CN101781351A - Method for extracting ginsenoside Rb1 from American ginseng and powder-injection thereof - Google Patents

Method for extracting ginsenoside Rb1 from American ginseng and powder-injection thereof Download PDF

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CN101781351A
CN101781351A CN200910077265A CN200910077265A CN101781351A CN 101781351 A CN101781351 A CN 101781351A CN 200910077265 A CN200910077265 A CN 200910077265A CN 200910077265 A CN200910077265 A CN 200910077265A CN 101781351 A CN101781351 A CN 101781351A
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ginsenoside
water
powder
american ginseng
extraction
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CN101781351B (en
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唐贤俊
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CHONGQING HUASEN PHARMACEUTICAL CO., LTD.
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Chengdu Huasen Parmaceutical High&new Technology Co Ltd
Huasen Pharm Co Ltd Chongqing
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Abstract

The invention discloses a method for extracting ginsenoside Rb1 from American Ginseng, which comprises the following steps: grinding the American ginseng into powder, soaking the powder with water, extracting by ultrasonic oscillation, conducting ginsenoside Rb1 solution through macroporous resin columns, collecting the elute, concentrating, drying up, separating and purifying monomer ginsenoside Rb1 from the American ginseng saponin extractive by SMBC (simulated moving bed chromatography) technology.. The method of the invention can save energy and time as well as reduce the environmental pollution. In the invention, the ginsenoside Rb1 content of the extracts is further enhanced and the treatment amount is increased. The method is beneficial for the industrial production.

Description

A kind ofly from Radix Panacis Quinquefolii, extract the Ginsenoside Rb 1Method and powder injection thereof
Technical field
The present invention relates to a kind of Ginsenoside Rb that from Radix Panacis Quinquefolii, extracts 1Method and with the powder injection that is used for the treatment of cardiovascular and cerebrovascular diseases that the ginsenoside Rb1 makes, belong to formulation art.
Background technology
Radix Panacis Quinquefolii claims Radix Panacis Quinquefolii again, is the dry root of Araliaceae Radix Panacis Quinquefolii Panax quinquefolium L..Originate in the U.S. and Canada, China is successful introduction, forms large-scale production, is called homemade Radix Panacis Quinquefolii, and Radix Panacis Quinquefolii is taken in 2000 editions one one 99 pages of Pharmacopoeias of People's Republic of China first.Its nature and flavor with return through for sweet, little hardship cold, the thoughts of returning home, lung, kidney channel.Its function is boosting qi and nourishing yin with curing mainly, and clearing heat and promoting fluid is used for that the deficiency of vital energy is cloudy loses, and interior heat is coughed and breathed heavily phlegm blood, and abnormal heat is tired tired, quenches one's thirst dryness of the mouth and throat.The main effective monomer component of Radix Panacis Quinquefolii is the Ginsenoside Rb 1
Chinese invention patent ZL200310100461.8 discloses " total panaquilon novel technology for extracting and powder injection thereof "; Chinese invention patent CN1072089 (application number 92111985) discloses " adsorption resin method extracts the Chinese medicine compound prescription significant part "; " Jilin Chinese materia medica " the 07th phase in 2006 has been delivered " Radix Panacis Quinquefolii saponin Rb 1The research of separation, purifying process "; " research and development of natural products " 2008 02 phases have been delivered " extraction separation purified ginsenoside R_ (b from Radix Panacis Quinquefolii 1) and the research of ginsenoside R_e "; " Hebei medical science " the 9th phase of calendar year 2001 has been delivered " the macroporous adsorbent resin method is extracted the total panaquilon craft discussion "; " Chinese Pharmaceutical Journal " 1997 the 10th phases have been delivered " development and the clinical study of Radix Panacis Quinquefolii glycol group saponin injection liquid ".The extraction process that above-mentioned patent and bibliographical information are adopted all is conventional water extraction, comprises warm water extraction, uses the adsorption resin method purifying then, consuming time, power consumption and to extract the rate of transform not high yet.At separation and purification ginsenoside Rb from total panaquilon 1The time, employing be single technology of separating wash-out with organic solvent recrystallization or silica gel column chromatography single-column, exist and use a large amount of organic solvent separation efficiencies low and consuming time, influence ginsenoside Rb 1The rate of recovery, suitability for industrialized production acquires a certain degree of difficulty.
Technology contents
An object of the present invention is to disclose a kind of Ginsenoside Rb that from Radix Panacis Quinquefolii, extracts 1Method, but this method save energy and time reduce pollution to environment, make the Ginsenoside Rb in the extract 1Content further improve, treatment capacity increases, and helps suitability for industrialized production.
Another object of the present invention is to disclose a kind of Ginsenoside Rb 1Powder injection, this powder injection quality is more stable.
Of the present inventionly from Radix Panacis Quinquefolii, extract the Ginsenoside Rb 1The preparation method comprise the steps:
Step 1. is got ginseng powder and is broken into fine powder, with 8-12 water logging bubble doubly, after soak time is 10-60 minute, uses ultrasonic oscillation extraction 1-3 time, each 20-50 minute, filters merging filtrate;
Step 2. filtrate is by macroporous adsorptive resins, and absorption finishes and is washed with water to the effluent liquid clarification, uses the aqueous solution of alkaline, inorganic salts again, and the concentration of alkali is 0.1-5%, washs, and to the elutant clarification, being washed with water to PH again is 5-7; With the ethanol elution of 20-95%, the eluent consumption is 1-5 a times of resin demand;
Step 3. is collected elutriant, concentrates, and drying promptly gets the American ginseng total saponins extract;
Step 4. adopts simulated moving bed chromatography technology separation and purification ginsenoside Rb1 monomer from the American ginseng total saponins extract.
In the described step 1, the temperature of soaking institute's water is a normal temperature.
In the described step 1, the frequency of ultrasonic oscillation extraction is 26-80kHz.
In the described step 2, the polymeric adsorbent consumption is 0.5-3 a times of medicinal material weight ratio; The resin model is JD-1 (WLD); Or among D-101, D-201, the XAD-4 any.
Among the above-mentioned preparation method, the aqueous solution of alkaline, inorganic salts can be inorganic salt such as sodium hydroxide or yellow soda ash.
Use simulated moving bed chromatography technology separation and purification ginsenoside Rb from the American ginseng total saponins extract in the described step 4 1Monomer methods is:
A. apparatus characteristic:
This system is made up of wash-out pump, sampling pump, extraction pump, under meter, chromatographic column, magnetic valve, check valve and programmable logic controller and computer;
Wash-out pumping capacity 0-1000ml/min, pressure 0-10mpa; Sampling pump flow 0-30ml/min, pressure 0-8mpa; Extraction pumping capacity 0-100ml/min, pressure 0-10mpa; Working temperature: 20-25 ℃.
Chromatographic column filler: filler is reverse phase silica gel ODS, filler granularity 30-40um;
B. separating step:
1. prepare sample liquid: step 3 gained American ginseng total saponins extract is dissolved in the methyl alcohol, sedimentation, 0.45 μ m membrane filtration, filter liquor concentration 0-10g/ml, standby;
2. the preparation of moving phase: V methyl alcohol: V water=40-55: 60-45;
3. simulated moving bed chromatography parameter: 3 posts of stripping stage, 3 posts of refining section, 2 posts of adsorption stage; Sample introduction flow velocity Uf=3-4ml/min; Wash-out flow rate pump Ud=50-70ml/min; Extraction liquid flow velocity Ue=20-40ml/min; Residual solution flow velocity Ur=10-12ml/min; Switching time ts=5-7min.
4. concentrate: simulation moving-bed effusive residual solution is concentrated into dried with the film rotatory evaporator at 65 ℃, washes out with methyl alcohol, vacuum is dried to constant weight for 65 ℃, is the simulation moving-bed product of preparing;
D. recrystallization: the said products is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filters, after the filtrate drying white powder, be sublimed ginsenoside Rb 1Monomer.
Another object of the present invention is to disclose a kind of Ginsenoside Rb of using 1The preparation method of preparation powder injection:
1, spray-drying process
Get the isolating Ginsenoside Rb of the present invention 1, in the workshop below 100 grades, adding 5-25 water doubly, 40--90 ℃ of stirring and dissolving adds suitable quantity of water dissolubility pharmaceutical excipient, and adjusting PH is 5.5-8.5, soup sterile filtration, aseptic spraying drying, aseptic subpackaged, promptly;
Among the above-mentioned preparation method, water-soluble pharmaceutical excipient can also be low molecular dextran, glucose, lactose, sodium-chlor, calcium chloride etc.;
2, freeze-drying
Get the isolating Ginsenoside Rb of the present invention 1, in the workshop below 100 grades, adding 5-25 water doubly, 40--90 ℃ of stirring and dissolving adds suitable quantity of water dissolubility pharmaceutical excipient, and adjusting PH is 5.5-8.5, and soup sterile filtration is aseptic subpackaged, aseptic lyophilize, sealing by fusing, promptly;
3, a step desiccating method
Get the isolating Ginsenoside Rb of the present invention 1, move into the workshop below 100 grades, add an amount of water for injection and auxiliary material, regulate pH value, sterile filtration, spraying drying or lyophilize, promptly;
By above-mentioned powder injection preparation method, with the 50mg Ginsenoside Rb 1Making specification is in the 50mg/2ml cillin bottle, or in the 2ml ampoule, perhaps the 100mg Ginsenoside Rb 1Making specification is in the 100mg/2ml cillin bottle, or in the 2ml ampoule.
The present invention is to extracting the Ginsenoside Rb from Radix Panacis Quinquefolii 1Carried out innovative research.The one, the change medicine materical crude slice is fine powder, is beneficial to the extraction of medicine; The 2nd, change is boiled and is soak at room temperature, has saved the energy, and has improved extraction yield; The 3rd, use ultrasonic oscillation extraction, save energy greatly, time and total panaquilon comprise the Ginsenoside Rb 1The extraction rate of transform; The 4th, at the absorption washing column period of the day from 11 p.m. to 1 a.m that finishes, used inorganic washing composition, make that total saponin content improves greatly in the extract.The 5th, simulated moving bed chromatography technology is separation and purification ginsenoside Rb from the American ginseng total saponins extract 1Monomer makes separation purifying technique simple to operate, and treatment capacity increases, minimizing consuming time.Powder injection preparation of the present invention is more stable, transports and store more convenient.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1: ultrasonic oscillation extraction and warm water soaking extraction process are relatively
Method 1: warm water soaking extraction+macroporous adsorbent resin
Get the Radix Panacis Quinquefolii of the following long shoot of Jilin, place of production 5g, grind and be powder, cross 100 mesh sieves, and detect ginsenoside Rb1's content, respectively get 50g, be numbered respectively 1 and No. 2.Get powder No. 1, steeped 1 hour with 40 times 90 ℃ water loggings, water bath heat preservation stirs frequently, leaves standstill 1 hour, filters.Filtrate is by 1.5 times of amount macroporous adsorbent resins (model: D-101 is product type lot number only: 070305 product standard: Tianjin Q, HG3790-91 Tianjin sea light chemical industry company limited produce), after absorption finishes, wash with water to colourless, be washed till colourlessly again with 0.5% NaOH solution, and wash with water, use 70% ethanol elution of 4 times of amount of resin again to neutrality, elutriant reclaims ethanol, concentrate, drying under reduced pressure gets the total panaquilon extract No. 1.
Method 2: ultrasonic extraction+macroporous adsorbent resin
Other gets powder No. 2, behind the water logging bubble 15min with 10 times of normal temperature, extracts 3 times with ultrasonic wave (ultrasonic wave medicine handler " the 4th generation " frequency 26KHz, 47KHz, 70KHz Jining Sinobest Electronics Co., Ltd. produce), extract frequency 26KHz, each 30 minutes, filter merging filtrate; Filtrate, washes with water to colourless after absorption finishes by 1.5 times of amount macroporous adsorbent resins, and other is washed till colourless with 0.5% NaOH solution, and wash with water to neutrality, use 70% ethanol elution of 4 times of amount of resin at last, elutriant reclaims ethanol, concentrate, drying under reduced pressure gets the total panaquilon extract No. 2.
More than experiment repeats 3 times, gets mean number 3 times.Ginsenoside Rb after testing 1Content (%) the results are shown in Table 1.
Table 1 ultrasonic oscillation extraction and warm water soaking extraction process are relatively
The Radix Panacis Quinquefolii medicine materical crude slice is extracted in this experiment, changes into Radix Panacis Quinquefolii fine powder after crushed extracting, and makes the surface-area of its contact solvent significantly improve total panaquilon, Ginsenoside Rb 1The isoreactivity composition more is soluble in the solvent, in order to improving its extraction yield.More beyond thoughtly be to boil and extract or method that warm water soaking extracts is changed into behind the soak at room temperature technology with ultrasonic oscillation extraction and significantly improved total panaquilon and comprise the Ginsenoside Rb 1The extraction rate of transform.
Experimental example 2: macroporous adsorbent resin technical study
Method 1: get the Radix Panacis Quinquefolii of the following long shoot of Jilin, place of production 5g, grind and be powder, cross 100 mesh sieves, and detect ginsenoside Rb1's content.Respectively get 50g, be numbered respectively 2-1 and 2-2 number.Get the 2-1 powder, behind the water logging bubble 15min with 10 times of normal temperature, (ultrasonic wave medicine handler " the 4th generation " frequency 26KHz, 47KHz, 70KHz Jining Sinobest Electronics Co., Ltd. produce with ultrasonic wave, extract 3 times down together), extract frequency 26KHz, each 30 minutes, filter merging filtrate; (model: D-101 is product type lot number only: 070305 product standard: Tianjin Q, HG3790-91 Tianjin sea light chemical industry company limited produce filtrate by 1.5 times of amount macroporous adsorbent resins, down together), after absorption finishes, wash with water to colourless, use 70% ethanol elution of 4 times of amount of resin again, elutriant reclaims ethanol, concentrates, drying under reduced pressure gets the total panaquilon extract 2-1 number.
Method 2: other gets the 2-2 powder, behind the water logging bubble 15min with 10 times of normal temperature, uses ultrasonic extraction 3 times, extracts frequency 26KHz, each 30 minutes, filters merging filtrate; Filtrate is by 1.5 times of amount macroporous adsorbent resins, after absorption finishes, wash with water to colourless, be washed till in addition colourlessly, and wash with water, use 70% ethanol elution of 4 times of amount of resin at last to neutrality with 0.5% NaOH solution, elutriant reclaims ethanol, concentrate, drying under reduced pressure gets the total panaquilon extract 2-2 number.More than experiment repeats 3 times, gets mean number 3 times.Ginsenoside Rb1's content (%) the results are shown in Table 2 after testing.
Table 2 compares with the technology of not washing adsorption column with the solution washing adsorption column of the inorganic salt that contain alkalescence
Figure G2009100772650D0000051
Experimental example 3: simulated moving bed chromatography technology is separation and purification ginsenoside Rb from the American ginseng total saponins extract 1Monomeric
From the total panaquilon extract, separating purified ginsenoside Rb 1In the monomeric technological process, what we adopted is simulated moving bed chromatography, and vacuum concentration evaporate to dryness and recrystallizing technology obtain ginsenoside Rb 1Monomeric.This technology has the separation efficiency height, and easily technology is amplified, the advantage of clean environmental protection.
Since simulated moving bed system be one non-linear, nonideal many-degrees of freedom system, the purity of product and yield depend on the parameter optimization of this nonlinear many-degrees of freedom system and selection.Below be optimization and selection to several important parameters
1. the selection of proportion of mobile phase
The selection of table 3 proportion of mobile phase
As seen from Table 3, when the methyl alcohol volume fraction is hanged down, ginsenoside Rb 1Yield is very low, and when the methyl alcohol volume fraction was high, separating power was poor, ginsenoside Rb when V (methyl alcohol): V (water)=45: 55 1Yield is the highest, so proportion of mobile phase is decided to be 45: 55.
2. the selection of ginsenoside mass concentration in the sample introduction
The selection of ginsenoside mass concentration in table 4 sample introduction
Rb when as seen from Table 4, the ginsenoside mass concentration is 0.2g/ml in the sample introduction 1Yield is the highest, so it is chosen as ginsenoside mass concentration in the sample introduction.
3. the selection of switching time
The selection of table 5 switching time
Figure G2009100772650D0000063
As seen from Table 5, switching time is too short, and the flushing of preceding impurity is not enough, is brought in the product and reduces ginsenoside Rb 1Purity.Switching time is oversize, again can be with ginsenoside Rb 1In the impurity, make ginsenoside Rb in the effluent before bringing into 1Purity drop, rear impurity increases.When be 6min switching time, ginsenoside Rb 1Purity the highest, and its yield is not subjected to obviously to influence, so will be chosen to be about 6min switching time.
4. the selection of elution flow rate
The selection of table 6 elution flow rate
Figure G2009100772650D0000071
As seen from Table 6, when elution flow rate was low, fast component flushing degree was not enough, brings impurity in the product into, has influenced ginsenoside Rb 1Yield.Elution flow rate is excessive, part ginsenoside Rb 1Can flow out from the impurity outlet, make ginsenoside Rb 1Yield and purity all be affected.When elution flow rate is 60ml/min, ginsenoside Rb 1Yield the highest, so the regulation elution flow rate is 60ml/min.
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment
Embodiment 1: ginsenoside Rb 1Method for making
Get ginseng powder and be broken into fine powder, with 8-12 water logging bubble doubly, after each soak time is 10-20 minute, use ultrasonic oscillation extraction 1-3 time, each 20-50 minute, the frequency of ultrasonic oscillation extraction is 26-80kHz, filter, merging filtrate, soup is by the macroporous adsorptive resins of 1.5 times of amounts, model is JD-1 (WLD), absorption finishes, and washes with water, and other washs with 0.5% sodium hydroxide solution, be washed with water to neutrality again, with 70% ethanol elution of 4 times of amounts of resin, collect elutriant, concentrate, drying promptly gets the American ginseng total saponins extract.Gained American ginseng total saponins extract is dissolved in the methyl alcohol, sedimentation, 0.45 μ m membrane filtration, filter liquor concentration 0-10g/ml, standby.The preparation of moving phase: V methyl alcohol: V water=45: 55.Simulated moving bed chromatography parameter: 3 posts of stripping stage, 3 posts of refining section, 2 posts of adsorption stage.Sample introduction flow velocity Uf=3-4ml/min; Wash-out flow rate pump Ud=50-70ml/min; Extraction liquid flow velocity Ue=20-40ml/min; Residual solution flow velocity Ur=10-12ml/min; Switching time ts=5-7min; Residual solution is the product of simulated moving bed chromatography.Concentrate: simulation moving-bed effusive residual solution is concentrated into dried with the film rotatory evaporator at 65 ℃, washes out with methyl alcohol, vacuum is dried to constant weight for 65 ℃, is the simulation moving-bed product of preparing.Recrystallization: the said products is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, get white powder after the filtrate drying, be sublimed ginsenoside Rb 1Monomer.After high performance liquid chromatograph mensuration purity, standby.
Embodiment 2: ginsenoside Rb 1The spraying drying powder injection
Get ginsenoside Rb 1The monomer extract adds 20 times water in the workshop below 100 grades, in 60 ℃ of stirring and dissolving, add 5% low molecular dextran, and adjusting PH is 6-7, soup sterile filtration, and aseptic spraying drying, aseptic subpackaged in the 2ml cillin bottle, every contains ginsenoside Rb 150mg, promptly.
Embodiment 3: ginsenoside Rb 1The lyophilize powder injection
Get ginsenoside Rb 1Monomer adds 7 times water in the workshop below 100 grades, in 60 ℃ of stirring and dissolving, add 5% low molecular dextran, and adjusting PH is 6-7, and soup sterile filtration is aseptic subpackaged in the 2ml ampoule, lyophilize, and sealing by fusing, every ampoule contains ginsenoside Rb 150mg, promptly.
Embodiment 4: ginsenoside Rb 1One step xeraphium injection
Get ginseng powder and be broken into fine powder, with 8-12 water logging bubble doubly, after each soak time is 10-20 minute, use ultrasonic oscillation extraction 1-3 time, each 20-50 minute, the frequency of ultrasonic oscillation extraction is 26-80kHz, filters merging filtrate, filtrate is by the macroporous adsorptive resins of 1.5 times of amounts of medicinal material, model is JD-1 (WLD), and absorption finishes, and washes with water, continue with the washing of 0.5% sodium hydroxide solution, after impurity is thoroughly removed, be washed with water to neutrality, with 70% ethanol elution of 4 times of amounts of resin, collect elutriant, concentrate, drying promptly gets the American ginseng total saponins extract.Gained American ginseng total saponins extract is dissolved in the methyl alcohol, sedimentation, 0.45 μ m membrane filtration, filter liquor concentration 0-10g/ml, standby.The preparation of moving phase: V methyl alcohol: V water=45: 55.Simulated moving bed chromatography parameter: 3 posts of stripping stage, 3 posts of refining section, 2 posts of adsorption stage.Sample introduction flow velocity Uf=3-4ml/min; Wash-out flow rate pump Ud=50-70ml/min; Extraction liquid flow velocity Ue=20-40ml/min; Residual solution flow velocity Ur=10-12ml/min; Switching time ts=5-7min; Residual solution is the product of simulated moving bed chromatography.Concentrate: simulation moving-bed effusive residual solution is concentrated into dried with the film rotatory evaporator at 65 ℃, washes out with methyl alcohol, vacuum is dried to constant weight for 65 ℃, is the simulation moving-bed product of preparing.Recrystallization: the said products is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, filtrate is adopted lyophilize or the resulting white powder of vacuum concentration evaporate to dryness technology, is sublimed ginsenoside Rb 1Monomer.After high performance liquid chromatograph mensuration purity, standby;
With ginsenoside Rb 1Monomer moves into the workshop below 100 grades, adds an amount of water for injection and auxiliary material, regulates pH value, sterile filtration, and the filtrate spraying drying is sub-packed in the 2ml cillin bottle, and every cillin bottle contains ginsenoside Rb 150mg rolls lid, promptly; Or the filtrate packing, lyophilize, sealing by fusing, every ampoule contains ginsenoside Rb 150mg, promptly.

Claims (9)

1. one kind is extracted the Ginsenoside Rb from Radix Panacis Quinquefolii 1The preparation method, it is characterized in that this method comprises the steps:
Step 1. is got ginseng powder and is broken into fine powder, with 8-12 water logging bubble doubly, after soak time is 10-60 minute, uses ultrasonic oscillation extraction 1-3 time, each 20-50 minute, filters merging filtrate;
Step 2. filtrate is by macroporous adsorptive resins, and absorption finishes and is washed with water to the effluent liquid clarification, is that the aqueous solution of the alkaline, inorganic salts of 0.1-5% washs with the concentration of alkali again, clarifies to elutant, and being washed with water to PH again is 5-7; Use the ethanol elution of 20-95% again, the eluent consumption is 1-5 a times of resin demand;
Step 3. is collected elutriant, concentrates, and drying promptly gets the American ginseng total saponins extract;
Step 4. adopts simulated moving bed chromatography technology separation and purification ginsenoside Rb from the American ginseng total saponins extract 1Monomer.
2. the method for claim 1 is characterized in that the temperature of immersion institute water in this method steps 1 is a normal temperature.
3. the method for claim 1, the frequency that it is characterized in that ultrasonic oscillation extraction in this method steps 1 is 26-80kHz.
4. the method for claim 1, it is characterized in that polymeric adsorbent consumption in this method steps 2 be the medicinal material weight ratio 0.5-3 doubly.
5. the method for claim 1 is characterized in that the aqueous solution of these method steps 2 neutral and alkali inorganic salt can be sodium hydroxide or yellow soda ash.
6. as described any one method of claim 1-5, it is characterized in that in this method steps 4 with simulated moving bed chromatography technology separation and purification ginsenoside Rb from the American ginseng total saponins extract 1In the monomer methods:
The sample liquid preparation: step 3 gained American ginseng total saponins extract is dissolved in the methyl alcohol, sedimentation, 0.45 μ m membrane filtration, filter liquor concentration 0-10g/ml, standby;
The preparation of moving phase: methyl alcohol: water=4540-55: 5560-45;
Simulated moving bed chromatography parameter: 3 posts of stripping stage, 3 posts of refining section, 2 posts of adsorption stage; Sample introduction flow velocity Uf=3-4ml/min; Wash-out flow rate pump Ud=50-70ml/min; Extraction liquid flow velocity Ue=20-40ml/min; Residual solution flow velocity Ur=10-12ml/min; Switching time ts=5-7min;
Concentrate: simulation moving-bed effusive residual solution is concentrated into dried with the film rotatory evaporator at 65 ℃, washes out with methyl alcohol, vacuum is dried to constant weight for 65 ℃, is the simulation moving-bed product of preparing;
Recrystallization: the said products is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, get white powder after the filtrate drying, be sublimed ginsenoside Rb 1Monomer.
7. method as claimed in claim 6 is characterized in that the Ginsenoside Rb 1Add 5-25 water doubly in the workshop below 100 grades, 40--90 ℃ of stirring and dissolving adds suitable quantity of water dissolubility pharmaceutical excipient, and adjusting PH is 5.5-8.5, soup sterile filtration, and aseptic spraying drying, aseptic subpackaged, make powder injection.
8. method as claimed in claim 6 is characterized in that the Ginsenoside Rb 1Add 5-25 water doubly in the workshop below 100 grades, 40-90 ℃ of stirring and dissolving adds suitable quantity of water dissolubility pharmaceutical excipient, and adjusting PH is 5.5-8.5, soup sterile filtration, the soup after the above-mentioned sterile filtration, aseptic subpackaged, aseptic lyophilize, sealing by fusing is made powder injection.
9. method as claimed in claim 6 is characterized in that the Ginsenoside Rb 1Move into the workshop below 100 grades, add an amount of water for injection and auxiliary material, regulate pH value, sterile filtration, powder injection is made in spraying drying or lyophilize.
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CN101230080B (en) * 2007-01-22 2011-08-17 李平亚 simulated moving bed chromatography separation of 20(S) and 20(R)-ginsenoside Rg3 enantiomer

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CN102336799A (en) * 2010-07-22 2012-02-01 辽宁科技大学 Simulated moving bed chromatography separation method for preparing ginsenoside Rb1
CN102793160A (en) * 2011-05-28 2012-11-28 张文知 Method for preparing American ginseng extract powder
CN103664855A (en) * 2012-09-20 2014-03-26 浙江大学苏州工业技术研究院 Preparation method of high-purity oligomer lotus seedpod procyanidin
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CN104193793A (en) * 2014-08-07 2014-12-10 中国农业科学院特产研究所 Method for preparing ginsenoside Rb3 in American ginseng fruit by adopting simulated moving bed
CN104193793B (en) * 2014-08-07 2016-09-07 中国农业科学院特产研究所 Simulation moving bed is used to prepare the method for ginsenoside Rb3 in Fructus Panacis Quinquefolii
CN106806394A (en) * 2015-11-30 2017-06-09 鄂尔多斯市威蒙医药科技有限公司 A kind of method for processing ginseng or American Ginseng active ingredients
CN107693558A (en) * 2017-11-09 2018-02-16 长春中医药大学 The separation method of general ginsenoside
CN107693558B (en) * 2017-11-09 2020-10-02 长春中医药大学 Method for separating total ginsenoside
CN109293711A (en) * 2018-09-30 2019-02-01 邵阳学院 A method of Lilium brownie class compound is extracted using Simulation moving bed
CN111072747A (en) * 2019-12-26 2020-04-28 王传涛 Ginsenoside and ultrasonic extraction method thereof

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