CN102058646B - Ginsenoside rh2 extract and preparation method thereof - Google Patents
Ginsenoside rh2 extract and preparation method thereof Download PDFInfo
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- CN102058646B CN102058646B CN 200910228462 CN200910228462A CN102058646B CN 102058646 B CN102058646 B CN 102058646B CN 200910228462 CN200910228462 CN 200910228462 CN 200910228462 A CN200910228462 A CN 200910228462A CN 102058646 B CN102058646 B CN 102058646B
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- Prior art keywords
- ginsenoside
- total saponins
- folium
- radix
- silica gel
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Landscapes
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to traditional Chinese medicine extract and preparation thereof, in particular to ginsenoside Rh2 extract and preparation thereof. The preparation method comprises the following steps of: 1, extracting a medicinal material which contains ginsenoside components by using water, performing column chromatography on extract liquid through a macroporous adsorption resin column, eluting by using ethanol, collecting eluent, and concentrating the eluent until the eluent is dried so as to obtain total saponins; 2, dissolving the total saponins obtained in the step 1 in acid solution for reaction, adjusting pH to be neutral after the reaction is completed, and collecting precipitate; and 3, dissolving the precipitate in the ethanol, mixing into reverse phase silica gel, performing reverse phase silica gel column chromatography, eluting by using acetonitrile and water mixed liquid, collecting a fraction which is rich in the ginsenoside Rh2, and concentrating the fraction to obtain the ginsenoside Rh2 extract. The prepared ginsenoside Rh2 extract has higher treatment effect and higher purity than that prepared by the prior art.
Description
Technical field
The present invention relates to a kind of Chinese medicine extract and preparation thereof, particularly ginsenoside Rh2's extract and preparation thereof.
Background technology
Radix Ginseng has many reports aspect the treatment cardiovascular and cerebrovascular disease.
The Ginseng secondary glycoside constituents can be treated coronary heart disease and cerebral infarction.
The ginsenoside Rh2 is the secondary saponin that the Radix Ginseng saponins produces through hydrolysis, and pharmacodynamic study shows: the ginsenoside Rh2 has significant specific inhibitory action to the propagation of cancerous cell such as hepatocarcinoma, melanin tumour b16, cervical cancer and sarcoma S180.Its mechanism of action is: in the cancer cell multiplication process, through ginsenoside Rh2's effect, make cancerous cell stop at certain propagation phase, and impel its reverse to be normal cell.
Prior art is separated ginsenoside Rh2's poor effect, and the inventor is carrying out in the research process ginsenoside Rh2's extract, adopts new isolation technics, test out one group of new ginsenoside Rh2's extract and preparation method thereof, ginsenoside Rh2's extract of preparation has the curative effect height, the purity height, good absorbing, steady quality, the preparation method separating effect is good simultaneously, the content height, technology is simple, easy to operate, with low cost, be fit to suitability for industrialized production.
Summary of the invention
The invention provides a kind of ginsenoside Rh2's extract.
Ginsenoside Rh2's extract of the present invention, preparation method is as follows:
Step 1, contain the medical material water extraction of ginsenoside's constituents, extracting solution use ethanol elution by macroporous adsorptive resins, and the collection eluent is concentrated into driedly, gets total saponins;
The total saponins that step 2, step 1 obtain is dissolved in the acid solution and reacts, and regulates PH after reaction is finished to neutral, the collecting precipitation thing;
Step 3, precipitate dissolve with ethanol are admixed in the reverse phase silica gel, carry out reversed-phase silica gel column chromatography, carry out eluting with the acetonitrile water mixed liquid, collect the stream part of being rich in the ginsenoside Rh2, concentrate namely;
Wherein, macroporous adsorbent resin described in the step 1 is low pole or nonpolar macroporous adsorption resin, and described ethanol scope is 30-95%;
Acid solution described in the step 2 is selected from hydrochloric acid, sulphuric acid or acetic acid solution,
The ratio of the described acetonitrile water mixed liquid of step 3 is 10-80%.
Preferred manufacturing procedure is as follows:
Step 1, be selected from Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng etc. and contain the medical material of ginsenoside's constituents through water extraction, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continue and use the 70-95% ethanol elution, collect ethanol elution, be concentrated into dried total saponins;
Step 2,, total saponins is dissolved in the acid solution about PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, the collecting precipitation thing gets total secondary ginseng glucoside's crude product;
Step 3, precipitate dissolve with ethanol are admixed in the reverse phase silica gel, carry out reversed-phase silica gel column chromatography, carry out eluting with the acetonitrile water mixed liquid of 30-80%, collect the stream part of being rich in the ginsenoside Rh2, concentrate namely.
Preferred preparation method is as follows:
Step 1, be selected from medical material that Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng etc. contain ginsenoside's constituents with water extraction 2-3 time, each 1-2 hour, add water 8-12 doubly measures at every turn, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continues and uses the 80-90% ethanol elution, collect ethanol elution, be concentrated into dried total saponins;
Step 2, total saponins is dissolved in the acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product;
Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 40-70% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The present invention also comprises the application of ginsenoside Rh2's extract in the preparation antitumor drug.
The most preferred preparation method of the present invention in embodiments of the present invention.
The present invention comprises that also described pharmaceutical composition is the pharmaceutical preparation that is prepared into as active constituents of medicine with above-mentioned ginsenoside Rh2's extract with the pharmaceutical composition of ginsenoside Rh2's extract preparation of the present invention.Pharmaceutical composition of the present invention can contain the medicine acceptable carrier as required, and wherein ginsenoside Rh2's extract is as active constituents of medicine, and its shared percentage by weight in preparation can be 0.1-99.9%, and all the other are the medicine acceptable carrier.Pharmaceutical preparations composition of the present invention exists with unit dosage form, and described unit dosage form refers to the unit of preparation, as every of tablet, and every capsules of capsule, every bottle of oral liquid, every bag of granule, every of injection etc.
Pharmaceutical composition of the present invention can be any pharmaceutically useful dosage form, and these dosage forms comprise: tablet, sugar coated tablet, film coated tablet, enteric coated tablet, capsule, hard capsule, soft capsule, oral liquid, suck agent, granule, electuary, pill, powder, unguentum, sublimed preparation, suspensoid, powder, solution, injection, suppository, ointment, plaster, cream, spray, drop, patch.
Pharmaceutical composition of the present invention, the preparation of its oral administration can contain excipient commonly used, such as binding agent, filler, diluent, tablet agent, lubricant, disintegrating agent, coloring agent, flavoring agent and wetting agent, can carry out coating to tablet in case of necessity.
The filler that is suitable for comprises cellulose, mannitol, lactose and other similar filler.Suitable disintegrating agent comprises starch, polyvinylpyrrolidone and starch derivatives, for example sodium starch glycollate.Suitable lubricant comprises, for example magnesium stearate.The acceptable wetting agent of appropriate drug comprises sodium lauryl sulphate.Can fill by mixing, the method that tabletting etc. are commonly used prepares solid oral composition.Mix repeatedly active substance is distributed in those compositionss of a large amount of filleies of whole use.
The form of oral liquid for example can be aqueous or oily suspensions, solution, Emulsion, syrup or elixir, perhaps can be a kind of available water before use or other suitable composite dry products of carrier.This liquid preparation can contain conventional additive, such as suspending agent, for example sorbitol, syrup, methylcellulose, gelatin, hydroxyethyl-cellulose, carboxymethyl cellulose, aluminium stearate gel or hydrogenation edible fat, emulsifying agent, for example lecithin, anhydro sorbitol monooleate or arabic gum; Non-aqueous carrier (they can comprise edible oil), for example almond oil, fractionated coconut oil, such as oily ester, propylene glycol or the ethanol of the ester of glycerol; Antiseptic, for example para hydroxybenzene methyl ester or propyl p-hydroxybenzoate or sorbic acid, and if desired, can contain conventional flavouring agent or coloring agent.
For injection, the liquid unit dosage forms of preparation contains active substance of the present invention and sterile carrier.According to carrier and concentration, this chemical compound can be suspended or dissolving.The preparation of solution is normally by being dissolved in active substance in a kind of carrier filter-sterilized before it is packed into a kind of suitable bottle or ampoule, sealing then.Adjuvant for example a kind of local anesthetic, antiseptic and buffer agent also can be dissolved in this carrier.In order to improve its stability, can be after the bottle of packing into that this compositions is freezing, and under vacuum, water is removed.
Pharmaceutical composition of the present invention, when being prepared into medicament, optionally add suitable medicine acceptable carrier, described medicine acceptable carrier is selected from: mannitol, sorbitol, sodium pyrosulfite, sodium sulfite, sodium thiosulfate, cysteine hydrochloride, TGA, methionine, vitamin C, the EDTA disodium, EDTA calcium sodium, the alkali-metal carbonate of monovalence, acetate, phosphate or its aqueous solution, hydrochloric acid, acetic acid, sulphuric acid, phosphoric acid, aminoacid, sodium chloride, potassium chloride, sodium lactate, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, mannitol, silicon derivative, cellulose and derivant thereof, alginate, gelatin, polyvinylpyrrolidone, glycerol, soil temperature 80, agar, calcium carbonate, calcium bicarbonate, surfactant, Polyethylene Glycol, cyclodextrin, beta-schardinger dextrin-, the phospholipid material, Kaolin, Pulvis Talci, calcium stearate, magnesium stearate etc.
Pharmaceutical composition of the present invention is determined usage and dosage according to patient's situation in use, but obeys every day three times, each 1-20 agent, as: 1-20 bag or grain or sheet, every dose of 1mg-1000mg.
Following data declaration beneficial effect of the present invention by experiment.
Ginsenoside Rh2's injection has the obvious suppression effect through pharmacodynamic experiment proof to the multiple transplantation experiments tumor of mice, and 50,25,12.5mg/kg ginsenoside Rh2 injection all has the obvious suppression effect to murine sarcoma (S180), hepatocarcinoma A22 (HepA22), ehrlich carcinoma (ESC), pulmonary carcinoma (Lewis); Ginsenoside Rh2's injection all has tangible potentiation to tumor-bearing mice peritoneal macrophage phagocytic function and humoral immune function, and can significantly improve the NK cytoactive, 40mg/kg ginsenoside Rh2 injection both can promote splenocyte to drench to be changeed, and can obviously improve interleukin II (IL-2) activity again.
Relevant test shows, ginsenoside Rh2's extract of the present invention is than prior art curative effect height, the purity height, and the productive rate height, good absorbing, steady quality, the purposes novelty, preparation method technology is simple, easy to operate, with low cost simultaneously, is fit to suitability for industrialized production.
The specific embodiment
Below with bright the present invention specifically, embodiment is for the ease of understanding the present invention, and the claim that does not limit the present invention in any way and core content.
The preparation of embodiment 1 ginsenoside Rh2's extract
Step 1, Folium Panacis Quinquefolii water extraction 2 times each 2 hours, add 10 times of amounts of water at every turn, extracting solution washes with water earlier by macroporous adsorptive resins, and it is closely colourless to be eluted to effluent, continue and use 85% ethanol elution, collect 85% ethanol elution, be concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product;
Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 45% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The preparation of embodiment 2 ginsenoside Rh2's extracts
Step 1, Radix Panacis Quinquefolii be with water extraction 3 times, and each 1 hour, add 10 times of amounts of water at every turn, extracting solution washes with water earlier by macroporous adsorptive resins, and it is closely colourless to be eluted to effluent, continues and use 30% ethanol elution, and the collection ethanol elution is concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product; Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 60% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The preparation of embodiment 3 ginsenoside Rh2's extracts
Step 1, Folium Notoginseng be with water extraction 2 times, and each 2 hours, add 10 times of amounts of water at every turn, extracting solution washes with water earlier by macroporous adsorptive resins, and it is closely colourless to be eluted to effluent, continues and uses 95% ethanol elution, collects 95% ethanol elution, is concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product;
Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 50% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The preparation of embodiment 4 ginsenoside Rh2's extracts
Step 1, Radix Notoginseng be with water extraction 1 time, and each 3 hours, add 10 times of amounts of water at every turn, extracting solution washes with water earlier by macroporous adsorptive resins, and it is closely colourless to be eluted to effluent, continues and uses 75% ethanol elution, collects 75% ethanol elution, is concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product;
Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 60% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The preparation of embodiment 5 ginsenoside Rh2's extracts
Step 1, Folium Ginseng be with water extraction 2 times, and each 2 hours, add 8 times of amounts of water at every turn, extracting solution washes with water earlier by macroporous adsorptive resins, and it is closely colourless to be eluted to effluent, continues and uses 90% ethanol elution, collects 90% ethanol elution, is concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product;
Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 70% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The preparation of embodiment 6 ginsenoside Rh2's extracts
Step 1, Radix Ginseng be with water extraction 3 times, and each 1 hour, add 12 times of amounts of water at every turn, extracting solution washes with water earlier by macroporous adsorptive resins, and it is closely colourless to be eluted to effluent, continues and uses 75% ethanol elution, collects 75% ethanol elution, is concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product; Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 55% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The preparation of embodiment 7 ginsenoside Rh2's extracts
Step 1, Folium Ginseng be through water extraction, and extracting solution washes with water earlier by the AB-8 macroporous adsorptive resins, and it is closely colourless to be eluted to effluent, continues and uses 40% ethanol elution, collects 40% ethanol elution, is concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product;
Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 50% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The preparation of embodiment 8 ginsenoside Rh2's extracts
Step 1, Folium Panacis Quinquefolii be through water extraction, and extracting solution washes with water earlier by the D101 macroporous adsorptive resins, and it is closely colourless to be eluted to effluent, continues and uses 70% ethanol elution, collects 70% ethanol elution, is concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets total secondary ginseng glucoside's crude product;
Step 3, total secondary ginseng glucoside's crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 40% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
The compositions of embodiment 9 ginsenoside Rh2's extracts
Be active constituents of medicine with ginsenoside Rh2's extract of the present invention, according to the galenic pharmacy routine techniques, be prepared into the pharmaceutical preparations composition of ginsenoside Rh2's extract, as tablet, capsule, injection etc.
The assay of embodiment 10 Radix Ginseng saponin Rh2 extracts of the present invention:
Ginsenoside Rh2's extract of embodiments of the invention 1,
The ginsenoside Rh
2Content is 40%.
The anti-tumor activity of embodiment 11 Radix Ginseng saponin Rh2 extracts of the present invention relatively
Test divides two groups, the ginsenoside Rh2's extract and the most preferred ginsenoside Rh2's extract of the present invention that obtain with extracting method of the prior art carry out the anti-tumor activity contrast, and it is higher to prove that what tumor mice ginsenoside Rh2's extract of the present invention waits go up anti-tumor activity in murine sarcoma (S180), hepatocarcinoma A22 (HepA22), ehrlich carcinoma (ESC), pulmonary carcinoma (Lewis).
Claims (9)
1. ginsenoside Rh2's extract is characterized in that preparation method is as follows:
Step 1, be selected from Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng and contain the medical material of ginsenoside's constituents through water extraction, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continue and use the 70-95% ethanol elution, collect ethanol elution, be concentrated into dried total saponins;
Step 2,, total saponins is dissolved in the acid solution about pH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated pH to nearly neutrality, separates out precipitation, the collecting precipitation thing gets the Radix Ginseng total saponins crude product;
Step 3, precipitate dissolve with ethanol are admixed in the reverse phase silica gel, carry out reversed-phase silica gel column chromatography, carry out eluting with the acetonitrile water mixed liquid of 10-80%, collect the stream part of being rich in the ginsenoside Rh2, concentrate namely;
Wherein, macroporous adsorbent resin described in the step 1 is low pole or nonpolar macroporous adsorption resin;
Wherein, the acid solution described in the step 2 is selected from hydrochloric acid, sulphuric acid or acetic acid solution.
2. ginsenoside Rh2's extract of claim 1 is characterized in that preparation method is as follows:
Step 1, be selected from medical material that Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng contain ginsenoside's constituents with water extraction 2-3 time, each 1-2 hour, add water 8-12 doubly measures at every turn, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continues and uses the 80-90% ethanol elution, collect ethanol elution, be concentrated into dried total saponins;
Step 2, total saponins is dissolved in the acid solution about 20 times pH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets the Radix Ginseng total saponins crude product;
Step 3, Radix Ginseng total saponins crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 50-80% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
3. the pharmaceutical composition that contains ginsenoside Rh2's extract of right requirement 1.
4. the application of ginsenoside Rh2's extract of claim 1 in the preparation antitumor drug.
5. ginsenoside Rh2's preparation method of extract of claim 1 is characterized in that step is as follows:
Step 1, be selected from Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng and contain the medical material of ginsenoside's constituents through water extraction, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continue and use the 70-95% ethanol elution, collect ethanol elution, be concentrated into dried total saponins;
Step 2,, total saponins is dissolved in the acid solution about pH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated pH to nearly neutrality, separates out precipitation, the collecting precipitation thing gets the Radix Ginseng total saponins crude product;
Step 3, precipitate dissolve with ethanol are admixed in the reverse phase silica gel, carry out reversed-phase silica gel column chromatography, carry out eluting with the acetonitrile water mixed liquid of 10-80%, collect the stream part of being rich in the ginsenoside Rh2, concentrate namely;
Wherein, macroporous adsorbent resin described in the step 1 is low pole or nonpolar macroporous adsorption resin;
Wherein, the acid solution described in the step 2 is selected from hydrochloric acid, sulphuric acid or acetic acid solution.
6. the preparation method of claim 5 is characterized in that, step is as follows:
Step 1, be selected from Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng and contain the medical material of ginsenoside's constituents through water extraction, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continue and use 85% ethanol elution, collect 85% ethanol elution, be concentrated into dried total saponins;
Step 2,, total saponins is dissolved in the acid solution about PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, the collecting precipitation thing gets the Radix Ginseng total saponins crude product;
Step 3, precipitate dissolve with ethanol are admixed in the reverse phase silica gel, carry out reversed-phase silica gel column chromatography, carry out eluting with the acetonitrile water mixed liquid of 40-70%, collect the stream part of being rich in the ginsenoside Rh2, concentrate namely.
7. the preparation method of claim 5 is characterized in that, step is as follows:
Step 1, be selected from medical material that Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng contain ginsenoside's constituents with water extraction 2-3 time, each 1-2 hour, add water 8-12 doubly measures at every turn, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continues and uses 85% ethanol elution, collect 85% ethanol elution, be concentrated into dried total saponins;
Step 2, total saponins is dissolved in the acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets the Radix Ginseng total saponins crude product;
Step 3, Radix Ginseng total saponins crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 40-70% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
8. the preparation method of claim 5 is characterized in that, step is as follows:
Step 1, be selected from medical material that Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng etc. contain ginsenoside's constituents with water extraction 2 times, each 2 hours, add 10 times of amounts of water at every turn, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continues and uses 85% ethanol elution, collect 85% ethanol elution, be concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets the Radix Ginseng total saponins crude product;
Step 3, Radix Ginseng total saponins crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 45-60% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
9. the preparation method of claim 5 is characterized in that, step is as follows:
Step 1, be selected from medical material that Folium Panacis Quinquefolii, Radix Panacis Quinquefolii, Radix Notoginseng, Folium Notoginseng, Radix Ginseng or Folium Ginseng etc. contain ginsenoside's constituents with water extraction 3 times, each 2 hours, add 10 times of amounts of water at every turn, extracting solution passes through macroporous adsorptive resins, wash with water earlier, it is closely colourless to be eluted to effluent, continues and uses 85% ethanol elution, collect 85% ethanol elution, be concentrated into dried total saponins;
Step 2, total saponins is dissolved in the hydrochloric acid solution about 20 times PH1.0, at 40 ℃ of stirring reaction 4h, reaction is finished the back and is regulated PH to nearly neutrality, separates out precipitation, and the collecting precipitation thing gets the Radix Ginseng total saponins crude product;
Step 3, Radix Ginseng total saponins crude product make dissolving with the ethanol heating, admix in the reverse phase silica gel of 2 times of amounts, carry out reversed-phase silica gel column chromatography, acetonitrile water mixed liquid with 50% carries out eluting, thin layer TLC checks the eluting result, collects the stream part of being rich in the ginsenoside Rh2, concentrates namely.
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| CN105063157A (en) * | 2015-08-19 | 2015-11-18 | 西安岳达植物科技有限公司 | Synthesis method for panaxoside Rh2 |
| CN107029004A (en) * | 2016-02-04 | 2017-08-11 | 南京生道源医药科技有限公司 | The preparation method and new application of adenophora tetraphylla saponin(e |
| CN109232702B (en) * | 2018-10-11 | 2020-05-26 | 云南三七科技有限公司 | Preparation method of ginsenoside Rh2 |
| CN110025564A (en) * | 2019-05-10 | 2019-07-19 | 吉林省一向科技有限责任公司 | A kind of anti-aging skin care compositions and preparation method thereof |
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