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A kind of acetyl ginsenoside rd and preparation method thereof

A technology of acetylated ginseng saponins, applied in chemical instruments and methods, glycoside steroids, steroids, etc., can solve the problems of prone to hydrolysis reaction and instability of acetyl group, shorten the operation steps, simplify the extraction process, Simple effect of separation process

Inactive Publication Date: 2017-07-11
吉林省参威人参产品科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the acetyl group in the molecule is unstable and prone to hydrolysis
[0003] Acetyl ginsenosides that have been separated mainly include Ac-Rg 1 , 20(S)-Ac-Rg 2 , 20(R)-Ac-Rg 2 , Acetyl ginsenoside Rd has been obtained by means of acetylation reaction, but its monomer has not been isolated from natural plants

Method used

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  • A kind of acetyl ginsenoside rd and preparation method thereof
  • A kind of acetyl ginsenoside rd and preparation method thereof
  • A kind of acetyl ginsenoside rd and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 4Kg of freshly dried ginseng flower buds, pulverize, add 12L of pure methanol solution, heat and reflux for 5 times, 2h each time, centrifugal filter, remove the residue to obtain a filtrate, the filtrate is recovered at 50 ℃ methanol, and concentrated under reduced pressure to prepare. The extract has a relative density of 1.1. Add 0.2 times the amount of water to the extract to disperse and dissolve. After extracting with cyclohexane and ethyl acetate in turn, recover the aqueous layer extract, and add the obtained extract to the macroporous adsorption solution. Adsorption was carried out on the resin Diaion HP-20. First, saccharides and inorganic salts in the extract were eluted with water, and then 60% methanol was used to enrich the acetyl ginsenoside Rd. The obtained enrichment solution was passed through a medium pressure MCI GEL column. Partial pigments and impurities were removed by analysis, and eluted with methanol water (60%, 80%) at a flow rate of 5 mL...

Embodiment 2

[0030] Weigh 4Kg of freshly dried ginseng flower buds, pulverize, add 16L of pure methanol solution, extract by heating under reflux for 4 times, 2h each time, centrifugal filter, remove the residue to obtain a filtrate, recover methanol at 50 ℃, and concentrate under reduced pressure to prepare. To form an extract with a relative density of 1.1, add 0.3 times the amount of water to the extract to disperse and dissolve, extract with cyclohexane and ethyl acetate in turn, recover the aqueous layer extract, and add the obtained extract to the macroporous adsorption solution. Adsorption was carried out on resin D101. First, saccharides and inorganic salts in the extract were eluted with water, and then 60% methanol was used to elute and enrich acetyl ginsenoside Rd. The obtained enrichment solution was subjected to medium pressure MCI GEL column chromatography to remove part Pigments and impurities were eluted with methanol water (60%, 80%), the flow rate was 6 mL / min, and the elu...

Embodiment 3

[0032] Weigh 4Kg of freshly dried ginseng flower buds, pulverize, add 20L of pure methanol solution, heat and reflux for extraction 3 times, 2h each time, centrifugal filtration, remove the residue, and obtain a filtrate. The filtrate is recovered at 50 °C with methanol, and concentrated under reduced pressure to prepare. To form an extract with a relative density of 1.1, add 0.5 times the amount of water to the extract to disperse and dissolve, extract with cyclohexane and ethyl acetate in turn, recover the aqueous layer extract, and add the obtained extract to the macroporous adsorption solution. Adsorption is carried out on resin HPD100. First, the sugars and inorganic salts in the extract are eluted with water, and then 60% methanol is used to elute and enrich the acetyl ginsenoside Rd. The obtained enrichment solution is removed by medium pressure MCI GEL column chromatography. Pigments and impurities were eluted with methanol water (60%, 80%), the flow rate was 8 mL / min, ...

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Abstract

The invention discloses acetyl ginsenoside Rd and a preparation method thereof. The preparation method comprises the following steps: 1), extracting: crushing ginseng buds, extracting with methanol solution, and concentrating under reduced pressure; 2), extracting: adding distilled water to concentrate extract for dissolving, extracting sequentially by using cyclohexane and ethyl acetate, and recycling a solvent from residual extract under reduced pressure; 3), enriching: adding obtained extract liquid into a macroporous adsorbing resin column for adsorbing, washing, and eluting with 60% methanol to obtain enrichment containing acetyl ginsenoside Rd; 4), performing medium-pressure MCI GEL column chromatography: subjecting the enrichment to MCI GEL column chromatography to remove part of pigments and impurities; 5), preparing: concentrating above eluent with a rotary evaporator under reduced pressure, then preparing a liquid efficiently, and eluting with methanol water. The method has the advantages of good simplicity of separation, high speed, good economy and high performance.

Description

technical field [0001] The invention discloses a preparation method for extracting and separating acetyl ginsenoside Rd (Ac-Rd) from ginseng flower buds, and belongs to the technical field of traditional Chinese medicine monomer extraction. Background technique [0002] Ginsenosides are the main active components of ginseng. Ginsenosides are contained in the roots, stems, leaves, flowers and fruits of ginseng, but the types and contents of ginsenosides in different parts are different. The aerial part of ginseng is a valuable resource that cannot be ignored. Among them, ginseng flower buds are the budding flowers of ginseng. The total saponin content in ginseng flowers is the highest (about 5-7%), and the content of some monomer saponins is more than ten times that in ginseng roots. (such as ginsenoside Re). The study found that the pharmacological activity of the saponins in the aerial parts of ginseng is similar to that of the total saponins of ginseng roots, so the aeria...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J17/00
CPCC07J17/005
Inventor 李珂珂弓晓杰陈丽荣李沙沙
Owner 吉林省参威人参产品科技股份有限公司
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