Epigallo-catechin gallate (EGCG) with high purity and preparation method thereof

A technology of epigallocatechin and gallate, which is applied in the field of pharmaceutical compositions with epigallocatechin gallate as the main component, epigallocatechin gallate and its preparation, can solve technical problems Difficulty in large-scale industrial production, inability to carry out industrial production, and inability to use industrial production to achieve good market advantages, low production costs, and good stability

Active Publication Date: 2010-02-10
JIANGSU TIANSHENG PHARMA
View PDF3 Cites 30 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although there are many preparation technologies for epigallocatechin gallate (EGCG) reported in the literature or disclosed in patents, most of the technologies belong to the level of laboratory preparation, and the preparation amount is usually between milligrams and several grams. With only tens of grams of preparation, these technologies are difficult to carry out large-scale industrial production, and they are far from meeting the growing market demand
[0006] For example, in the invention patent of "purification method of epigallocatechin gallate monomer" with the patent number of CN 1193994C, a high-content purification method of epigallocatechin gallate is disclosed. Sephadex LH-20 was used for separation and purification. Although a small amount of epigallocatechin gallate monomer was also prepared, it is well known that Sephadex LH-20 is an expensive separation material. The price per kilogram is tens of thousands of RMB. Generally, it is only suitable for the separation of a small amount of reference substance in the laboratory. Obviously, this technology cannot be used in industrial production.
There are also many such disclosed technologies, such as the patent No. CN 1164583C "separation and preparation process of epigallocatechin gallate", using high performance liquid chromatography (HPLC) to prepare column separation, the separation material selected is expensive C 18 , also belongs to the category of laboratory separation, and the preparation amount is usually only at the level of milligrams to several grams, which cannot be industrialized
[0007] The technologies cited above are not practical. In addition, although there are many technologies disclosed in documents and patents that have certain practicability, the process is complicated and the production cost is high.
For example, in the invention patent of "a purification method of epigallocatechin gallate monomer" with the patent number CN 1733753A, methods such as microporous membrane filtration and freeze-drying were used to purify epigallocatechin gallate. The preparation of ester monomers, the production cost will obviously be very high
In addition, there is also a method for preparing epigallocatechin gallate monomers by using inorganic salts such as aluminum salts, calcium salts, and magnesium salts for complex precipitation, which will inevitably bring a certain degree of pollution during the production process. And the production cost is relatively high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 10 kg of crude tea polyphenols (with an EGCG content of 40.4%), add 100 L of purified water, soak and stir at 45°C for extraction twice, each time for 0.5 hours, combine the extracts, filter, and discard the residue;

[0036] After the extract was concentrated to 50L under reduced pressure at 60°C, 50L ethyl acetate was added for liquid-liquid extraction twice, the ethyl acetate layer was combined and recovered under reduced pressure at 60°C to a thick paste, and 50L purified water was added to dissolve to obtain tea Polyphenol sample solution.

[0037] Pass the above tea polyphenol sample solution through a tandem chromatographic column equipped with 100-200 mesh polyamide (front column) and HPD-100 macroporous adsorption resin (back column), add 100L of purified water to fully elute, and remove In series, add 100L of 20% ethanol to the back column (HPD-100 macroporous adsorption resin column) for desorption and elution, collect the eluate, and obtain an epigalloc...

Embodiment 2

[0041] Take 10 kg of crude tea polyphenols (with an EGCG content of 45.1%), add 50 L of ethanol (concentration: 10%), soak and stir at 45°C for 3 times, each time for 1 hour, combine the extracts, filter, and discard the residue;

[0042] After the extract was concentrated to 50L under reduced pressure at 55°C, 50L ethyl acetate was added for liquid-liquid extraction three times, the ethyl acetate layers were combined and recovered under reduced pressure at 50°C to a thick paste, and dissolved in 100L purified water to obtain tea Polyphenol sample solution.

[0043] Pass the above-mentioned tea polyphenol sample solution through a tandem chromatography column equipped with 30-100 mesh polyamide (front column) and D101 macroporous adsorption resin (rear column) respectively, add 80L of purified water for sufficient elution, and release the tandem column. Add 70L of 30% ethanol to the back column (D101 macroporous adsorption resin column) for desorption and elution, and collect ...

Embodiment 3

[0047] Take 50 kg of crude tea polyphenols (with an EGCG content of 35.4%), add 300 L of purified water, soak and stir at 40°C for extraction twice, each time for 1 hour, combine the extracts, filter, and discard the residue;

[0048] After the extract was concentrated to 300L under reduced pressure at 65°C, 300L ethyl acetate was added for liquid-liquid extraction twice, the ethyl acetate layer was combined and recovered under reduced pressure at 50°C to a thick paste, and 600L purified water was added to dissolve to obtain tea Polyphenol sample solution.

[0049] The above-mentioned tea polyphenol sample solution is passed through the tandem chromatographic columns respectively equipped with model HPD-100 macroporous adsorption resin (front column) and D101 macroporous adsorption resin (back column), after adding 500 L of purified water to fully elute, Remove the series connection, add 400L of 25% ethanol to the back column (D101 macroporous adsorption resin column) for deso...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
particle sizeaaaaaaaaaa
Login to view more

Abstract

The invention provides an epigallo-catechin gallate (EGCG) with high purity and a preparation method thereof. The EGCG content is 98.0 percent to 99.9 percent. The preparation method mainly comprisesthe working procedures of extracting, separating by a chromatography and crystallizing. The invention has favorable reproducibility of preparation process, high acquired EGCG content, low cost and stable and controllable quality and is suitable for industrialized production.

Description

technical field [0001] The invention discloses a high-purity epigallocatechin gallate (EGCG) and a preparation method thereof, and a pharmaceutical composition mainly composed of the epigallocatechin gallate. The invention belongs to the field of medicine and health care. Background technique [0002] Tea polyphenols are a kind of polyphenols extracted from green tea. It is composed of more than six monomers, of which epigallocatechin gallate (EGCG) is the main active with the highest content and the strongest activity. Element. Because of its special polyhydroxyl chemical structure, epigallocatechin gallate has very strong antioxidant activity, can protect cells and DNA from damage, and plays an important role in anti-cancer and cardiovascular diseases. Studies have shown that EGCG has significant anti-oxidation, scavenging free radicals in the body, anti-tumor, anti-mutation, anti-aging, anti-inflammation, anti-virus and a series of biological activities. Cerebral throm...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62A61K31/353B01D15/08A61P39/06A61P31/12A61P31/04A61P9/00A61P35/00
Inventor 季浩刘佳
Owner JIANGSU TIANSHENG PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap