A method for separating and purifying ginsenoside

Abstract

The invention discloses a method for separating and purifying ginsenosides of ginsenosides, comprising the following steps: S1, adding total saponins of Panax notoginseng and ethanol with a concentration greater than 95% to a reflux tank, stirring and heating to reflux; S2, after reflux is completed, filtering while hot, and collecting insolubles as product A; after the solution part is allowed to stand at room temperature and cooled to room temperature, filtering and collecting precipitate product C, and concentrating and drying the filtrate to obtain product B; S3, placing product C in a reflux tank, adding ethanol with a concentration greater than 95%, stirring and heating to reflux; S4, after reflux is completed, filtering while hot, and collecting insolubles as product D; after the solution part is allowed to stand at room temperature and cooled to room temperature, filtering and collecting precipitate product F, and concentrating and drying the filtrate to obtain product E; S5, drying product F to obtain ginsenosides of ginsenosides. Extracting, separating and purifying ginsenosides of ginsenosides from total saponins of Panax notoginseng by the present invention has the advantages of simple steps, simple operation and high product purity.

Description

Technical Field

[0001] The invention belongs to the technical field of natural drug extraction, and specifically relates to a method for separating and purifying ginsenoside. Background Art

[0002] Ginsenosides are the main biologically active ingredients of ginseng and ginseng plants, such as ginseng, American ginseng, Panax notoginseng and other precious Chinese medicinal materials.

[0003] The main component of ginsenosides is dammarane-type tetracyclic triterpenoid saponins, which can be divided into two categories according to whether there is a hydroxyl group at the C-6 position. One category is (20S)-protopanaxadiol saponins, such as ginsenosides Ra1, Rd, Rb1, etc.; the other category is 20S-protopanaxatriol saponins, such as ginsenosides Re, Rf, Rg1, etc.

[0004] Although both belong to the dammarane-type tetracyclic triterpenoid saponins, there are great differences in the pharmacological effects and pharmacological activities between protopanaxadiol saponins and protopanaxantriol saponins. For example, protopanaxantriol saponins have significant hemolytic and central nervous system stimulant effects, and have the effects of enhancing immunity, improving cardiovascular function, anti-aging, and anti-inflammatory. Protopanaxadiol saponins have significant anti-hemolytic and central nervous system inhibitory effects, and have anti-fatigue, antioxidant, anti-tumor, hypoglycemic, and hypolipidemic effects.

[0005] As the research deepens, more and more data show that there are significant differences in the pharmacological effects and biological activities of ginsenosides from the ginsenoside group and ginsenosides from the ginsenoside group. Even the different monomers in ginsenosides from the ginsenosides from the ginsenosides from the ginsenosides have significant differences in pharmacological effects.

[0006] At present, the main methods used for separating ginsenosides of ginsenodiol and ginsenotriol are: column chromatography, solvent extraction, etc., which use a variety of reagents, have a complicated preparation process, and it is not easy to obtain high content of protopanaxadiol saponins and protopanaxantriol saponins.

[0007] Therefore, in order to better play the role of ginsenosides in the treatment of human diseases, it is urgent to find a method for separating ginsenosides of ginsenodiol and ginsenotriol. Summary of the invention

[0008] In order to overcome the problems existing in the prior art, the present invention proposes a method for separating and purifying ginsenosides, which can separate ginsenosides from ginsenosides, and has the advantages of simple steps, simple operation and high product purity.

[0009] To achieve the above object, the present invention is implemented through the following technical solutions:

[0010] A method for separating and purifying ginsenosides, comprising the following steps:

[0011] S1, adding Panax notoginseng total saponins and ethanol with a concentration greater than 95% into a reflux tank, stirring and heating to reflux;

[0012] S2, after the reflux is completed, the product is filtered while hot, and the insoluble matter is collected as product A; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitate product C is collected by filtration, and the filtrate is concentrated and dried to obtain product B;

[0013] S3, placing the product C in a reflux tank, adding ethanol with a concentration greater than 95%, stirring and heating under reflux;

[0014] S4, after the reflux is completed, the hot part is filtered, and the insoluble matter is collected as product D; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitated product F is collected by filtration, and the filtrate is concentrated and dried to collect the product E;

[0015] S5, drying the product F to obtain ginsenoside.

[0016] Furthermore, the amount of ethanol added is 2L-8L of ethanol per 1kg of Panax notoginseng total saponins;

[0017] Furthermore, in the steps S1 and S3, the heating reflux time is: 10-20 min;

[0018] Furthermore, in the step S3, the amount of ethanol added is 2L-6L of ethanol per 1kg of product C.

[0019] Through the above technical scheme, the present invention can at least achieve the following beneficial effects: the extraction, separation and purification of ginsenosides from notoginseng total saponins by the present invention has the advantages of simple steps, simple operation and high product purity. The entire extraction process only requires heating reflux, filtering and drying to obtain ginsenosides, and the overall efficiency is high. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is a high performance liquid chromatogram of the product prepared by the method described in Example 1 of the present invention;

[0021] Figure 2 This is a high performance liquid chromatogram of the product prepared by the method described in Example 2 of the present invention;

[0022] Figure 3 It is a high performance liquid chromatogram of the product prepared by the method described in Example 3 of the present invention. DETAILED DESCRIPTION

[0023] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0024] The inventors of the present invention found during the study of separation and extraction of ginsenoside diol saponins from notoginseng total saponins that after the total saponins of Panax notoginseng are placed in ethanol with a concentration greater than 95%, stirred, heated and refluxed for extraction, the extract is filtered while hot, and after the filtrate is cooled, the precipitated product is collected, and then the precipitated product is extracted with ethanol with a concentration greater than 95%, stirred, heated and refluxed, and after the filtrate is cooled, the precipitated product is filtered while hot, and after the precipitated product is dried, it is ginsenoside diol saponins.

[0025] Based on this, the present application provides a method for separating and purifying ginsenosides, comprising the following steps:

[0026] S1, adding Panax notoginseng total saponins and ethanol with a concentration greater than 95% into a reflux tank, stirring and heating to reflux;

[0027] S2, after the reflux is completed, the product is filtered while hot, and the insoluble matter is collected as product A; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitate product C is collected by filtration, and the filtrate is concentrated and dried to obtain product B (product B is ginsenoside);

[0028] S3, placing the product C in a reflux tank, adding ethanol with a concentration greater than 95%, stirring and heating under reflux;

[0029] S4, after the reflux is completed, the hot part is filtered, and the insoluble matter is collected as product D; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitated product F is collected by filtration, and the filtrate is concentrated and dried to collect the product E;

[0030] S5, drying the product F to obtain ginsenoside.

[0031] According to a preferred embodiment of the present invention, the amount of ethanol added is 2L-8L of ethanol per 1kg of Panax notoginseng total saponins;

[0032] According to a preferred embodiment of the present invention, in the steps S1 and S3, the heating reflux time is: 10-20 min;

[0033] According to a preferred embodiment of the present invention, in the step S3, the amount of ethanol added is 2L-6L of ethanol per 1kg of product C.

[0034] In order to make the obtained ginsenosides of higher purity, the product F obtained in step S5 can be used as the product C in step S3, and the above steps S3-S5 can be repeated to purify ginsenosides.

[0035] The present invention will be described in detail below by way of examples. It should be understood that the following examples are only used to further explain and illustrate the content of the present invention by way of example, and are not intended to limit the present invention.

[0036] In the following examples, unless otherwise specified, the reagents and materials used are commercial products purchased from regular chemical / biological reagent or material suppliers.

[0037] Example 1

[0038] A method for separating and purifying ginsenosides, comprising the following steps:

[0039] S1, adding Panax notoginseng total saponins and ethanol with a concentration greater than 95% to a reflux tank, stirring, heating and reflux for 15 minutes; the amount of ethanol added is 5L of ethanol per 1kg of Panax notoginseng total saponins;

[0040] S2, after the reflux is completed, the product is filtered while hot, and the insoluble matter is collected as product A; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitate product C is collected by filtration, and the filtrate is concentrated and dried to obtain product B;

[0041] S3, place product C in a reflux tank, add ethanol with a concentration greater than 95%, stir and heat under reflux for 15 minutes; the amount of ethanol added is 5L of ethanol for every 1kg of product C

[0042] S4, after the reflux is completed, the hot part is filtered, and the insoluble matter is collected as product D; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitated product F is collected by filtration, and the filtrate is concentrated and dried to collect the product E;

[0043] S5, drying the product F under reduced pressure to obtain ginsenoside.

[0044] The raw materials of total saponins of Panax notoginseng used in Example 1 and the ginsenosides of ginsenosides obtained in step S5 were subjected to HPLC detection. The detection method was carried out according to the method described in [Content Determination] of total saponins of Panax notoginseng in the Pharmacopoeia of the People's Republic of China. The detection results are shown in Table 1 below. The HPLC chromatogram of ginsenosides of ginsenosides is shown in the attached figure. Figure 1 shown.

[0045] Table 1 Raw materials of Panax notoginseng total saponins and ginsenoside components

[0046]

[0047] Example 2

[0048] A method for separating and purifying ginsenosides, comprising the following steps:

[0049] S1, add Panax notoginseng total saponins and ethanol with a concentration greater than 95% to a reflux tank, stir and heat to reflux for 10 minutes; the amount of ethanol added is 2L of ethanol per 1kg of Panax notoginseng total saponins

[0050] S2, after the reflux is completed, the product is filtered while hot, and the insoluble matter is collected as product A; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitate product C is collected by filtration, and the filtrate is concentrated and dried to obtain product B;

[0051] S3, placing the product C in a reflux tank, adding ethanol with a concentration greater than 95%, stirring, heating and reflux for 10 minutes; the amount of ethanol added is 2L of ethanol for every 1kg of product C;

[0052] S4, after the reflux is completed, the hot part is filtered, and the insoluble matter is collected as product D; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitated product F is collected by filtration, and the filtrate is concentrated and dried to collect the product E;

[0053] S5, drying the product F under reduced pressure to obtain ginsenoside.

[0054] The raw materials of Panax notoginseng total saponins used in Example 2 and the ginsenosides obtained in step S5 were subjected to HPLC detection. The detection method was carried out according to the method described in [Content Determination] of Panax notoginseng total saponins in the Pharmacopoeia of the People's Republic of China. The detection results are shown in Table 2 below. The HPLC chromatogram of ginsenosides is shown in the attached figure. Figure 2 shown.

[0055] Table 2 Raw materials of Panax notoginseng total saponins and ginsenoside components

[0056]

[0057] Example 3

[0058] A method for separating and purifying ginsenosides, comprising the following steps:

[0059] S1, adding Panax notoginseng total saponins and ethanol with a concentration greater than 95% to a reflux tank, stirring, heating and reflux for 20 minutes; the amount of ethanol added is 8L of ethanol per 1kg of Panax notoginseng total saponins;

[0060] S2, after the reflux is completed, the product is filtered while hot, and the insoluble matter is collected as product A; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitate product C is collected by filtration, and the filtrate is concentrated and dried to obtain product B;

[0061] S3, the product C, placed in a reflux tank, add ethanol concentration greater than 95%, stirring and heating under reflux for 20min; the amount of ethanol added is 6L of ethanol per 1kg of product C;

[0062] S4, after the reflux is completed, the hot part is filtered, and the insoluble matter is collected as product D; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitated product F is collected by filtration, and the filtrate is concentrated and dried to collect the product E;

[0063] S5, drying the product F under reduced pressure to obtain ginsenoside.

[0064] The raw materials of total saponins of Panax notoginseng used in Example 4 and the ginsenosides of ginsenosides obtained in step S5 were subjected to HPLC detection. The detection method was carried out according to the method described in [Content Determination] of total saponins of Panax notoginseng in the Pharmacopoeia of the People's Republic of China. The detection results are shown in Table 3 below. The HPLC chromatogram of ginsenosides of ginsenosides is shown in the attached figure. Figure 3 shown.

[0065] Table 3 Raw materials of Panax notoginseng total saponins and ginsenoside components

[0066]

[0067] Finally, it should be noted that the above preferred embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail through the above preferred embodiments, those skilled in the art should understand that various changes can be made in form and details without departing from the scope defined by the claims of the present invention.

Claims

1. A method for separating and purifying ginsenosides, characterized in that: The following steps are involved: S1, adding Panax notoginseng total saponins and ethanol with a concentration greater than 95% to a reflux tank, stirring, heating and reflux; wherein the amount of ethanol added is 2L-8L of ethanol per 1kg of Panax notoginseng total saponins; S2, after the reflux is completed, the product is filtered while hot, and the insoluble matter is collected as product A; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitate product C is collected by filtration, and the filtrate is concentrated and dried to obtain product B; S3, placing the product C in a reflux tank, adding ethanol with a concentration greater than 95%, stirring and heating under reflux; S4, after the reflux is completed, the solution is filtered while hot, and the insoluble matter is collected as product D; after the solution is allowed to stand at room temperature and cooled to room temperature, the precipitated product F is collected by filtration, and the filtrate is concentrated and dried to collect the product E; S5, drying the product F to obtain ginsenoside.

2. The method for separating and purifying ginsenosides according to claim 1, characterized in that: In the steps S1 and S3, the heating reflux time is 10-20 min.

3. The method for separating and purifying ginsenosides according to claim 1, characterized in that: In the step S3, the amount of ethanol added is 2L-6L of ethanol per 1kg of product C.

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