CN101781351B - 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 PDFInfo
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- CN101781351B CN101781351B CN2009100772650A CN200910077265A CN101781351B CN 101781351 B CN101781351 B CN 101781351B CN 2009100772650 A CN2009100772650 A CN 2009100772650A CN 200910077265 A CN200910077265 A CN 200910077265A CN 101781351 B CN101781351 B CN 101781351B
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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
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 to treat cardiovascular and cerebrovascular diseases that the ginsenoside Rb1 processes, belong to formulation art.
Background technology
Radix Panacis Quinquefolii is claimed 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 away heat and promoting production of body 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 tcm-" 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 a large amount of organic solvent separation efficiencies of use low and consuming time, influence ginsenoside Rb
1The 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, and after soak time is 10-60 minute, with ultrasonic oscillation extraction 1-3 time, 20-50 minute at every turn, filtration, merging filtrate;
Step 2. filtrating is through macroporous adsorptive resins, and absorption finishes and is washed with water to the effluent 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 SMBC technology separation and purification ginsenoside Rb1 monomer from the American ginseng total saponins extract.
In the said step 1, the temperature of soaking institute's water is a normal temperature.
In the said step 1, the frequency of ultrasonic oscillation extraction is 26-80kHz.
In the said 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 the D-101, D-201, 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.
In the said step 4 with SMBC technology separation and purification ginsenoside Rb from the American ginseng total saponins extract
1Monomer methods is:
A. apparatus characteristic:
This system is made up of wash-out pump, sampling pump, extraction pump, under meter, chromatographic column, SV, vacuum breaker 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, subsequent use;
2. the preparation of moving phase: V methyl alcohol: V water=40-55: 60-45;
3. SMBC 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: said product is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filters, after the filtrating 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 get;
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 gets;
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 get;
By above-mentioned powder injection preparation method, with the 50mg Ginsenoside Rb
1Processing specification is in the 50mg/2ml cillin bottle, or in the 2ml ampoule, perhaps the 100mg Ginsenoside Rb
1Processing 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 practiced thrift 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, SMBC 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.Filtrating is through 1.5 times of amount macroporous adsorbent resins (model: D-101 is article type lot number only: 070305 product standard: Tianjin Q, HG3790-91 Tianjin sea light chemical industry ltd produce), and after absorption finished, water was washed till colourless; Be washed till colourlessly again with 0.5% NaOH solution, and water is washed till neutrality, uses 70% ethanol elution of 4 times of amount of resin again; 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 UW (UW medicine handler " the 4th generation " frequency 26KHz, 47KHz, 70KHz Jining Sinobest Electronics Co., Ltd. produce); Extract frequency 26KHz; Each 30 minutes, filter merging filtrate; Filtrating is through 1.5 times of amount macroporous adsorbent resins, and after absorption finished, water was washed till colourless, and other is washed till colourless with 0.5% NaOH solution; And water is washed till neutrality, uses 70% ethanol elution of 4 times of amount of resin at last, and elutriant reclaims ethanol; Concentrate, drying under reduced pressure gets the total panaquilon extract No. 2.
More than the experiment repetition is 3 times, gets mean number 3 times.Through detecting ginsenoside Rb
1Content (%), the result sees 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, (UW medicine handler " the 4th generation " frequency 26KHz, 47KHz, 70KHz Jining Sinobest Electronics Co., Ltd. produce with UW; Extract 3 times down together), extract frequency 26KHz, each 30 minutes; Filter merging filtrate; Filtrate through 1.5 times of amount macroporous adsorbent resins (model: D-101 is article type lot number only: 070305 product standard: Tianjin Q, HG3790-91 Tianjin sea light chemical industry ltd produce, down together), after absorption finishes; Water is washed till 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 of 10 times of normal temperature bubble 15min, with ultrasonic extraction 3 times, extracts frequency 26KHz, and each 30 minutes, filtration, merging filtrate; Filtrating is through 1.5 times of amount macroporous adsorbent resins, and after absorption finished, water was washed till colourless; Be washed till in addition colourlessly with 0.5% NaOH solution, and water is washed till neutrality, uses 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 2-2 number.More than the experiment repetition is 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
Experimental example 3: SMBC 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 SMBC, and vacuum concentration evaporate to dryness and recrystallizing technology obtain ginsenoside Rb
1Monomeric.This technology has the separation efficiency height, is prone to technology and amplifies the advantage of clean environmental protection.
Since simulated moving bed system be one non-linear, nonideal many-degrees of freedom system, product gas purity 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
Visible from table 3, when the methyl alcohol volume(tric)fraction is hanged down, ginsenoside Rb
1Yield is very low, and when the methyl alcohol volume(tric)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
Visible from table 4, Rb when 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
Visible from table 5, switching time is too short, and preceding impurity flushing 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 elute before bringing into
1Purity drop, rear impurity increases.When be 6min switching time, ginsenoside Rb
1Purity the highest, and its yield do not receive 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
Visible 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, with ultrasonic oscillation extraction 1-3 time; Each 20-50 minute, the frequency of ultrasonic oscillation extraction was 26-80kHz, filtered merging filtrate; Soup is through the macroporous adsorptive resins of 1.5 times of amounts, and model is JD-1 (WLD), and absorption finishes, and uses water washing; Other washs with 0.5% sodium hydroxide solution, is washed with water to neutrality again, with 70% ethanol elution of 4 times of amounts of resin, collects 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, subsequent use.The preparation of moving phase: V methyl alcohol: V water=45: 55.SMBC 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 SMBC.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: said product is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, get white powder after the filtrating drying, be sublimed ginsenoside Rb
1Monomer.After high performance liquid chromatograph mensuration purity, subsequent use.
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 gets.
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 gets.
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, with ultrasonic oscillation extraction 1-3 time; Each 20-50 minute, the frequency of ultrasonic oscillation extraction was 26-80kHz, filtered merging filtrate; Filtrating is through the macroporous adsorptive resins of 1.5 times of amounts of medicinal material, and model is JD-1 (WLD), and absorption finishes, and uses water washing; Continue with the washing of 0.5% sodium hydroxide solution, impurity is thoroughly removed after, 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, subsequent use.The preparation of moving phase: V methyl alcohol: V water=45: 55.SMBC 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 SMBC.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: said product is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, filtrating 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, subsequent use;
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 filtrating spraying drying is sub-packed in the 2ml cillin bottle, and every cillin bottle contains ginsenoside Rb
150mg rolls lid, promptly gets; Or the filtrating packing, lyophilize, sealing by fusing, every ampoule contains ginsenoside Rb
150mg promptly gets.
Claims (7)
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, and after soak time is 10-60 minute, with ultrasonic oscillation extraction 1-3 time, 20-50 minute at every turn, filtration, merging filtrate;
Step 2. filtrating is through macroporous adsorptive resins, and absorption finishes and is washed with water to the effluent clarification, and the concentration of using alkali is again washed as the aqueous solution of the alkaline, inorganic salts of 0.1-5%, and to the elutant clarification, 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 SMBC technology separation and purification ginsenoside Rb from the American ginseng total saponins extract
1Monomer, described SMBC technology is:
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, subsequent use;
The preparation of moving phase: methyl alcohol: water=40-55: 60-45;
SMBC 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: said product is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, get white powder after the filtrating drying, be sublimed ginsenoside Rb
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 medicinal material weight 0.5-3 doubly.
5. use the Ginsenoside Rb for one kind
1The preparation method of preparation powder injection is characterized in that the Ginsenoside Rb
1Powder injection is processed by following method:
Step 1. is got ginseng powder and is broken into fine powder, with 8-12 water logging bubble doubly, and after soak time is 10-60 minute, with ultrasonic oscillation extraction 1-3 time, 20-50 minute at every turn, filtration, merging filtrate;
Step 2. filtrating is through macroporous adsorptive resins, and absorption finishes and is washed with water to the effluent clarification, and the concentration of using alkali is again washed as the aqueous solution of the alkaline, inorganic salts of 0.1-5%, and to the elutant clarification, 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 SMBC technology separation and purification ginsenoside Rb from the American ginseng total saponins extract
1Monomer, described SMBC technology is:
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, subsequent use;
The preparation of moving phase: methyl alcohol: water=40-55: 60-45;
SMBC 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: said product is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, get white powder after the filtrating drying, be sublimed ginsenoside Rb
1Monomer;
With above-mentioned sublimed Ginsenoside Rb
1Monomer adds 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, process powder injection.
6. use the Ginsenoside Rb for one kind
1The preparation method of preparation powder injection is characterized in that the Ginsenoside Rb
1The following method of powder injection is processed:
Step 1. is got ginseng powder and is broken into fine powder, with 8-12 water logging bubble doubly, and after soak time is 10-60 minute, with ultrasonic oscillation extraction 1-3 time, 20-50 minute at every turn, filtration, merging filtrate;
Step 2. filtrating is through macroporous adsorptive resins, and absorption finishes and is washed with water to the effluent clarification, and the concentration of using alkali is again washed as the aqueous solution of the alkaline, inorganic salts of 0.1-5%, and to the elutant clarification, 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 SMBC technology separation and purification ginsenoside Rb from the American ginseng total saponins extract
1Monomer, described SMBC technology is:
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, subsequent use;
The preparation of moving phase: methyl alcohol: water=40-55: 60-45;
SMBC 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: said product is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, get white powder after the filtrating drying, be sublimed ginsenoside Rb
1Monomer;
Above-mentioned sublimed Ginsenoside Rb
1Monomer adds 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 processed powder injection.
7. use the Ginsenoside Rb for one kind
1The preparation method of preparation powder injection is characterized in that the Ginsenoside Rb
1Powder injection is processed by following method:
Step 1. is got ginseng powder and is broken into fine powder, with 8-12 water logging bubble doubly, and after soak time is 10-60 minute, with ultrasonic oscillation extraction 1-3 time, 20-50 minute at every turn, filtration, merging filtrate;
Step 2. filtrating is through macroporous adsorptive resins, and absorption finishes and is washed with water to the effluent clarification, and the concentration of using alkali is again washed as the aqueous solution of the alkaline, inorganic salts of 0.1-5%, and to the elutant clarification, 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 SMBC technology separation and purification ginsenoside Rb from the American ginseng total saponins extract
1Monomer, described SMBC technology is:
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, subsequent use;
The preparation of moving phase: methyl alcohol: water=40-55: 60-45;
SMBC 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: said product is added propyl carbinol 5ml ratio ultrasonic dissolution in 1g, filter, get white powder after the filtrating drying, be sublimed ginsenoside Rb
1Monomer;
With above-mentioned sublimed Ginsenoside Rb
1Monomer moves into the workshop below 100 grades, adds an amount of water for injection and auxiliary material, regulates the pH value, sterile filtration, and powder injection is processed in spraying drying or lyophilize.
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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 |
| CN103664855B (en) * | 2012-09-20 | 2015-09-09 | 浙江大学苏州工业技术研究院 | A kind of high purity oligomer LSPC preparation method |
| 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 |
| 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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