CN101084929B - Method for extracting saponins of traditional Chinese medicine - Google Patents
Method for extracting saponins of traditional Chinese medicine Download PDFInfo
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- CN101084929B CN101084929B CN 200610014218 CN200610014218A CN101084929B CN 101084929 B CN101084929 B CN 101084929B CN 200610014218 CN200610014218 CN 200610014218 CN 200610014218 A CN200610014218 A CN 200610014218A CN 101084929 B CN101084929 B CN 101084929B
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Abstract
The invention discloses a preparation method of saponins from medicinal herbs which comprises, adding medicinal herbs into solvent, regulating to alkality, extracting, loading on macroporous basic anion-exchange column, eluting with alkali solution and pure water, discarding the flushing liquor, eluting with aqueous ethanol to give eluant, and concentrating.The inventive extraction method has the advantages of high extraction efficiency, high saponins content, good biological activity presevation, and easy industrialization.
Description
Technical field
The invention belongs to the extracting method of Chinese medicine extract, specifically, relate to the extracting method of Chinese medicine saponin component.
Background technology
Saponin (saponins) is the relatively more complicated glycosides compound of a class, and it is that alduronic acid or other organic acid are formed by sapogenin (sapogenins) and sugar.Common sugar has glucose, galactose, rhamnose, arabinose, xylose and other pentose class in the saponin; Common alduronic acid has glucuronic acid, galacturonic acid etc.The form that these sugar or alduronic acid are combined into sugar chain earlier links to each other with sapogenin again.Chemical constitution according to aglycon can be divided into triterpene saponin and steroidal saponin two big classes.The sapogenin of triterpene saponin is a triterpenoid compound, except that indivedual, forms by 30 carbon atoms, and basic framework can be divided into pentacyclic triterpene and tetracyclic triterpene two big classes.Triterpene saponin is distributed widely in nature, its quantity substantially exceeds steroidal saponin, relatively the concentrated area is distributed in the plants such as pulse family, Araliaceae, Cucurbitaceae, campanulaceae, Polygalaceae, Umbelliferae, and plants such as this external Caryophyllaceae, Mimosaceae, Ranunculaceae, Compositae, Sapindaceae, Chenopodiaceae, Rubiaceae, Primulaceae, Theaceae, Hippocastanaceae are also more common.Particularly deep to the research of triterpene saponin in Araliaceae (Radix Ginseng, Caulis Hederae Sinensis etc.), Cucurbitaceae (Herb Gynostemmae Pentaphylli, Fructus Momordicae charantiae etc.), pulse family (Radix Astragali etc.), Umbelliferae (Radix Bupleuri etc.) plant in recent years, and find that some saponin have important biological.The sapogenin of steroidal saponin is a steroid derivative, except that indivedual, forms by 27 carbon atoms, and basic framework is a spirostane, and A, B, C, D, six rings of E, F are arranged.Steroidal saponin is a class important biological material in the plant.Up to now, from plant, be separated to about 400 kinds of steroidal saponins, mostly be distributed in the plants such as Liliaceae, Dioscoreaceae, Solanaceae, Amaryllidaceae, Smilacaceae, pulse family, imperial stone the orchid family, Scrophulariaceae, Palmae and Zingiberaceae.Many-sided effect such as that saponin has is antibiotic, antiviral, anticancer, antifertility, blood sugar lowering, blood fat reducing, antiinflammatory, immunomodulating, cardiovascular system, nervous system, interrenal system and enzymatic activity all there is tangible physiologically active, the research of saponin has entered a new stage since the eighties in 20th century, a lot of important Chinese herbal medicine such as Radix Ginseng, Radix Notoginseng, Herb Gynostemmae Pentaphylli, Radix Bupleuri, Radix Polygalae, Radix Glycyrrhizae, Radix Platycodonis, the Rhizoma Anemarrhenae, Rhizoma Dioscoreae Nipponicae etc. have obtained systematic study, and dark people's discussion has been carried out in the aspects such as extraction, separation, evaluation and biological activity of various saponin.On the extraction separation method of saponin, the application of methods such as chromatography method such as reversed-phase silica gel chromatography method, gel chromatography, drop adverse current Partition Chromatography and macroporous resin, the efficient that is the saponins extraction separation is much improved, but because the molecular weight of saponin is big, polarity is big, and existing saponin technology is comparatively loaded down with trivial details, loss of effective components is bigger, be not easy to suitability for industrialized production, therefore, the extraction separation method of studying more effective and highly purified saponin component has great importance.
Summary of the invention
The object of the present invention is to provide the extracting method of the Chinese medicine saponin component that a kind of technology is reasonable more, efficient is higher.
The present invention is implemented by following technical proposals.
The extracting method of Chinese medicine saponin component of the present invention comprises the steps: in order
(1) get the Chinese medicine medical material, add solvent, extract again after solution is transferred to alkalescence, extracting solution;
(2) macroporous type alkali anion exchange column on the extracting solution, with aqueous alkali and pure water rinsing, flushing liquor discards earlier, reuse aquiferous ethanol eluting, eluent concentrates, and promptly gets saponin component.
The described solvent of step (1) is water or aquiferous ethanol; Described solution transfers to alkalescence and is adjust pH 9～14, available NaOH or KOH or Na
2CO
3Perhaps NaHCO
3Regulate pH value.
The further remove impurity of the described extracting solution of step (1), aqueous extract can be used the alcohol precipitating method remove impurity, and alcohol extract can be used the remove impurity of water precipitating method.
The preferred macroporous type weakly-basic anion of step (2) described macroporous type alkali anion exchange column D392, D380, D382, D371 exchange column, perhaps macroporous type strong alkalinity anion D201 exchange column; Aqueous alkali can be 1～3%NaOH or KOH or Na
2CO
3Described aquiferous ethanol is 40～95% ethanol.
Prepared Chinese medicine saponin component can be independent, perhaps share with other active component, the various dosage forms that are mixed and made into adjuvant such as starch, dextrin, lactose, microcrystalline Cellulose, hydroxypropyl methylcellulose, Polyethylene Glycol, magnesium stearate, micropowder silica gel, xylitol, lactose, glucose, glycine, mannitol, glycine, HP-etc. on any or more than one pharmaceuticss, for example, can be made into injection, tablet, slow releasing tablet, drop pill, granule, injectable powder, capsule, microgranule.
Compared with prior art, the extraction separation efficient height of Chinese medicine saponin component extracting method of the present invention, saponin component content height can keep higher physiologically active, and is easy to industrialized great production.
The specific embodiment
To be easier to understand the present invention with reference to the following example, and provide embodiment and be in order to illustrate the present invention, rather than in order to limit the scope of the invention.
Embodiment one
Get the Radix Bupleuri medical material, pulverizing, add water boil and extract three times and control acid-base value, is for the first time the Na2CO3 of the 6 times of water yields and the 0.7% medical material amount of medical material amount, for the second time being the Na2CO3 of the 4 times of water yields and the 0.3% medical material amount of medical material amount, is 4 times of water yields of medical material amount for the third time; The side circulated in countercurrent is extracted, and keeps respectively after boiling 1.5,1,1 hours; Medicinal liquid merges and to be chilled to room temperature, and concentrated medicament is to 2 times of volumes of medical material amount, adds ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill 24 hours, filters, and decompression filtrate recycling ethanol is dissolved in water to there not being the alcohol flavor, filters; The macroporous type weakly-basic anion D382 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 70% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Bupleuri total saponin (total saponin content 85.4%).Radix Bupleuri total saponin assay reference literature (Tianjin pharmacy, October calendar year 2001,13 (5): 60).
Embodiment two
Get the residue after the radix bupleuri extract volatile oil, add 50% alcohol reflux three times and control acid-base value, for the first time be the Na2CO3 of 5 times of 50% amount of alcohol and the 1% medical material amount of medical material amount, for the second time being the Na2CO3 of 4 times of 50% amount of alcohol and the 0.5% medical material amount of medical material amount, is 4 times of 50% amount of alcohol of medical material amount for the third time; Side circulated in countercurrent reflux, extract, kept respectively 1.5,1,1 hours after the beginning that refluxes; Medical filtration and merging filtrate, be evaporated under 70 ℃ of the filtrates do not have the alcohol flavor after, concentrated solution thin up to medical material medicinal liquid ratio is 1: 1.5, filter, the macroporous type strong alkalinity anion D201 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 85% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Bupleuri total saponin (total saponin content 71.4%).Radix Bupleuri total saponin assay reference literature (Tianjin pharmacy, October calendar year 2001,13 (5): 60).
Embodiment three
Get Radix Et Caulis Acanthopanacis Senticosi medical material (root, rhizome, stem), pulverize, add 50% alcohol reflux three times and control acid-base value, for the first time be the Na2CO3 of 5 times of 50% amount of alcohol and the 1% medical material amount of medical material amount, for the second time being the Na2CO3 of 4 times of 50% amount of alcohol and the 0.5% medical material amount of medical material amount, is 4 times of 50% amount of alcohol of medical material amount for the third time; Side circulated in countercurrent reflux, extract, kept respectively 1.5,1,1 hours after the beginning that refluxes; Medical filtration and merging filtrate, be evaporated under 70 ℃ of the filtrates do not have the alcohol flavor after, concentrated solution thin up to medical material medicinal liquid ratio is 1: 1.5, filter, the macroporous type strong alkalinity anion D201 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 85% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get manyprickle acanthopanax general saponin extractive (total saponin content 47.3%).Radix Et Caulis Acanthopanacis Senticosi total saponins assay reference literature (Chinese patent medicine, in January, 2003,25 (1): 12).
Embodiment four
Get Folium Acanthopanacis Senticosi, smashing to pieces, add water boil and extract three times and control acid-base value, is for the first time the Na2CO3 of the 6 times of water yields and the 0.7% medical material amount of medical material amount, for the second time being the Na2CO3 of the 4 times of water yields and the 0.3% medical material amount of medical material amount, is 4 times of water yields of medical material amount for the third time; The side circulated in countercurrent is extracted, and keeps respectively after boiling 1.5,1,1 hours; Medicinal liquid merges and to be chilled to room temperature, and concentrated medicament is to 2 times of volumes of medical material amount, adds ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill 24 hours, filters, and decompression filtrate recycling ethanol is dissolved in water to there not being the alcohol flavor, filters; The macroporous type weakly-basic anion D382 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 70% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get manyprickle acanthopanax general saponin extractive (total saponin content 64.6%).Radix Et Caulis Acanthopanacis Senticosi total saponins assay reference literature (Chinese patent medicine, in January, 2003,25 (1): 12).
Embodiment five
Get Milkvetch Root, pulverizing, add water supersound extraction four times and control acid-base value, is for the first time the NaHCO3 of the 5 times of water yields and the 0.9% medical material amount of medical material amount, for the second time being the NaHCO3 of the 4 times of water yields and the 0.5% medical material amount of medical material amount, is 3 times of water yields of medical material amount with the 4th time for the third time; The medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D380 exchange column of having handled well on the medicinal liquid filtrate (Chemical Plant of Nankai Univ.), with the 2.5%NaOH solution flushing of 1.5 times of resin bed volumes, flushing liquor discards; 4 times of pure water rinsing again, aqueous rinse solution discards; With 65% ethanol elution of 8 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Astragali total saponins (total saponin content 87.5%, astragaloside 71.4%).(northwest pharmaceutical journal, August calendar year 2001,16 (4): 157), Astragaloside content was measured reference literature (2005 editions one one of Chinese Pharmacopoeia, 213 pages of Astragaloside contents are measured) to Radix Astragali total saponins assay reference literature.
Embodiment six
Get Milkvetch Root, pulverize, add 70% ethanol ultrasonic extraction three times and control acid-base value, for the first time be the Na2CO3 of 5 times of 70% amount of alcohol and the 1% medical material amount of medical material amount, for the second time being the Na2CO3 of 4 times of 70% amount of alcohol and the 0.5% medical material amount of medical material amount, is 4 times of 70% amount of alcohol of medical material amount for the third time; The medicinal liquid merging is chilled to room temperature, filter, be evaporated under 70 ℃ of the filtrates do not have the alcohol flavor after, concentrated solution thin up to medical material medicinal liquid ratio is 1: 1.5, centrifugal, the macroporous type weakly-basic anion D371 exchange column of having handled well on the supernatant (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 75% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Astragali total saponins (total saponin content 95.6%, astragaloside 78.1%).(northwest pharmaceutical journal, August calendar year 2001,16 (4): 157), Astragaloside content was measured reference literature (2005 editions one one of Chinese Pharmacopoeia, 213 pages of Astragaloside contents are measured) to Radix Astragali total saponins assay reference literature.
Embodiment seven
Get the Radix Platycodonis medical material, pulverizing, add water supersound extraction four times and control acid-base value, is for the first time the NaHCO3 of the 5 times of water yields and the 0.9% medical material amount of medical material amount, for the second time being the NaHCO3 of the 4 times of water yields and the 0.5% medical material amount of medical material amount, is 3 times of water yields of medical material amount with the 4th time for the third time; The medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D380 exchange column of having handled well on the medicinal liquid filtrate (Chemical Plant of Nankai Univ.), with the 2.5%NaOH solution flushing of 1.5 times of resin bed volumes, flushing liquor discards; 4 times of pure water rinsing again, aqueous rinse solution discards; With 65% ethanol elution of 8 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Platycodi total saponins (total saponins yield 7.5%).Radix Platycodi total saponins is measured reference literature (2005 editions one one of Chinese Pharmacopoeia, 196 pages of Radix Platycodonis assays).
Embodiment eight
Get the Radix Platycodonis medical material, pulverize, add 50% alcohol reflux three times and control acid-base value, for the first time be the Na2CO3 of 5 times of 50% amount of alcohol and the 1% medical material amount of medical material amount, for the second time being the Na2CO3 of 4 times of 50% amount of alcohol and the 0.5% medical material amount of medical material amount, is 4 times of 50% amount of alcohol of medical material amount for the third time; Side circulated in countercurrent reflux, extract, kept respectively 1.5,1,1 hours after the beginning that refluxes; Medical filtration and merging filtrate, be evaporated under 70 ℃ of the filtrates do not have the alcohol flavor after, concentrated solution thin up to medical material medicinal liquid ratio is 1: 1.5, filter, the macroporous type strong alkalinity anion D201 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 85% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Platycodi total saponins (total saponins yield 5.3%).Radix Platycodi total saponins is measured reference literature (2005 editions one one of Chinese Pharmacopoeia, 196 pages of Radix Platycodonis assays).
Embodiment nine
Get medical material Radix Ophiopogonis, pulverizing, add water boil and extract three times and control acid-base value, is for the first time the Na2CO3 of the 6 times of water yields and the 0.7% medical material amount of medical material amount, for the second time being the Na2CO3 of the 4 times of water yields and the 0.3% medical material amount of medical material amount, is 4 times of water yields of medical material amount for the third time; The side circulated in countercurrent is extracted, and keeps respectively after boiling 1.5,1,1 hours; The medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D392 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 70% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Ophiopogonis total saponins (total saponin content 82.3%).Radix Ophiopogonis total saponins assay reference literature (Chinese herbal medicine, in December, 2003,34 (12): 1090).
Embodiment ten
Get medical material Radix Ophiopogonis, pulverize, add 70% ethanol ultrasonic extraction three times and control acid-base value, for the first time be the Na2CO3 of 5 times of 70% amount of alcohol and the 1% medical material amount of medical material amount, for the second time being the Na2CO3 of 4 times of 70% amount of alcohol and the 0.5% medical material amount of medical material amount, is 4 times of 70% amount of alcohol of medical material amount for the third time; The medicinal liquid merging is chilled to room temperature, filter, be evaporated under 70 ℃ of the filtrates do not have the alcohol flavor after, concentrated solution thin up to medical material medicinal liquid ratio is 1: 1.5, centrifugal, the macroporous type weakly-basic anion D371 exchange column of having handled well on the supernatant (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 75% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Ophiopogonis total saponins (total saponin content 87.9%).Radix Ophiopogonis total saponins assay reference literature (Chinese herbal medicine, in December, 2003,34 (12): 1090).
Embodiment 11
Get Folium Ginseng, smashing to pieces, add water supersound extraction four times and control acid-base value, for the first time is the NaHCO3 of the 5 times of water yields and the 0.9% medical material amount of medical material amount, for the second time being the NaHCO3 of the 4 times of water yields and the 0.5% medical material amount of medical material amount, is 3 times of water yields of medical material amount with the 4th time for the third time; The medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D380 exchange column of having handled well on the medicinal liquid filtrate (Chemical Plant of Nankai Univ.), with the 2.5%NaOH solution flushing of 1.5 times of resin bed volumes, flushing liquor discards; 4 times of pure water rinsing again, aqueous rinse solution discards; With 65% ethanol elution of 8 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Ginseng total saponins (total saponin content 87.2%).Radix Ginseng total saponins assay reference literature (Anhui Chinese Medicine College journal, in August, 2003,22 (4): 51).
Embodiment 12
Get ginseng crude drug's (root, stem), pulverizing, add water supersound extraction four times and control acid-base value, is for the first time the NaHCO3 of the 5 times of water yields and the 0.9% medical material amount of medical material amount, for the second time being the NaHCO3 of the 4 times of water yields and the 0.5% medical material amount of medical material amount, is 3 times of water yields of medical material amount with the 4th time for the third time; Medicinal liquid merges and to be chilled to room temperature, and concentrated medicament is to 2 times of volumes of medical material amount, adds ethanol and makes and contain the alcohol amount and reach 80%, leaves standstill 24 hours, filters, and decompression filtrate recycling ethanol is dissolved in water to there not being the alcohol flavor, filters; The macroporous type strong alkalinity anion D201 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2.5%NaOH solution flushing of 1.5 times of resin bed volumes, flushing liquor discards; 4 times of pure water rinsing again, aqueous rinse solution discards; With 85% ethanol elution of 8 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Ginseng total saponins (total saponin content 92.1%).Radix Ginseng total saponins assay reference literature (Anhui Chinese Medicine College journal, in August, 2003,22 (4): 51).
Embodiment 13
Get pseudo-ginseng (root, stem), pulverize, add 50% alcohol reflux three times and control acid-base value, for the first time be the Na2CO3 of 5 times of 50% amount of alcohol and the 1% medical material amount of medical material amount, for the second time being the Na2CO3 of 4 times of 50% amount of alcohol and the 0.5% medical material amount of medical material amount, is 4 times of 50% amount of alcohol of medical material amount for the third time; Side circulated in countercurrent reflux, extract, kept respectively 1.5,1,1 hours after the beginning that refluxes; Medical filtration and merging filtrate, be evaporated under 70 ℃ of the filtrates do not have the alcohol flavor after, concentrated solution thin up to medical material medicinal liquid ratio is 1: 1.5, filter, the macroporous type strong alkalinity anion D201 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 85% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Notoginseng total arasaponins (total saponin content 95.7%).Content of the total saponins in radix notoginseng is measured reference literature (Shenyang Pharmaceutical University's journal, in March, 2002,19 (2): 122).
Embodiment 14
Getting Folium Notoginseng, smash to pieces, add water boil and extract three times and control acid-base value, be for the first time the Na2CO3 of the 6 times of water yields and the 0.7% medical material amount of medical material amount, and be the Na2CO3 of the 4 times of water yields and the 0.3% medical material amount of medical material amount the second time, is 4 times of water yields of medical material amount for the third time; The side circulated in countercurrent is extracted, and keeps respectively after boiling 1.5,1,1 hours; Medicinal liquid merges and to be chilled to room temperature, and concentrated medicament is to 2 times of volumes of medical material amount, adds ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill 24 hours, filters, and decompression filtrate recycling ethanol is dissolved in water to there not being the alcohol flavor, filters; The macroporous type weakly-basic anion D382 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 70% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get Radix Notoginseng total arasaponins (total saponin content 97.7%).Content of the total saponins in radix notoginseng is measured reference literature (Shenyang Pharmaceutical University's journal, in March, 2002,19 (2): 122).
Embodiment 15
Get stem and leaf of Radix Panacis Quinquefolii, pulverizing, add water supersound extraction four times and control acid-base value, is for the first time the NaHCO3 of the 5 times of water yields and the 0.9% medical material amount of medical material amount, for the second time being the NaHCO3 of the 4 times of water yields and the 0.5% medical material amount of medical material amount, is 3 times of water yields of medical material amount with the 4th time for the third time; The medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D380 exchange column of having handled well on the medicinal liquid filtrate (Chemical Plant of Nankai Univ.), with the 2.5%NaOH solution flushing of 1.5 times of resin bed volumes, flushing liquor discards; 4 times of pure water rinsing again, aqueous rinse solution discards; With 65% ethanol elution of 8 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get American ginseng total saponins (total saponin content 93.5%).American ginseng total saponins assay reference literature (Medical University Of Tianjin's journal, in January, 2000,6 (1): 26).
Embodiment 16
Get American ginseng root, pulverize, add 50% alcohol reflux three times and control acid-base value, for the first time be the Na2CO3 of 5 times of 50% amount of alcohol and the 1% medical material amount of medical material amount, for the second time being the Na2CO3 of 4 times of 50% amount of alcohol and the 0.5% medical material amount of medical material amount, is 4 times of 50% amount of alcohol of medical material amount for the third time; Side circulated in countercurrent reflux, extract, kept respectively 1.5,1,1 hours after the beginning that refluxes; Medical filtration and merging filtrate, be evaporated under 70 ℃ of the filtrates do not have the alcohol flavor after, concentrated solution thin up to medical material medicinal liquid ratio is 1: 1.5, filter, the macroporous type strong alkalinity anion D201 exchange column of having handled well on the filtrate (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 85% ethanol elution of 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (50 ℃ of following relative densities are 1.28～1.33), with dynamic belt drying equipment drying, get American ginseng total saponins (total saponin content 95.3%).American ginseng total saponins assay reference literature (Medical University Of Tianjin's journal, in January, 2000,6 (1): 26).
Claims (5)
1. the preparation method of a Chinese medicine saponin component comprises the steps: in order
(1) get the Chinese medicine medical material, add solvent, extract again after solution is transferred to alkalescence, extracting solution;
(2) macroporous type alkali anion exchange column on the extracting solution, with aqueous alkali and pure water rinsing, flushing liquor discards earlier, reuse 40～95% ethanol elutions, eluent concentrates, and promptly gets saponin component;
It is characterized in that the solvent in the described step (1) is water or 40～95% ethanol;
Alkalescence that solution is transferred in the described step (1) is adjust pH 9～14;
Macroporous type alkali anion exchange column in the described step (2) is selected from macroporous type weakly-basic anion D392 exchange column, macroporous type weakly-basic anion D380 exchange column, macroporous type weakly-basic anion D382 exchange column, macroporous type weakly-basic anion D371 exchange column or macroporous type strong alkalinity anion D201 exchange column;
Aqueous alkali in the described step (2) is 1～3%NaOH, 1～3%KOH or 1～3%Na
2CO
3
2. preparation method according to claim 1 is characterized in that, with NaOH, KOH, Na
2CO
3Perhaps NaHCO
3The regulator solution pH value.
3. preparation method according to claim 1 is characterized in that, after described step (1) obtains extracting solution, and further remove impurity, aqueous extract alcohol precipitating method remove impurity, perhaps alcohol extract water precipitating method remove impurity.
4. preparation method according to claim 1 is characterized in that it comprises the steps: in order
(1) get the Chinese medicine medical material, add entry or 40～95% ethanol, solution is transferred to alkalescence be adjust pH 9～14, heating or supersound extraction 2～4 times, merge extractive liquid, filters; The further remove impurity of filtrate, aqueous extract alcohol precipitating method remove impurity, alcohol extract is then used the remove impurity of water precipitating method, obtains the clear liquor after the remove impurity;
(2) macroporous type weakly-basic anion D392 exchange column, macroporous type weakly-basic anion D380 exchange column, macroporous type weakly-basic anion D382 exchange column, macroporous type weakly-basic anion D371 exchange column or macroporous type strong alkalinity anion D201 exchange column on the clear liquor are earlier with 1～3%NaOH, 1～3%KOH or 1～3%Na
2CO
3Flushing, the reuse pure water rinsing, flushing liquor discards, and uses 40～95% ethanol elutions then, and eluent concentrates, and drying promptly gets saponin component.
5. the preparation method of a Chinese medicine saponin component preparation, it is characterized in that, the saponin component that the weighting profit requires 1 or 4 described methods to obtain, share separately or with other active component, make injection, tablet, drop pill, granule, injectable powder, capsule or microgranule with the adjuvant on any above pharmaceutics.
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| CN102743307A (en) * | 2011-04-22 | 2012-10-24 | 王瑞闵 | Method for purifying chinese soapberry fruit saponins element |
| KR102021764B1 (en) * | 2013-05-03 | 2019-09-18 | (주)아모레퍼시픽 | Skin external composition containing ginsenoside Rh4 |
| CN105012355A (en) * | 2015-07-08 | 2015-11-04 | 莆田学院 | Method for extracting saponin from pleurotus eryngii |
| CN107375503A (en) * | 2017-08-02 | 2017-11-24 | 瑞阳制药有限公司 | The preparation method of soapberry pericarp activity extract and its antimycotic application |
| CN109430854B (en) * | 2018-09-18 | 2021-10-26 | 广东精核生物科技发展有限公司 | Health product and preparation method thereof |
| CN110522025A (en) * | 2019-10-08 | 2019-12-03 | 大连山海物华科技开发有限公司 | A kind of loss of weight fat reducing health food and preparation method thereof |
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| CN1513461A (en) * | 2003-07-17 | 2004-07-21 | 吉林省中医中药研究院 | Feeze-dried powder injection contg. tatol saponin by refinement of American ginseng and leaves and stem of Americal ginseng, and its prodn. process |
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| CN1513461A (en) * | 2003-07-17 | 2004-07-21 | 吉林省中医中药研究院 | Feeze-dried powder injection contg. tatol saponin by refinement of American ginseng and leaves and stem of Americal ginseng, and its prodn. process |
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| 宋海妹等.柴胡皂苷的提取与鉴定.《大连轻工业学院学报》.2005,第24卷(第1期), * |
| 靳燕等.油茶皂甙提纯分离和结构鉴定方法综述.《化学世界》.2000,第41卷(第5期), * |
| 黎海彬等.植物三萜皂苷的提取分离技术.《食品工业科技》.2006,第27卷(第1期), * |
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