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Method for extracting and purifying Gypenoside from Gynostemma pentaphyllum

A technology of Gynostemma saponin and Gynostemma pentaphyllum is applied in the directions of pharmaceutical formulations, medical preparations containing active ingredients, plant raw materials, etc., which can solve the problems of high extraction production cost, difficult separation of saponin pigments, complicated processes, etc., and achieves reduction of extraction time and extraction. The number of times, is conducive to large-scale industrial production, the effect of reducing the amount of solvent

Active Publication Date: 2015-01-28
宁波中药制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to reports, the method used to extract gypenoside is relatively single, the yield of gypenoside is low, and the purity is low, and a series of complete extraction and separation methods have not been formed to be applied to industrial production.
[0005] In order to solve the above-mentioned technical problems of gypenoside extraction, the current extraction methods of gypenosides include water extraction, organic solvent extraction, microwave-assisted extraction, ultrasonic-assisted extraction, and enzymatic extraction. For specific patent applications, please refer to the application Patent applications No. 201310470936.6 and 201210125255.1, but the extraction yields of the total glycosides of Gynostemma pentaphylla by these methods are not high, and the production cost of extracting active ingredients in Gynostemma pentaphyllum is relatively high, and the extraction technology needs to be further improved
In addition, such as a Chinese invention patent application with an application number of 201010105011.8 "A Method for Extracting Total Gynosides from Gynostemma Gynostemma", which uses lye boiling extraction and resin chromatography to extract high-purity Gynostemma saponins from Gynostemma pentaphyllum, which solves the problem of the extreme saponins contained in Gynostemma pentaphyllum. However, by heating and extracting in a weakly alkaline medium, and then using resin trees and activated carbon to decolorize, the process is complicated and the production cost is high. Therefore, it is necessary to further improve the extraction and purification process of gypenoside

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Extraction:

[0028] Crush the rhizome of Gynostemma pentaphyllum into coarse powder, pass through a 10-mesh sieve, take 100kg of coarse powder and put it in the extraction tank, mix Gynostemma pentaphyllum powder and ethanol with a concentration of 65% in a ratio of 1:4 by weight, stir evenly and heat at 80°C Under reflux extraction for 3 times, each time for 1.5 hours, the extracts were filtered to remove the residue and combined, the combined filtrate was concentrated under reduced pressure at 55°C, the vacuum pressure during the reduced pressure concentration process was -0.07Mpa, and the filtrate was concentrated to alcohol-free.

[0029] (2) Resin purification:

[0030] Dilute the concentrated solution of step (1), dilute the concentrated solution until the weight ratio of Gynostemma pentaphyllum rhizome and the diluted solution is 1:1, use the macroporous resin of D101 to absorb and saturate, and the column flow rate is 1BV / h. The resin adsorbed to saturati...

Embodiment 2

[0034] (1) Extraction:

[0035] Crush the rhizome of Gynostemma pentaphylla into coarse powder, pass through a 15-mesh sieve, take 200kg of coarse powder and put it in the extraction tank, mix Gynostemma pentaphyllum powder and ethanol with a concentration of 75% in a ratio of 1:3 by weight, stir evenly and heat at 85°C Under reflux extraction for 3 times, each time for 2 hours, the extracts were filtered to remove the slag and combined, the combined filtrate was concentrated under reduced pressure at 60°C, the vacuum pressure during the reduced pressure concentration process was -0.095Mpa, and the filtrate was concentrated to alcohol-free.

[0036] (2) Resin purification:

[0037] Dilute the concentrated solution of step (1), dilute the concentrated solution until the weight ratio of Gynostemma pentaphyllum rhizome and the diluted solution is 1:2, use the macroporous resin of D130 to absorb and saturate, and the column flow rate is 2BV / h. The resin adsorbed to saturation is...

Embodiment 3

[0041] (1) Extraction:

[0042]Crush the rhizome of Gynostemma pentaphyllum into coarse powder, pass through a 20-mesh sieve, take 300kg of coarse powder and put it in the extraction tank, mix Gynostemma pentaphyllum powder and ethanol with a concentration of 65% in a ratio of 1:6 by weight, stir evenly and heat at 82°C Under reflux extraction for 3 times, each time for 1.8 hours, the extracts were filtered to remove the residue and combined, the combined filtrate was concentrated under reduced pressure at 70°C, the vacuum pressure during the reduced pressure concentration process was -0.08Mpa, and the filtrate was concentrated to alcohol-free.

[0043] (2) Resin purification:

[0044] Dilute the concentrated solution of step (1), dilute the concentrated solution until the weight ratio of Gynostemma pentaphyllum rhizome and the diluted solution is 1:2, use the macroporous resin model AB-8 to absorb and saturate, and the column flow rate is 2BV / h , the resin adsorbed to satur...

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Abstract

The invention relates to a method for extracting and purifying Gypenoside from Gynostemma pentaphyllum. The method is as below: crushing and sieving Gynostemma pentaphyllum, extracting by ethanol, and filtering and concentrating an extracted liquid to an alcohol-free state; passing the concentrated liquid through macroporous resin for adsorption, eluting by water to a clarified state, eluting by alcohol solution, and concentrating the eluent to an alcohol-free state; extracting the concentrated liquid with an organic solvent, concentrating and drying, and at the same time recovering the organic solvent. The invention has the advantages of simple process, reasonable technology and economical affordability; the adsorption-extraction combined technology is employed to obtain a product with high purity. The method adapts to the production of small and medium-sized enterprises, and reduces the equipment required by production and the cost of production.

Description

technical field [0001] The invention relates to the purification, separation and purification of natural compounds, in particular to a method for extracting and purifying gypenoside from gynostemma rhizome raw materials. Background technique [0002] Gynostemma pentaphyllum (Gynostemma pentaphyllum), also known as seven-leaf gallbladder, five-leaf ginseng, seven-leaf ginseng, etc., is a perennial herbaceous vine of the genus Gynostemma cucurbitaceae. It is distributed in India, Sri Lanka, Nepal, Myanmar, Indochina Peninsula, Malaysia, the Philippines, and North Korea. And Japan and other regions, distributed in the southwest of China, among which Yunnan is the most widely distributed, the most abundant resources, the most species, most of which are distributed at an altitude of 1000 ~ 2000m. Gynostemma is mostly bitter and sweet, chewing refreshing, the whole herb can be used as medicine, pharmacological Studies have proved that Gynostemma pentaphyllum has no toxic and side ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/424
CPCA61K36/424A61K2236/15A61K2236/333A61K2236/39A61K2236/51
Inventor 董玲燕赵丽娟杨盛鑫何敏菲方明
Owner 宁波中药制药股份有限公司
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