Method for preparing 20 (R)-ginseniside Rg3

A technology of ginsenosides and Panax notoginseng saponins, which is applied in the field of preparation of ginsenoside Rg3, can solve the problems of difficult industrial production, complex and expensive extraction and preparation, etc.

Inactive Publication Date: 2012-11-14
YUNNAN AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to 20(R)-ginsenoside Rg 3 The content in ginseng is very small, only 3/100,000, the extractio...

Method used

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  • Method for preparing 20 (R)-ginseniside Rg3

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Experimental program
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Effect test

Embodiment 1

[0014] Preparation of the present invention 20(R)-ginsenoside Rg 3 The specific steps of the method are as follows:

[0015] (1) Acidification

[0016] Dissolve Panax notoginseng saponins in water, add acid (hydrochloric acid, phosphoric acid, sulfuric acid, acetic acid, glacial acetic acid, formic acid and other acids) to adjust the pH to 1~3, heat and reflux for 30~60 min, recover the acid solution and concentrate to a paste, dry A crude conversion product was obtained.

[0017] (2) Separation and purification by column chromatography

[0018] The crude conversion product obtained in step (1) was dissolved and adsorbed in methanol to 1.5 times the amount of silica gel to mix the sample, evaporated to dryness at room temperature, and subjected to silica gel column chromatography, eluted with a mixed solvent of chloroform:methanol:water gradient, and collected the eluate , with 20(R)-ginsenoside Rg 3 As a control, follow-up detection with thin-layer chromatography (TLC),...

Embodiment 2

[0026] First obtain the total saponins of notoginseng according to the method of Example 1, then dissolve 100 g of total saponins of notoginseng in 1000 ml of water, adjust the pH to 3 with hydrochloric acid, heat and reflux for 60 min, recover the acid solution and concentrate it to a paste, and dry to obtain crude Conversion product 101.2 g. The crude conversion product was dissolved in an appropriate amount of methanol, adsorbed on 150 g of 200-300 mesh silica gel, mixed with the sample, evaporated to dryness at room temperature, and subjected to silica gel column chromatography. Carry out gradient elution, collect eluate, with 20 (R)-ginsenoside Rg 3 As a control, follow-up detection with thin-layer chromatography (TLC), combined with 20(R)-ginsenoside Rg 3 Fractions, reclaim the solvent to 200 ml, let stand, filter, and dry the filter cake to obtain 20(R)-ginsenoside Rg 3 16.8 g. Detected by high performance liquid chromatography (HPLC), the resulting product 20(R)...

Embodiment 3

[0028] First obtain the total saponins of notoginseng according to the method of Example 1, then dissolve 100 g of total saponins of notoginseng in 1000 ml of water, adjust the pH to 1 with hydrochloric acid, heat and reflux for 50 min, recover the acid solution and concentrate it to a paste, and dry to obtain crude Conversion product 102.5 g. The crude conversion product was dissolved in an appropriate amount of methanol, adsorbed on 150 g of 200-300 mesh silica gel, mixed with the sample, evaporated to dryness at room temperature, and subjected to silica gel column chromatography. Carry out gradient elution, collect eluate, with 20 (R)-ginsenoside Rg 3 As a control, follow-up detection with thin-layer chromatography (TLC), combined with 20(R)-ginsenoside Rg 3 Fractions, reclaim the solvent to 200 ml, let stand, filter, and dry the filter cake to obtain 20(R)-ginsenoside Rg 3 15.9 g. Detected by high performance liquid chromatography (HPLC), the resulting product 20(R)...

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Abstract

A method for the preparing 20 (R)-ginseniside Rg3 includes dissolving panax notoginseng saponins (PNS) with water, adding acids (hydrochloric acid, phosphoric acid, sulfuric acid, acetic acid, glacial acetic acid, formic acid and the like) to adjust the pH to be 1 to 3, heating and returning the mixture for 30 minutes to 60 minutes, recycling an acid liquor and concentrating the acid liquor into paste, and drying the pasted liquor to obtain coarse converted products; and performing silica-gel column chromatography on the coarse converted products, performing gradient elution on chloroform-methanol-water, collecting an eluent, performing tracking detection through thin layer chromatography (TLC) compared with the ginseniside Rg3, merging flow parts mainly containing the ginseniside Rg3, recycling solvents with the amount two times of the amount of the pseudo-ginseng saponin before transformation, performing standing and filtration, and drying filter cakes to obtain the 20 (R)-ginseniside Rg3. Tested by high performance liquid chromatography (HPLC), the content of the 20 (R)-ginseniside Rg3 is larger than 90%. The method for preparing the 20 (R)-ginseniside Rg3 has the advantages of being simple, low in cost, high in product purity, and suitable for industrial production.

Description

Technical field: [0001] The invention belongs to the field of natural medicine preparation, in particular to a kind of ginsenoside Rg 3 method of preparation. Background technique: [0002] 20(R)-Ginsenoside Rg 3 It was first prepared by Japanese scholar Kitagawa Isao in 1980, and its molecular formula was determined. Subsequently, scholars from Japan, China, South Korea, Germany, the United States and other countries also carried out research on it to varying degrees. 20(R)-Ginsenoside Rg 3 It is extracted from red ginseng (cultivated ginseng dried or dried and then steamed), and its extraction rate is only 0.003%. 42 h 72 o 13 , molecular weight 784.30, chemical name: 20(R)-dammarane diol-3-O-β-D-glucopyranosyl (1-2)-β-D-glucopyranose. Soluble in methanol and ethanol, low solubility in water, insoluble in ether and chloroform. 20(R)-Ginsenoside Rg 3 It is an effective active ingredient in ginseng, which can improve and prevent many diseases. It has a good curativ...

Claims

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Application Information

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IPC IPC(8): C07J17/00
Inventor 沈勇艾洪莲赵大克郑丽张丽梅李晓波字淑慧
Owner YUNNAN AGRICULTURAL UNIVERSITY
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