CN102772462B - A kind of method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii - Google Patents
A kind of method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii Download PDFInfo
- Publication number
- CN102772462B CN102772462B CN201110120199.8A CN201110120199A CN102772462B CN 102772462 B CN102772462 B CN 102772462B CN 201110120199 A CN201110120199 A CN 201110120199A CN 102772462 B CN102772462 B CN 102772462B
- Authority
- CN
- China
- Prior art keywords
- solution
- resin
- hour
- ethanol
- column volumes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Steroid Compounds (AREA)
Abstract
The invention discloses a kind of method extracted from Radix Panacis Quinquefolii and separate Radix Ginseng total saponins.The present invention uses alcohol reflux, water precipitating, macroporous adsorbent resin remove impurity, a series of efficient extracting and developing such as ion-exchange resin decolorization and the technological means of purification, the Radix Ginseng total saponins obtained is white powder, this Radix Ginseng total saponins includes ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, Ginsenoside Rc, ginsenoside Rd, and wherein total purity of ginsenoside Rg1, ginsenoside Re and ginsenoside Rb1 is more than 74.0%.This production technology is simple, pollution-free, is suitable for producing greatly.
Description
Technical field
The present invention relates to a kind of method extracted from Radix Panacis Quinquefolii and separate Radix Ginseng total saponins.
Background technology
Radix Panacis Quinquefolii (Panax quinquefolium L.) is Araliaceae (Araliaceae) Panax (Panax) herbaceos perennial, originates in eastern United States and Canada.Have another name called U.S.'s Radix Ginseng, Radix Panacis Quinquefolii, Radix Panacis Quinquefolii and Guangzhou ginseng.Begin to be loaded in supplementary Amplifications of the Compendium of Materia Medica in China, the medicinal history of existing more than 200 year.There is the effect such as lung benefiting asthenic fire cloudy, clear, promoting the production of body fluid to quench thirst, control chronic cough of deficiency lung, lose blood, dry throat and mouth, deficiency-heat are tired of tired etc.." Records of Tradition Chinese and Western Medicine in Combination " carries: " Radix Panacis Quinquefolii, cool in nature and mend, all Radix Ginsengs to be used and not by the temperature compensation person of Radix Ginseng, all can with this instead of." just because of Radix Panacis Quinquefolii has the benefit of Radix Ginseng, and without the dry property of Radix Ginseng, it is described as famous and precious tonic and well-known.
Containing saponins, polyacetylene class, volatile oil, polysaccharide and amino acids in Radix Panacis Quinquefolii, main active component is saponins compound.Numerous studies show, difference due to structure, various ginsenosides have the pharmacologically active of its uniqueness, thus pharmacologically active is multiformity: ginsenoside has resisting fatigue, slow down aging, regulates central nervous system, improves immunity of organisms, improve the effects such as cardiovascular and cerebrovascular vessel blood supply insufficiency, suppression growth of tumour cell.
Disclose the patent of invention of the extraction of some American ginseng total saponins, purification in recent years.Chinese Patent Application No. 03127613.X discloses a kind of method extracted from Fructus Panacis Quinquefolii, refine Radix Ginseng total saponins, Fructus Panacis Quinquefolii is carried out water carry, macroporous adsorbent resin remove impurity, decolour, be dried, although the method is simple, but color is relatively deep, yield and purity the highest.Chinese Patent Application No. 03127632.6 discloses a kind of production technology refining total saponins from Radix Panacis Quinquefolii and stem and leaf of Radix Panacis Quinquefolii, Radix Panacis Quinquefolii is crossed stem and leaf of Radix Panacis Quinquefolii and pulverizes as coarse powder, water carries, precipitate with ethanol, alkali deposited, macroporous adsorbent resin remove impurity, activated carbon decolorizing, lyophilizing.The purity of the method gained total saponins is higher, but complex steps, yield are low.Chinese Patent Application No. 200610014229.6 discloses the preparation method of a kind of American ginseng total saponins, and Radix Panacis Quinquefolii adds solvent, extracts after alkali tune, and macroporous type anion exchange resin remove impurity, decolouring, the method may make some ginsenoside's structure change.Chinese Patent Application No. 200610109414.3 discloses a kind of preparation method extracting total saponins from Radix Panacis Quinquefolii or stem and leaf of Radix Panacis Quinquefolii, circulated in countercurrent supersound extraction, precipitate with ethanol, macroporous resin column remove impurity, decolorizing column decolouring, spray drying etc., the method step is cumbersome.
Summary of the invention
The present invention provides a kind of method extracted from Radix Panacis Quinquefolii and separate Radix Ginseng total saponins, and the method comprises the steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 6-12 times amount 30%-70% ethanol solution, heating and refluxing extraction 2-3 time, each 1h-3h every time, soak 60min-90min first, filter；Filtrate merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 1:2-2:1, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 3 ~ 5 times, shakes up, place refrigerator 12h ~ 24h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: the weight ratio of amount of resin is that 1:2-1.6:1 weighs macroporous adsorbent resin, and loading blade diameter length ratio is the chromatographic column of 1:3-1:13, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 4.5-9 times of column volume/hour, saturated 1h-3h;With the distilled water of 5 times of-10 times of column volumes carry out eluting except sugar, elution flow rate be 4.5-12 times of column volume/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 4.5-12 times of column volume/hour；Carry out eluting with the ethanol solution of 5-15 times of column volume 70%, elution flow rate be 4.5-12 times of column volume/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: the weight ratio of amount of resin is that 3:1-1:1 weighs weak-base anion-exchange resin, and loading blade diameter length ratio is the chromatographic column of 1:3-1:6, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 3 times of-5 times of column volumes 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
The present invention extracts from Radix Panacis Quinquefolii and separates the method for Radix Ginseng total saponins and preferably comprise following steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 6 times amount 70% ethanol solution, heating and refluxing extraction 3 times, each 3h every time, soak 60min first, filter；Filtrate merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 1:2, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 5 times, shakes up, place refrigerator 12h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: the weight ratio of amount of resin is that 1:2 weighs macroporous adsorbent resin, and loading blade diameter length ratio is the chromatographic column of 1:13, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 4.5 times of column volumes/hour, saturated 3h;With the distilled water of 5 times of column volumes carry out eluting except sugar, elution flow rate be 12 times of column volumes/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 4.5 times of column volumes/hour；Carry out eluting with the ethanol solution of 15 times of column volumes 70%, elution flow rate be 4.5 times of column volumes/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: the weight ratio of amount of resin is that 1:1 weighs weak-base anion-exchange resin, and loading blade diameter length ratio is the chromatographic column of 1:3, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 5 times of column volume 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
The present invention extracts the method for separation Radix Ginseng total saponins from Radix Panacis Quinquefolii and also preferably comprises the steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 12 times amount 30% ethanol solution, heating and refluxing extraction 2 times, each 1h every time, soak 90min first, filter；Filtrate merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 2:1, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 3 times, shakes up, place refrigerator 24h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: the weight ratio of amount of resin is that 1.6:1 weighs macroporous adsorbent resin, and loading blade diameter length ratio is the chromatographic column of 1:3, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 9 times of column volumes/hour, saturated 1h;With the distilled water of 10 times of column volumes carry out eluting except sugar, elution flow rate be 4.5 times of column volumes/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 12 times of column volumes/hour；Carry out eluting with the ethanol solution of 5 times of column volumes 70%, elution flow rate be 12 times of column volumes/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: the weight ratio of amount of resin is that 2:1 weighs weak-base anion-exchange resin, and loading blade diameter length ratio is the chromatographic column of 1:6, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 3 times of column volume 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
The present invention extracts the method for separation Radix Ginseng total saponins from Radix Panacis Quinquefolii and also preferably comprises the steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 9 times amount 50% ethanol solution, heating and refluxing extraction 3 times, each 2h every time, soak 75min first, filter；Filtrate merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 1:1, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 4 times, shakes up, place refrigerator 18h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: the weight ratio of amount of resin is that 1:1.5 weighs macroporous adsorbent resin, and loading blade diameter length ratio is the chromatographic column of 1:8, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 6 times of column volumes/hour, saturated 2h;With the distilled water of 7.5 times of column volumes carry out eluting except sugar, elution flow rate be 6 times of column volumes/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 6 times of column volumes/hour；Carry out eluting with the ethanol solution of 10 times of column volumes 70%, elution flow rate be 6 times of column volumes/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: the weight ratio of amount of resin is that 3:2 weighs weak-base anion-exchange resin, and loading blade diameter length ratio is the chromatographic column of 1:4.5, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 4 times of column volume 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
The macroporous adsorbent resin that the present invention extracts used in the method separating Radix Ginseng total saponins from Radix Panacis Quinquefolii is preferably the one in HPD100, HPD100A, HPD300, HPD450, AB-8 or D101 resin, and used weak-base ion-exchange resin is 330 resins.
The present invention extracts the method for separation Radix Ginseng total saponins from Radix Panacis Quinquefolii and more preferably comprises the steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 10 times amount 50% ethanol solution, heating and refluxing extraction 3 times, each 1h every time, soak 60min first, filter；Filtrate merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 1:1, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 5 times, shakes up, place refrigerator 12h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: the weight ratio of amount of resin is that 1:1 weighs AB-8 macroporous adsorbent resin, and loading blade diameter length ratio is the chromatographic column of 1:6, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 4.5 times of column volumes/hour, saturated 1h;With the distilled water of 10 times of column volumes carry out eluting except sugar, elution flow rate be 12 times of column volumes/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 12 times of column volumes/hour；Carry out eluting with the ethanol solution of 5 times of column volumes 70%, elution flow rate be 12 times of column volumes/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: the weight ratio of amount of resin is that 3:1 weighs 330 weak-base anion-exchange resins, and loading blade diameter length ratio is the chromatographic column of 1:6, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 3 times of column volume 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
The present invention extracts the Classification system of the raw materials of traditional Chinese medicinal materials Radix Panacis Quinquefolii in the method separating Radix Ginseng total saponins: PANACIS from Radix Panacis Quinquefolii
QUINQUEFOLII RADIX, for the dry root of Araliaceae Radix Panacis Quinquefolii Panax quique folium L..
Radix Panacis Quinquefolii coarse powder of the present invention refers to " coarse powder " of regulation in the Chinese Pharmacopoeia note on the use, it may be assumed that referring to can be all by No. two sieve.But being mixed with can be by No. four sieves powder less than 40%.The volume of the solvent during present invention extraction is that the weight according to medical material is calculated, as used 70% ethanol of 6 times amount, refer to per kilogram medical material, add the ethanol of lower 6 liter 70% of room temperature, i.e. w/v, the medicinal liquid concentrated also refers to per kilogram medical material how many liters, such as with the envelope-bulk to weight ratio of medical material: " being settled to medicinal liquid: medical material envelope-bulk to weight ratio is 1:2 " i.e. per kilogram medical material is concentrated into 2L.
The present invention is used to extract the method separating Radix Ginseng total saponins from Radix Panacis Quinquefolii, five batches of Radix Ginseng total saponinss are produced according to the continuous parameters of embodiment 1, HPLC analyzes total saponins and includes ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, Ginsenoside Rc, ginsenoside Rd, and wherein total purity of ginsenoside Rg1, ginsenoside Re and ginsenoside Rb1 is more than 74.0%.Detailed results is shown in Table 1
The continuous five batches of purity producing ginsenoside of table 1 and rate of transform result
| Lot number | Determination of Content of Ginsenoside Rg_1 % | Ginsenoside Re content % | Ginsenoside Rb1 content % | Rate of transform % |
| 071101 | 2.22 | 19.02 | 53.95 | 100.0 |
| 071112 | 2.12 | 19.29 | 52.69 | 99.1 |
| 071124 | 2.26 | 19.27 | 53.09 | 100.0 |
| 071203 | 2.24 | 19.14 | 53.73 | 99.8 |
| 071219 | 2.28 | 19.20 | 53.28 | 99.4 |
As can be seen here, process for purification of the present invention, process stabilizing is reliable, it is easy to industrialized production, and total purity of the ginsenoside Rg1, ginsenoside Re and the ginsenoside Rb1 that produce is more than 74.0%.And have the advantage that this production technology is simple, pollution-free, it is suitable for producing greatly；And the purity of obtained Radix Ginseng total saponins and yield are the highest.
Detailed description of the invention
The method that following embodiment separates Radix Ginseng total saponins for illustrating the present invention to extract from Radix Panacis Quinquefolii, but it can not constitute any restriction to the scope of the present invention.
Embodiment
1
:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder 10kg, add 60L70% ethanol solution, heating and refluxing extraction 3 times, each 3h every time, soak 60min first, filter；Filtrate merges, and is evaporated to, without alcohol taste, constant volume 20L, obtain concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 100L, shake up, and places refrigerator 12h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: weigh HPD100 macroporous resin 6.25kg, load a diameter of 9.4cm, and height is 122cm, and volume is the chromatographic column of 8.5L, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate is 38L/h, saturated 3h;Carrying out eluting with the distilled water of 42.5L and remove sugar, elution flow rate is 102L/h；With 60L20% ethanol solution remove impurity, elution flow rate is 38L/h；Carrying out eluting with the ethanol solution of 127L70%, elution flow rate is 38L/h, collects the ethanol elution of 70%, obtains refined solution A；
D, for the second time purification: weigh 330 weak-base anion-exchange resin 10kg, load a diameter of 18.2cm, and height is 54.6cm, and volume is the chromatographic column of 14.2L, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, and flow velocity is 71L, collects effluent；Use 71L
70% ethanol solution flows through weak anion resin post, collects effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
Result: Determination of Content of Ginsenoside Rg_1 is 2.15%, ginsenoside Re's content is 19.03% and ginsenoside Rb1's content is 53.77%, turning interest rate is 99.6%.
Embodiment
2
:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder 15Kg, add 180L30% ethanol solution, heating and refluxing extraction 2 times, each 1h every time, soak 90min first, filter；Filtrate merges, and is evaporated to, without alcohol taste, be settled to 30L, obtain concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 90L, shake up, and places refrigerator 24h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: weigh HPD100A macroporous adsorbent resin 15kg, load a diameter of 20cm, and height is 60cm, and volume is the chromatographic column of 19L, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 9 times of column volumes of 171L/h/hour, saturated 1h;Carrying out eluting with the distilled water of 190L and remove sugar, elution flow rate is 86L/h；With 133L20% ethanol solution remove impurity, elution flow rate is 228L/h；Carrying out eluting with the ethanol solution of 190L70%, elution flow rate is 95L/h, collects the ethanol elution of 70%, obtains refined solution A；
D, for the second time purification: weigh D900 weak-base anion-exchange resin 7.5kg, load a diameter of 13cm, and height is 80cm, and volume is the chromatographic column of 11L, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, and flow velocity is 55L/h, collects effluent；Flow through weak anion resin post with 33L70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
Result: Determination of Content of Ginsenoside Rg_1 is 2.20%, ginsenoside Re's content is 19.25% and ginsenoside Rb1's content is 53.12%, turning interest rate is 99.7%.
Embodiment
3
:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder 20kg, add 180L50% ethanol solution, heating and refluxing extraction 3 times, each 2h every time, soak 75min first, filter；Filtrate merges, and is evaporated to, without alcohol taste, be settled to 20L, obtain concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 80L, shake up, and places refrigerator 18h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: weigh HPD300 macroporous adsorbent resin 13Kg, load a diameter of 14cm, and height is 112cm, and volume is the chromatographic column of 17L, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate is 102L/h, saturated 2h;Carrying out eluting with the distilled water of 127.5L and remove sugar, elution flow rate is 102L/h；With 119L20% ethanol solution remove impurity, elution flow rate is 102L/h；Carrying out eluting with the ethanol solution of 170L70%, elution flow rate is 102L/h, collects the ethanol elution of 70%, obtains refined solution A；
D, for the second time purification: weigh 335 weak-base anion-exchange resin 13kg, load a diameter of 17.5cm, and height is 80cm, and volume is the chromatographic column of 19L, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, and flow velocity is 95L/h, collects effluent；Flow through weak anion resin post with 76L70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
Result: Determination of Content of Ginsenoside Rg_1 is 2.17%, ginsenoside Re's content is 19.23% and ginsenoside Rb1's content is 53.06%, turning interest rate is 99.0%.
Embodiment
4
:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder 10kg, add 100L50% ethanol solution, heating and refluxing extraction 3 times, each 1h every time, soak 60min first, filter；Filtrate merges, and is evaporated to, without alcohol taste, be settled to 10L, obtain concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 50L, shake up, and places refrigerator 12h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: weigh AB-8 macroporous adsorbent resin 10kg, load a diameter of 15cm, and height is 85cm, and volume is the chromatographic column of 15L, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate is 67.5L/h, saturated 1h;Carrying out eluting with the distilled water of 150L and remove sugar, elution flow rate is 180L/h；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate is 180L/h；Carrying out eluting with the ethanol solution of 75L70%, elution flow rate is 180L/h, collects the ethanol elution of 70%, obtains refined solution A；
D, for the second time purification: weigh 330 weak-base anion-exchange resin 3.3kg, load a diameter of 10cm, and height is 65cm, and volume is the chromatographic column of 5L, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, and flow velocity is 25L/h, collects effluent；Flow through weak anion resin post with 15L70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
Result: Determination of Content of Ginsenoside Rg_1 is 2.29%, ginsenoside Re's content is 19.32% and ginsenoside Rb1's content is 53.54%, turning interest rate is 100.0%.
Embodiment
5
:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder 10kg, add 60L70% ethanol solution, heating and refluxing extraction 3 times, each 3h every time, soak 60min first, filter；Filtrate merges, and is evaporated to, without alcohol taste, constant volume 20L, obtain concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 100L, shake up, and places refrigerator 12h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: weigh HPD450 macroporous resin 6.25kg, load a diameter of 9.4cm, and height is 122cm, and volume is the chromatographic column of 8.5L, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate is 38L/h, saturated 3h;Carrying out eluting with the distilled water of 42.5L and remove sugar, elution flow rate is 102L/h；With 60L20% ethanol solution remove impurity, elution flow rate is 38L/h；Carrying out eluting with the ethanol solution of 127L70%, elution flow rate is 38L/h, collects the ethanol elution of 70%, obtains refined solution A；
D, for the second time purification: weigh D900 weak-base anion-exchange resin 10kg, load a diameter of 18.2cm, and height is 54.6cm, and volume is the chromatographic column of 14.2L, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, and flow velocity is 71L, collects effluent；Use 71L
70% ethanol solution flows through weak anion resin post, collects effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
Result: Determination of Content of Ginsenoside Rg_1 is 2.37%, ginsenoside Re's content is 18.81% and ginsenoside Rb1's content is 52.91%, turning interest rate is 99.87%.
Embodiment
6
:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder 10kg, add 100L50% ethanol solution, heating and refluxing extraction 3 times, each 1h every time, soak 60min first, filter；Filtrate merges, and is evaporated to, without alcohol taste, be settled to 10L, obtain concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 50L, shake up, and places refrigerator 12h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: weigh D101 macroporous adsorbent resin 10kg, load a diameter of 15cm, and height is 85cm, and volume is the chromatographic column of 15L, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate is 67.5L/h, saturated 1h;Carrying out eluting with the distilled water of 150L and remove sugar, elution flow rate is 180L/h；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate is 180L/h；Carrying out eluting with the ethanol solution of 180L70%, elution flow rate is 180L/h, collects the ethanol elution of 70%, obtains refined solution A；
D, for the second time purification: weigh 330 weak-base anion-exchange resin 3.3kg, load a diameter of 10cm, and height is 65cm, and volume is the chromatographic column of 5L, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, and flow velocity is 25L/h, collects effluent；Flow through weak anion resin post with 15L70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
Result: Determination of Content of Ginsenoside Rg_1 is 2.48%, ginsenoside Re's content is 19.85% and ginsenoside Rb1's content is 54.68%, turning interest rate is 99.95%.
Claims (4)
1. extracting the method separating Radix Ginseng total saponins from Radix Panacis Quinquefolii, the method comprises the steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 6-12 times amount 30%-70% ethanol solution, heating and refluxing extraction 2-3 time, each 1h-3h every time, soak 60min-90min first, filter；The filtrate extracted merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 1:2-2:1, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 3 ~ 5 times, shakes up, place refrigerator 12h ~ 24h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: amount of resin weight ratio is that 1:2-1.6:1 weighs macroporous adsorbent resin, loading blade diameter length ratio is the chromatographic column of 1:3-1:13, described macroporous adsorbent resin is the one in HPD100, HPD100A, HPD300, HPD450, AB-8, D101 resin, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 4.5-9 times of column volume/hour, saturated 1h-3h;With the distilled water of 5 times of-10 times of column volumes carry out eluting except sugar, elution flow rate be 4.5-12 times of column volume/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 4.5-12 times of column volume/hour；Carry out eluting with the ethanol solution of 10-15 times of column volume 70%, elution flow rate be 4.5-12 times of column volume/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: amount of resin weight ratio is that 3:1-1:1 weighs 330 type weak-base anion-exchange resins, loading blade diameter length ratio is the chromatographic column of 1:3-1:6, use acid-alkali treatment weak-base anion-exchange resin, be finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 3 times of-5 times of column volumes 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
The method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii the most according to claim 1, it is characterised in that the method comprises the steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 6 times amount 70% ethanol solution, heating and refluxing extraction 3 times, each 3h every time, soak 60min first, filter；The filtrate extracted merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 1:2, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 5 times, shakes up, place refrigerator 12h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: amount of resin weight ratio is that 1:2 weighs macroporous adsorbent resin, loading blade diameter length ratio is the chromatographic column of 1:13, described macroporous adsorbent resin is the one in HPD100, HPD100A, HPD300, HPD450, AB-8, D101 resin, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 4.5 times of column volumes/hour, saturated 3h;With the distilled water of 5 times of column volumes carry out eluting except sugar, elution flow rate be 12 times of column volumes/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 4.5 times of column volumes/hour；Carry out eluting with the ethanol solution of 15 times of column volumes 70%, elution flow rate be 4.5 times of column volumes/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: amount of resin weight ratio is that 1:1 weighs 330 type weak-base anion-exchange resins, and loading blade diameter length ratio is the chromatographic column of 1:3, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 5 times of column volume 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
The method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii the most according to claim 1, it is characterised in that the method comprises the steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 12 times amount 30% ethanol solution, heating and refluxing extraction 2 times, each 1h every time, soak 90min first, filter；The filtrate extracted merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 2:1, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 3 times, shakes up, place refrigerator 24h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: amount of resin weight ratio is that 1.6:1 weighs macroporous adsorbent resin, loading blade diameter length ratio is the chromatographic column of 1:3, described macroporous adsorbent resin is the one in HPD100, HPD100A, HPD300, HPD450, AB-8, D101 resin, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 9 times of column volumes/hour, saturated 1h;With the distilled water of 10 times of column volumes carry out eluting except sugar, elution flow rate be 4.5 times of column volumes/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 12 times of column volumes/hour；Carry out eluting with the ethanol solution of 10 times of column volumes 70%, elution flow rate be 12 times of column volumes/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: amount of resin weight ratio is that 2:1 weighs 330 type weak-base anion-exchange resins, and loading blade diameter length ratio is the chromatographic column of 1:6, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 3 times of column volume 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
The method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii the most according to claim 1, it is characterised in that the method comprises the steps:
A, extraction: weigh Radix Panacis Quinquefolii coarse powder, add 9 times amount 50% ethanol solution, heating and refluxing extraction 3 times, each 2h every time, soak 75min first, filter；The filtrate extracted merges, and is evaporated to without alcohol taste, is settled to medicinal liquid: medical material envelope-bulk to weight ratio is 1:1, obtains concentrated solution；
B, water precipitating: concentrated solution is diluted with water to 4 times, shakes up, place refrigerator 18h, filters, discards filtering residue, obtain extracting solution；
C, for the first time purification: according to medical material amount: amount of resin weight ratio is that 1:1.5 weighs macroporous adsorbent resin, loading blade diameter length ratio is the chromatographic column of 1:8, described macroporous adsorbent resin is the one in HPD100, HPD100A, HPD300, HPD450, AB-8, D101 resin, processes clean with 95% ethanol and distilled water；By extracting solution loading, adsorption flow rate be 6 times of column volumes/hour, saturated 2h;With the distilled water of 7.5 times of column volumes carry out eluting except sugar, elution flow rate be 6 times of column volumes/hour；With 7 times of column volume 20% ethanol solution remove impurity, elution flow rate be 6 times of column volumes/hour；Carry out eluting with the ethanol solution of 12 times of column volumes 70%, elution flow rate be 6 times of column volumes/hour, collect 70% ethanol elution, obtain refined solution A；
D, for the second time purification: according to medical material amount: amount of resin weight ratio is that 3:2 weighs 330 type weak-base anion-exchange resins, and loading blade diameter length ratio is the chromatographic column of 1:4.5, uses acid-alkali treatment weak-base anion-exchange resin, is finally 7 with distilled water flushing to pH value；Refined solution A is flow through weak-base anion-exchange resin bed, flow velocity be 5 times of column volumes/hour, collect effluent；Flow through weak anion resin post with 4 times of column volume 70% ethanol solution, collect effluent；Two-part effluent is merged and is concentrated into without alcohol taste, obtain refined solution B；
E, lyophilizing: by refined solution B lyophilizing, obtain Radix Ginseng total saponins.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110120199.8A CN102772462B (en) | 2011-05-11 | 2011-05-11 | A kind of method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110120199.8A CN102772462B (en) | 2011-05-11 | 2011-05-11 | A kind of method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102772462A CN102772462A (en) | 2012-11-14 |
| CN102772462B true CN102772462B (en) | 2016-08-24 |
Family
ID=47117719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110120199.8A Active CN102772462B (en) | 2011-05-11 | 2011-05-11 | A kind of method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102772462B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104415070B (en) * | 2013-08-30 | 2019-06-25 | 河北以岭医药研究院有限公司 | A kind of isolation and purification method of Ginsenosides in Panax Ginseng |
| JP6527744B2 (en) * | 2014-04-16 | 2019-06-05 | 花王株式会社 | Method for producing carrot extract |
| CN110974858A (en) * | 2019-03-28 | 2020-04-10 | 泰州医药城国科化物生物医药科技有限公司 | Refined American ginseng total saponin component and method for purifying and preparing American ginseng total saponin |
| CN110025645B (en) * | 2019-04-28 | 2021-05-04 | 云南汉德生物技术有限公司 | Method for extracting total saponins of American ginseng |
| CN111972581A (en) * | 2019-05-23 | 2020-11-24 | 任广哲 | Fresh ginseng liquid beverage and preparation method thereof |
| CN112010911A (en) * | 2019-05-31 | 2020-12-01 | 泰州医药城国科化物生物医药科技有限公司 | Method for purifying total ginsenoside |
| CN110898091A (en) * | 2019-12-18 | 2020-03-24 | 宁波杰顺生物科技有限公司 | Ginseng extract and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1277205A (en) * | 2000-05-17 | 2000-12-20 | 徐绥绪 | Extraction of gensenoside |
| CN101084954A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力之骄药业有限公司 | Method for preparing American ginseng total saponins |
-
2011
- 2011-05-11 CN CN201110120199.8A patent/CN102772462B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1277205A (en) * | 2000-05-17 | 2000-12-20 | 徐绥绪 | Extraction of gensenoside |
| CN101084954A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力之骄药业有限公司 | Method for preparing American ginseng total saponins |
Non-Patent Citations (1)
| Title |
|---|
| 正交试验法优选西洋参醇提工艺;段晓颖;《中国现代应用药学杂志》;20060930;第23卷(第8期);第772-773页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102772462A (en) | 2012-11-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102772462B (en) | A kind of method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii | |
| CN103923152B (en) | A kind of extracting method of mogroside V | |
| CN101336949B (en) | Method for extracting polysaccharide and flavone from Gynura divaricata | |
| CN107898868B (en) | Method for synchronously separating and preparing lycium erythrophyll, lycium barbarum polysaccharide and lycium barbarum flavone from lycium barbarum | |
| CN103387620B (en) | Polysaccharide, total flavones and total alkaloids and preparation method thereof is prepared from Plumula Nelumbinis | |
| CN112870236B (en) | Flavone effective part of abelmoschus manihot and preparation method and application thereof | |
| CN102453075A (en) | Separation and purification process of glycyrrhizic acid | |
| CN104069151B (en) | A kind of high method for preparing extractive of content of mogroside IV | |
| KR101341755B1 (en) | The effective isolation method of panaxadiol saponin fraction from ginseng using pectinase | |
| CN107126452A (en) | Gypenosides and preparation method thereof | |
| CN101348474A (en) | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem | |
| CN102228515B (en) | Separation and enrichment method of total flavones and total alkaloids of Lotus Plumule | |
| CN103965096B (en) | A kind of preparation method being applicable to industrial 1-DNJ | |
| JP5524971B2 (en) | Method for producing an extract fraction enriched with ginsenoside Rg1 or Rb1 from ginseng | |
| CN101974094A (en) | Method for comprehensively extracting cudrania tricuspidata polysaccharides and flavones | |
| CN105213441A (en) | A kind of technique simultaneously preparing glycosides and Folium hydrangeae strigosae total polyphenols | |
| CN103421074A (en) | Method for preparing high purity astragaloside from radix astragali | |
| CN112266399A (en) | High-purity separation and extraction method of epimedium extract | |
| CN110922413A (en) | Extraction and separation method of glabridin | |
| CN103288900A (en) | Icariin preparation process flow | |
| CN102648965A (en) | Industrialization preparation method of lophatherum gracile general flavone | |
| CN102329345A (en) | Method for extracting and purifying sarmentosin in Sedum sarmentosum Bunge | |
| CN107595908A (en) | A kind of extracting method that notoginsenoside is extracted from fresh pseudo-ginseng | |
| CN101234133A (en) | Technique for using tribulus whole grass to extract total saponins of tribulus | |
| CN107619427A (en) | A kind of method of the extraction purification rhizoma paridis saponin I from Paris polyphylla |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |