CN107722100B

CN107722100B - Method for purifying ginsenoside Rg1

Info

Publication number: CN107722100B
Application number: CN201711034686.6A
Authority: CN
Inventors: 黄京山; 邵伟
Original assignee: Reyoung Pharmaceutical Co Ltd
Current assignee: Reyoung Pharmaceutical Co Ltd
Priority date: 2017-10-30
Filing date: 2017-10-30
Publication date: 2021-05-14
Anticipated expiration: 2037-10-30
Also published as: CN107722100A

Abstract

The invention belongs to the technical field of traditional Chinese medicine extraction, and particularly relates to a method for purifying ginsenoside Rg 1. Dissolving Panax notoginsenosides in 95% ethanol to obtain solution; weighing neutral alumina powder, soaking in 95% ethanol, and packing; loading the obtained solution; washing with 95% ethanol, and then washing with 85% ethanol; collecting eluate rich in ginsenoside Rg1, and evaporating to obtain ginsenoside Rg1 crude product; dissolving the obtained crude ginsenoside Rg1 in n-butanol phase, extracting with water phase of the same volume, collecting n-butanol phase, and evaporating to obtain ginsenoside Rg 1. The invention finds the cheap and easily obtained filler suitable for purifying the ginsenoside Rg1 and the purification method, and effectively reduces the production cost.

Description

Method for purifying ginsenoside Rg1

Technical Field

The invention belongs to the technical field of traditional Chinese medicine extraction, and particularly relates to a method for purifying ginsenoside Rg 1.

Background

The panax notoginseng is dry root or rhizome of a plant in the family of Araliaceae, is a famous and precious Chinese medicinal material, and the main active ingredients of the panax notoginseng are saponin compounds which mainly comprise notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rd and the like. It is used for promoting blood circulation, removing blood stasis, dredging collaterals, activating collaterals, and treating hyperlipidemia, blood hyperviscosity, hypertension, myocardial ischemia, atherosclerosis, thrombosis, and heart and brain ischemia.

The ginsenoside Rg1 has good pharmacological activity, and has effects of treating cardiovascular disease and cerebrovascular disease, resisting thrombi and fibrosis, treating senile dementia, improving immunity, dilating blood vessel, relieving fatigue, and adjuvant treating tumor.

The traditional process utilizes silica gel column chromatography to separate and prepare the ginsenoside Rg1, needs a large amount of organic solvents such as methanol, chloroform, dichloromethane, ethyl acetate and the like, and has the defects of time and labor waste, low efficiency, difficult operation, high production cost, easy environmental pollution, inconvenient recycling of used solvents and the like.

Methods for separating ginsenoside Rg1 by reverse phase silica gel column chromatography or sephadex column chromatography are reported in patent CN101463061B and patent CN 101575357B. The eluent used in the method is an ethanol-water system, so that the use of an organic solvent is avoided, but the used filler is C18 reverse phase bonded silica gel or sephadex, so that the method is expensive and is not suitable for industrial production.

In patent CN105801656A, a method for separating saponins such as ginsenoside Rg1 and ginsenoside Re by monodisperse polymeric silica gel column chromatography is reported. The eluent used in the method is an ethanol-water system, so that the use of an organic solvent is avoided, but the used filler is monodisperse polymeric silica gel, so that the method is expensive and is not suitable for large-scale industrial production.

Disclosure of Invention

The invention aims to provide a method for purifying ginsenoside Rg1, which is simple and feasible, is suitable for industrial production and reduces the production cost.

The purification method of the ginsenoside Rg1 comprises the following steps:

(1) dissolving Panax notoginsenosides in 95% ethanol to obtain solution;

(2) weighing neutral alumina powder, soaking in 95% ethanol, and packing;

(3) loading the solution obtained in the step (1);

(4) washing with 95% ethanol, and then washing with 85% ethanol;

(5) collecting eluate rich in ginsenoside Rg1, and evaporating to obtain ginsenoside Rg1 crude product;

(6) and (3) dissolving the crude ginsenoside Rg1 product obtained in the step (5) in a n-butanol phase, then extracting with an isovolumetric aqueous phase, collecting the n-butanol phase, and evaporating to dryness to obtain the ginsenoside Rg 1.

The proportion of the panax notoginseng saponins and 95% ethanol in the step (1) is 1:5-1:10, the panax notoginseng saponins are counted by g, and the 95 percent ethanol is counted by mL.

The mesh number of the neutral alumina powder in the step (2) is 80-400 meshes.

The ratio of the neutral alumina powder to 95% ethanol in the step (2) is 1:2-1:5, neutral alumina powder in g, 95% ethanol in mL.

The ratio of the mass of the panax notoginseng saponins to the column volume in the step (2) is 1:50, mass in g, column volume in ml.

The flow rate of 95 percent ethanol washing in the step (4) is 4-6 BV.

The flow rate of the 85 percent ethanol washing in the step (4) is 10-12 BV.

In the step (6), the ratio of the crude ginsenoside Rg1 to the n-butanol phase is 1:15-1:30, the crude product of the ginsenoside Rg1 is counted by g, and the n-butanol phase is counted by mL.

The number of extraction times in step (6) was 4.

Compared with the prior art, the invention has the following beneficial effects:

aiming at the defects of the prior art, the invention finds the cheap and easily obtained filler and the purification method which are suitable for purifying the ginsenoside Rg1, and effectively reduces the production cost.

Detailed Description

The present invention is further described below with reference to examples.

Example 1

Dissolving Notoginseng radix total saponin 5.0g in 40ml 95% ethanol; weighing 80-160 mesh neutral alumina powder, soaking in 95% ethanol, and packing with a column volume of 250 ml; loading ethanol solution of Panax notoginsenosides, washing with 95% ethanol for 4BV, and washing with 85% ethanol for 10 BV; collecting eluate rich in ginsenoside Rg1, and evaporating to obtain ginsenoside Rg1 crude product; dissolving the ginsenoside Rg1 crude product with n-butanol, wherein the ratio of the ginsenoside crude product (g) to the n-butanol (mL) is 1:30, extracting with an equal volume of water phase for 4 times, collecting n-butanol phase, and evaporating to dryness to obtain ginsenoside Rg 10.94g; the purity of the ginsenoside Rg1 is 98.5%.

Example 2

Dissolving Notoginseng radix total saponin 5.0g in 50ml 95% ethanol; weighing 80-160 mesh neutral alumina powder, soaking in 95% ethanol, and packing with a column volume of 250 ml; loading ethanol solution of Panax notoginsenosides, washing with 95% ethanol for 6BV, and washing with 85% ethanol for 12 BV; collecting eluate rich in ginsenoside Rg1, and evaporating to obtain ginsenoside Rg1 crude product; dissolving the ginsenoside Rg1 crude product with n-butanol, wherein the ratio of the ginsenoside crude product (g) to the n-butanol (mL) is 1:15, extracting with water phase with the same volume for 4 times, collecting n-butanol phase, and evaporating to dryness to obtain ginsenoside Rg 10.98g; the purity of the ginsenoside Rg1 is 98.1%.

Example 3

Dissolving Notoginseng radix total saponin 5.0g in 40ml 95% ethanol; weighing 300-400 mesh neutral alumina powder, soaking in 95% ethanol, and packing with volume of 250 ml; loading ethanol solution of Panax notoginsenosides, washing with 95% ethanol for 4BV, and washing with 85% ethanol for 10 BV; collecting eluate rich in ginsenoside Rg1, and evaporating to obtain ginsenoside Rg1 crude product; dissolving the ginsenoside Rg1 crude product with n-butanol, wherein the ratio of the ginsenoside crude product (g) to the n-butanol (mL) is 1:30, extracting with an equal volume of water phase for 4 times, collecting n-butanol phase, and evaporating to dryness to obtain ginsenoside Rg 10.92g; the purity of the ginsenoside Rg1 is 99.2%.

Example 4

Dissolving Notoginseng radix total saponin 5.0g in 25ml 95% ethanol; weighing 300-400 mesh neutral alumina powder, soaking in 95% ethanol, and packing with volume of 250 ml; loading ethanol solution of Panax notoginsenosides, washing with 95% ethanol for 6BV, and washing with 85% ethanol for 12 BV; collecting eluate rich in ginsenoside Rg1, and evaporating to obtain ginsenoside Rg1 crude product; dissolving the ginsenoside Rg1 crude product with n-butanol, wherein the ratio of the ginsenoside crude product (g) to the n-butanol (mL) is 1: 20, extracting with water phase with the same volume for 4 times, collecting n-butanol phase, and evaporating to dryness to obtain ginsenoside Rg 10.95g; the purity of the ginsenoside Rg1 is 98.7%.

Claims

1. A method for purifying ginsenoside Rgl is characterized by comprising the following steps:

(1) dissolving Panax notoginsenosides in 95% ethanol to obtain solution;

(2) weighing neutral alumina powder, soaking in 95% ethanol, and packing;

(3) loading the solution obtained in the step (1);

(4) washing with 95% ethanol, and then washing with 85% ethanol;

(5) collecting eluate rich in ginsenoside Rgl, and evaporating to obtain ginsenoside Rgl crude product;

(6) dissolving the ginsenoside Rgl crude product obtained in the step (5) in an n-butanol phase, then extracting with an equal-volume water phase, collecting the n-butanol phase, and evaporating to dryness to obtain ginsenoside Rgl;

in the step (4), the flow rate of 95 percent ethanol washing is 4-6BV, and the flow rate of 85 percent ethanol washing is 10-12 BV;

in the step (6), the ratio of the ginsenoside Rgl crude product to the n-butyl alcohol phase is 1:15-1:30, wherein the ginsenoside Rgl crude product is counted by g, and the n-butyl alcohol phase is counted by mL.

2. A method of purifying ginsenoside Rgl of claim 1, wherein: the proportion of the panax notoginseng saponins and the 95% ethanol in the step (1) is 1:5-1:10, and the panax notoginseng saponins are counted by g and the 95% ethanol is counted by mL.

3. A method of purifying ginsenoside Rgl of claim 1, wherein: the mesh number of the neutral alumina powder in the step (2) is 80-400 meshes.

4. A method of purifying ginsenoside Rgl of claim 1, wherein: the ratio of the neutral alumina powder to 95% ethanol in the step (2) is 1:2-1:5, wherein the neutral alumina powder is calculated by g, and the 95% ethanol is calculated by mL.

5. A method of purifying ginsenoside Rgl of claim 1, wherein: the ratio of the mass of the panax notoginseng saponins to the column volume in the step (2) is 1:50, the mass is calculated by g, and the column volume is calculated by mL.

6. A purification method of ginsenoside Rg1 in claim 1, wherein the number of times of extraction in step (6) is 4.