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Artemisinin molecule imprinting polymer on surface of porous microsphere silica gel as well as preparation and application methods thereof

A technology of porous microspheres and molecular imprinting, applied in organic chemistry, bulk chemical production, etc., can solve the problems of low adsorption capacity, non-specific adsorption, slow diffusion, long mass transfer time, etc., and achieve simple, convenient and specific preparation methods Effect of adsorption and selectivity, good mechanical stability

Inactive Publication Date: 2010-09-29
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the current development of molecular imprinting technology is relatively fast, there are still many problems: slow diffusion of sample molecules in imprinted adsorbents, long mass transfer time, low adsorption capacity, and non-specific adsorption.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1 Synthesis example of artemisinin molecularly imprinted polymer

[0019] 1. Silicone modification

[0020] Put 50g of silica gel into a 500mL round bottom flask, add 200mL of a mixed solution of hydrochloric acid / deionized water with a volume ratio of 1:1, stir and reflux on an electric heating pot for 8h (about 110°C). After reflux, let it stand overnight, cool the silica gel and hydrochloric acid solution to room temperature, remove the hydrochloric acid solution by suction filtration, rinse the silica gel repeatedly with deionized water, and then wash it with an appropriate amount of methanol. Finally, collect the silica gel and dry it in a vacuum oven. The dried silica gel was placed in an infrared electric oven and activated at 200°C for 12h. Weigh 30g of activated silica gel and put it into a 250mL Erlenmeyer flask with a stopper, add 150mL of toluene, 15mL of vinyltriethoxysilane (VTES), 10mL of pyridine, and 3mL of triethylamine, and ultrasonically vi...

Embodiment 2

[0023] Example 2 Examples of adsorption experiments under normal pressure and temperature conditions

[0024] 1. Adsorption kinetics experiment, with artemisinin as the target, 200 mg of artemisinin molecularly imprinted polymer was dispersed in 20 mL of artemisinin toluene solution with an initial concentration of 2 mg / mL, sealed, placed on an air bath shaker, Oscillating adsorption at 30°C, sampling and testing every hour, the adsorption of artemisinin by molecularly imprinted polymer reached equilibrium in about 10 hours.

[0025] 2. Equilibrium binding experiment, with artemisinin as the target, 50 mg of artemisinin molecularly imprinted polymer was dispersed in 5 mL of artemisinin toluene solution with different initial concentrations (0.2-2 mg / mL), sealed and placed in an air bath On a shaking table, shake and adsorb at 30°C for at least 18 hours. Sampling and testing show that the maximum adsorption amount of artemisinin by molecularly imprinted polymers is about 32.4...

Embodiment 3

[0027] Example 3 Examples of Adsorption Experiments Under Supercritical Conditions

[0028] 1. Adsorption kinetics experiment, with artemisinin as the target, 0.02g artemisinin and about 0.2g artemisinin molecularly imprinted polymer were placed in supercritical CO 2 Under the conditions, the adsorption is carried out at a temperature of 313K and a pressure of 20MPa, sampling and testing every 15-30 minutes, and the adsorption reaches equilibrium in about 3 hours.

[0029] 2. Equilibrium binding experiment, with artemisinin as the target, 0.02g artemisinin and about 0.2g artemisinin molecularly imprinted polymer were placed in supercritical CO 2 Under the condition of adsorption under the conditions of temperature 313K and pressure 20MPa for more than 3 hours, the adsorption amount of artemisinin by molecularly imprinted polymer of artemisinin has exceeded 100mg / g.

[0030] 3. Selectivity evaluation experiment, with artemisinin and artemether as targets, 0.015g artemisinin ...

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Abstract

The invention relates to an artemisinin molecule imprinting polymer on the surface of porous microsphere silica gel. The artemisinin molecule imprinting polymer is prepared by adopting the steps of: selecting the porous microsphere silica gel as a basal material, taking vinyl triethoxysilane as a coupling agent, artemisinin as a template molecule, methacrylate and acrylamide as functional monomers, ethylene glycol dimethacrylate as a cross-linking agent and azodiisobutyronitrile as an initiating agent, preparing a polymer and removing the artemisinin in the polymer. The invention also provides a preparation method and an application method of the artemisinin molecule imprinting polymer on the surface of the porous microsphere silica gel. The artemisinin molecule imprinting polymer on the surface of the porous microsphere silica gel can separate the artemisinin from other structural analogues, such as artemether, and the like under normal pressure and temperature and supercritical conditions, is especially suitable for supercritical conditions and has specific adsorption property, selectivity and favorable mechanical stability; and the preparation method is simple, convenient and suitable for large-scale 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 artemisinin molecularly imprinted polymers, in particular to an artemisinin molecularly imprinted polymer on the surface of porous microsphere silica gel and its preparation and application method, especially suitable for supercritical Conditions for separation and purification of artemisinin. Background technique [0002] Artemisia annua L (Chinese medicine Artemisia annua) has been used as an antimalarial traditional Chinese medicine for more than 2,000 years in China. Chinese scientists isolated a new type of sesquiterpene lactone containing peroxy groups for the first time in the 1970s, and named it artemisinin (Artemisinin; Arteannuin; Qinghaosu; AR). Artemisinin is an effective antimalarial ingredient with a unique structure and a special antimalarial mechanism, and it has special effects against chloroquine-induced falciparum ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F2/44C08F220/06C08F220/56C08J9/26C07D493/20
CPCY02P20/54
Inventor 曹学君龚小雁郁晓娟
Owner EAST CHINA UNIV OF SCI & TECH
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