applications. The porous silica gel silicon face ursodesoxycholic acid molecular imprinted polymer has high adsorption capacity, high selective absorption property and excellent stability on the ursodesoxycholic acid, can effectively separate the ursodesoxycholic acid in bile acid analogues, and has the function of guiding the massive production ofthe ursodesoxycholic acid; and the preparation method is simple and convenient and is suitable for massive popularization and application.

Description

technical field [0001] The invention relates to the technical field of molecularly imprinted polymers, in particular to the technical field of ursodeoxycholic acid molecularly imprinted polymers, in particular to a porous silica surface ursodeoxycholic acid molecularly imprinted polymer and its preparation and application, suitable for separation Purification of ursodeoxycholic acid. Background technique [0002] Ursodeoxycholic acid (3α, 7β-Dihydroxy-5β-cholan-24-oicacid, Ursodeoxycholic Acid, UDCA), whose structural formula is shown in formula (1), is a hydrophilic cholic acid that exists in normal human bile , accounting for about 3% of the total bile acid in the human body. It has the functions of relaxing the common bile duct sphincter, promoting glycogen accumulation in the liver, protecting the liver and detoxifying, and is used in the treatment of primary biliary cirrhosis and primary sclerosing cholangitis. It is FDA-approved for the treatment of primary biliary ci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F220/56C08F222/14C08F2/44C08J9/26B01J20/26B01J20/28B01J20/30
Inventor 曹学君朱建良
Owner ZHONGSHAN BAILING BIOTECHNOLOGY CO LTD
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