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Preparation method of gallocatechin gallate

A technology of gallocatechin and gallic acid ester, applied in the field of medicine and chemical industry, can solve the problems of poor environment and product quality, inconvenient operation and application, complicated operation steps, etc., achieve low reaction conversion efficiency, reduce risk factor, and process The effect of cycle shortening

Pending Publication Date: 2021-06-18
JIANGSU TIANSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although this invention patent discloses a feasible method for preparing gallocatechin gallate, it is not difficult to find from its examples that the reaction conditions required by the method are continuous high-temperature reactions, and the reaction duration is mostly between About 5 days, the process cycle is long, the cost is high, and it causes great inconvenience to the actual operation and application
In addition, organic reagents such as ethyl acetate and n-butanol are repeatedly used in the subsequent purification process, which has a bad impact on the environment and product quality; moreover, the selection of macroporous adsorption resin column chromatography requires at least The elution treatment of four gradients of different solutions is complicated, and a large amount of acid-base and alcohol solutions are required to regenerate the resin column, causing serious environmental pressure

Method used

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  • Preparation method of gallocatechin gallate
  • Preparation method of gallocatechin gallate
  • Preparation method of gallocatechin gallate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 50g of EGCG powder as a raw material, add 2500ml of 0.001mol / L hydrochloric acid solution to dissolve, gradually heat to 100°C, stir and react for 16 hours, stop heating and cool to room temperature, add 0.001mol / L sodium hydroxide solution to adjust the pH to near Neutral to obtain the post-reaction solution; gradually add the post-reaction solution to the chromatographic column equipped with PS-DVB microspheres that have been treated (the particle size range of the microspheres is 100-200um, and the column volume is 2500ml), and then Elute with 5% ethanol solution until there is no obvious GCG outflow, receive the eluent according to the outflow of every 0.5 column volume, detect and select the eluent containing the target component by thin layer, concentrate and remove alcohol, and place it for crystallization. That is, 16.2 g of white powder was obtained.

[0032] After identification, the white powder obtained in this example was determined to be GCG (gallocat...

Embodiment 2

[0034] Take 50g of EGCG powder as a raw material, add 100ml of 0.1mol / L acetic acid solution to dissolve, gradually heat to 60°C, stir and react for 4 hours, stop heating and cool to room temperature, add 0.1mol / L sodium hydroxide solution to adjust the pH to near Neutral to obtain the post-reaction solution; gradually add the post-reaction solution into the chromatographic column that has been treated with PS-DVB microspheres (the particle size range of the microspheres is 20-40um, and the column volume is 250ml), and then Use 5% methanol solution to elute until there is no obvious GCG outflow, receive the eluent according to the outflow of every 0.5 column volume, perform thin-layer detection and select the eluent containing the target component, concentrate and remove alcohol, and place it for crystallization. That is, 24.1 g of gallocatechin gallate white powder was obtained, and its purity was 96.0% as detected by HPLC.

Embodiment 3

[0036] Take 50g of EGCG powder as a raw material, add 500ml of 0.01mol / L phosphoric acid solution to dissolve, gradually heat to 80°C, stir and react for 10 hours, stop heating and cool to room temperature, add 0.01mol / L sodium hydroxide solution to adjust the pH to near Neutral to obtain the post-reaction solution; gradually add the post-reaction solution into the chromatographic column equipped with PS-DVB microspheres that have been treated (the particle size range of the microspheres is 60-100um, and the column volume is 500ml), and then Use 30% ethanol solution to elute until there is no obvious GCG outflow, receive the eluent according to the outflow of every 0.5 column volume, perform TLC detection and select the eluent containing the target component, concentrate and remove alcohol, and place it for crystallization. That is, 15.9 g of gallocatechin gallate white powder was obtained, and its purity was 95.8% as detected by HPLC.

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Abstract

The invention discloses a preparation method of gallocatechin gallate, which comprises the following steps: by taking EGCG (epigallocatechin gallate) as a raw material, adding an acid solution with a certain concentration according to a proper proportion for dissolving, conducting gradually heating and stirring to react for a certain time, and conducting cooling to room temperature; adding alkali liquor with the same concentration to adjust the pH to be nearly neutral to obtain a solution after reaction; gradually adding the reacted solution into a treated chromatographic column filled with PS-DVB microspheres, and then conducting eluting with an alcoholic solution until no obvious GCG flows out; receiving eluate according to the outflow volume per 0.5 column volume, performing thin-layer detection and selecting the eluate containing the target component; and conducting concentration and alcohol removal, then conducting standing and crystallization to obtain gallocatechin gallate. Therefore, a more efficient way is provided for preparing high-purity GCG.

Description

technical field [0001] The invention relates to a preparation method of gallocatechin gallate, which belongs to the field of medicine and chemical industry. Background technique [0002] Gallocatechin gallate (EGCG) is one of the main catechins in tea. As a natural antioxidant and free radical scavenger, it has obvious anti-aging, anti-mutation, anti-cancer and anti-cancer, prevention of cardiovascular diseases, Radiation protection and other biological activities are widely used in the fields of food processing, medicine and health care, and daily chemical industry. However, due to its unstable characteristics, it is easily affected by environmental factors, such as being easily oxidized in the air, easily decomposed in alkali, and poor in stability under high temperature conditions. [0003] Gallocatechin gallate (GCG) is an isomer of EGCG, which exists in a very small amount in natural green tea, and it is difficult to obtain GCG with high purity directly from green tea,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62
CPCC07D311/62
Inventor 季浩卢魏魏刘佳阚建伟窦长清
Owner JIANGSU TIANSHENG PHARMA
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