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Method for preparing high-purity EGCG from hydrogen-bonded macroporous resin

A macroporous resin and high-purity technology, applied in the field of preparation of high-purity EGCG, can solve the problems that toxic chemical reagents cannot be guaranteed and are not suitable for large-scale production

Inactive Publication Date: 2015-03-25
中国医科大学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention provides a method for preparing high-purity EGCG with a hydrogen-bonding macroporous resin. The purpose of the method is that in the previous preparation process, there were problems such as toxic chemical reagents that could not guarantee drug safety, and were not suitable for large-scale production.

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  • Method for preparing high-purity EGCG from hydrogen-bonded macroporous resin
  • Method for preparing high-purity EGCG from hydrogen-bonded macroporous resin
  • Method for preparing high-purity EGCG from hydrogen-bonded macroporous resin

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specific Embodiment approach

[0023] Detailed ways: The present invention is described in detail through the following examples, but the technical solution of the present invention is not limited to the following examples.

[0024] Among the present invention, the HPLC assay method is as follows:

[0025] Type of instrument used: high performance liquid chromatography Elution method: gradient elution;

[0026] Detector: UV detector Instrument model: Agilent 1200;

[0027] Detection wavelength: 278nm Injection volume: 20μL Flow rate: 1mL / min;

[0028] Column temperature: 30°C Column type: Diamonsil C18 column (150mm×4.6mm, 5μm);

[0029] Integral method: area normalization method.

[0030] Liquid chromatography gradient elution process:

[0031] time (min) Methanol (A) 0.8% glacial acetic acid in water (B) 0 10 90 1 15 85 11 18 82 21 21 79 51 70 30

Embodiment 1

[0033] Take 500g of green tea, add 10L of water, heat to 60°C for extraction, extract for 1 hour, extract 3 times, add the extract to the treated HPD-826 hydrogen bond type macroporous adsorption resin column for adsorption, wash with 5 BV of water Removed, discarded, and then eluted with 5 BV 20% ethanol water, recovered the solvent, discarded the residue, then eluted with 10 BV 30% ethanol water, collected 30% eluate, concentrated under reduced pressure, and freeze-dried to obtain EGCG crude product 10.69g, such as image 3 shown; the crude product was recrystallized with ethanol:water:acetic acid (9:1:1) to obtain 6.94g of EGCG, and the content of EGCG was 98.60% by HPLC analysis, as attached Figure 4 shown.

Embodiment 2

[0035] Take 500g of green tea, add 20L of water, heat to 70°C for extraction, extract for 2 hours, extract 3 times, add the extract to the treated HPD-200 hydrogen bond type macroporous adsorption resin column for adsorption, and elute with 5BV of water , discarded, and then eluted with 5 BV of 20% ethanol water, the solvent was recovered, the residue was discarded, and then eluted with 10 BV of 30% ethanol water, the 30% eluate was collected, concentrated under reduced pressure, and freeze-dried to obtain EGCG crude product 15.85g, the crude product was recrystallized with ethanol:water:acetic acid (8:2:1) to obtain 9.12g of EGCG, the content of EGCG was 98.32% by HPLC analysis.

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Abstract

The invention provides a method for preparing high-purity EGCG from a hydrogen-bonded macroporous resin, aiming to solve the problems that toxic chemical reagents are adopted by the existing methods for preparing EGCG so that the safety of medicines can not be guaranteed, and the existing methods for preparing EGCG are not suitable for large-scale production. The method is characterized by comprising the following steps: (1) weighing green tea, adding an appropriate amount of distilled water, heating the green tea to the temperature of 60-80 DEG C, and extracting to obtain green-tea extract; (2) adsorbing the green-tea extract with the hydrogen-bonded macroporous adsorption resin directly, eluting with 10-20% ethanol water to remove impurities, further eluting with 30% ethanol water, and collecting eluate; and (3) concentrating the eluate, freeze-drying, and recrystallizing to obtain the finished product. The macroporous resin can be recycled, the method is simple in technical route, is low in cost and is high in separation efficiency, is environment-friendly and is suitable for the industrial production of EGCG.

Description

technical field [0001] What this patent relates to is a kind of preparation method that can be used as the raw material medicine of pharmaceutical industry, what specifically relates to is the preparation method of high-purity EGCG. Background technique [0002] Green tea is a beverage commonly used in East Asian countries for its health benefits, and was also used as a traditional Chinese medicine in ancient China. EGCG is a member of the catechin family and is the most abundant polyphenolic compound in green tea. EGCG has a large number of phenolic hydroxyl groups and is often used as a natural antioxidant in the medical field, food field, and cosmetic field. Pharmacological experiments show that EGCG has a variety of biological activities, including its anti-oxidation, anti-inflammation, anti-mutation, anti-cancer, and anti-HIV effects. Recently, our research group found that EGCG can treat Alzheimer's disease caused by β-amyloid (Aβ) peptide and neuronal loss. Therefo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62
CPCC07D311/62
Inventor 魏敏杰靳鑫刘明妍高华姚维范毛瑞琨杨时伦
Owner 中国医科大学
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