CN104435060B - A kind of method that gynosaponin is extracted from gynostemma pentaphylla - Google Patents
A kind of method that gynosaponin is extracted from gynostemma pentaphylla Download PDFInfo
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- CN104435060B CN104435060B CN201410620033.6A CN201410620033A CN104435060B CN 104435060 B CN104435060 B CN 104435060B CN 201410620033 A CN201410620033 A CN 201410620033A CN 104435060 B CN104435060 B CN 104435060B
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- gynosaponin
- gynostemma pentaphylla
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/42—Cucurbitaceae (Cucumber family)
- A61K36/424—Gynostemma
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The invention discloses a kind of method that gynosaponin is extracted from gynostemma pentaphylla, comprise the steps:Feedstock treating, high pressure extraction, aqueous two-phase extraction, desalination, concentrate drying, obtain gynosaponin.High with content, recovery rate is high, and technique is simple, is adapted to produce, the advantages such as production cost is low.
Description
Technical field
It is specifically a kind of that gynosaponin is extracted from gynostemma pentaphylla the present invention relates to the extracting method of biological technical field
Method.
Background technology
Gynostemma pentaphylla, it is perennial herbaceous stem rattan wood, also known as paradise grass, Gospel grass, Chao Rencan, public arched bottom, Herba Gynostemmatis, seven
Leaf courage, Pentapanax leschenaultii and gynostemma pentaphyllum makino etc., Japan are referred to as sweet climing tea, are Curcurbitaceae gynostemma pentaphyllum genus herbaceous perennial vine plant.Strand
Indigo plant likes dark and damp gentle weather, how wild at the concealments such as sylvan life, brook bank, perennial to climb up by holding on to draft.In Chinese main distribution
In Shaanxi, flat interest, Structure, Hunan, Hubei, Yunnan, Guangxi etc. save, and are known as " south ginseng ", are grown in southern gynostemma pentaphylla
Medicinal comparision contents are high, " the elixir grass " among the people for being called mystery, 1986, State Scientific and Technological Commission in Spark Program,
Gynostemma pentaphylla is classified as the first place of " rare traditional Chinese medicine " leaved for development, on March 5th, 2002, health ministry was included in the health care name of an article
It is single.Result of study show gynostemma pentaphylla contain gynosaponin, carbohydrate, flavonoids, amino acid, protein, fat, inorganic elements,
Cellulose and vitamin.Wherein former three is main health-care efficacy composition, and other still have polysaccharide, flavonoids, amino acid, dimension
Raw element and zinc, copper, iron, manganese etc..Gynosaponin is the active ingredient that gynostemma pentaphyllum herb contains, and modern pharmacology research proves to twist
The blue saponin of stock have reduce blood fat, hypotensive, prevent aging, suppress tumour, strengthen immunity, sedation-analgesia, cardioprotection and
The effects such as liver, antiatherosclerosis, protection blood vessel, and have no toxic side effect.The active ingredient saponin of gynostemma pentaphylla is eaten in health care
There is huge application prospect in product and novel medicine research and development, there is greatly research and value, in states such as Japan, will twist
Saponin during stock is basket individually extracts that plurality kinds of health care product are made and are sold turns into a kind of trend.In field of medicaments, will twist
Gynosaponin granule medicament is made with dextrin, lactose in the blue saponin of stock, can be used in the treatment of hyperlipemia, gynosaponin
Grain formulation advantage be:Fast, effective rapid, easy to carry, steady quality etc. is absorbed, as Chinese medicine preparation, has poison is secondary to make again
With small, lasting medicine, treat both principal and secondary aspect of disease the features such as.
The extracting method of gynosaponin has water extraction, organic solvent extraction, microwave―assisted extraction, ultrasonic wave at present
The methods of assisted extraction method, Enzymatic Extraction, above method typically all can be after extraction using macroporous resin purification as main
Separating step, but macroporous resin purification method is used, for resin with before needing to handle, purifying need to pass through absorption and elution process,
Production cycle is grown.When carrying out purifying elution with macroreticular resin, due to physical absorption, a part of sample is also easily caused
Dead absorption, and cause the rate of transform to reduce.It is larger using macroporous resin purification effluent volume in addition, solvent recovery time length, increase
Production cost is added, and solvent recovery produces more waste liquid, and certain burden is caused to environmental protection.Additionally due to macroreticular resin
Use, add and introduce benzene,toluene,xylene, styrene, alkanes, the risk of the organic residual solvent such as diethylbenzene class,
The security of product is exerted a certain influence.
In summary, the extracting method for studying the small gynosaponin of a kind of simple possible, environmental pollution has very well
Realistic meaning.
The content of the invention
It is an object of the invention to provide a kind of method that gynosaponin is extracted from gynostemma pentaphylla, has technique simple, fits
The advantages that symphysis is produced, and the time is short.
The present invention is achieved through the following technical solutions, and is specifically comprised the following steps：
1) Feedstock treating：Gynostemma pentaphylla is crushed or smashed；
2) high pressure extraction：The raw material after processing is put into pressure pan, adds the pure water of identical weight, added suitable
In raw material weight 0.05-0.25% organic silicon modified by polyether, 4kgf/cm is forced into2, make its pressure uniform, and keep 10-
15min, recover normal pressure, filtering, obtain extract solution；
3) separate：Gynostemma pentaphyllum Makino carries out aqueous two-phase extraction, obtains the upper phase of extraction and the lower phase of extraction, and aqueous two-phase extraction is used
Double-aqueous phase system be made up of polyethylene glycol, sodium hydroxide and water, quality percentage of the polyethylene glycol in the double-aqueous phase system
Than being 10-15% for 15-25%, mass percent of the sodium hydroxide in the double-aqueous phase system, surplus is water, the poly- second
The weight average molecular weight of glycol is 1000-8000；
4) subsequent treatment：Phase in the extraction that step 3) is obtained, desalination, concentrate drying, under the extraction that step 3) is obtained
Phase, add equivalent to the lower phase mass percent 5-10% sodium hydroxides of extraction, desalination, concentrate drying；
5) merge dried acquisition thing and obtain gynosaponin.
Gynostemma pentaphylla of the present invention is fresh and/or dried gynostemma pentaphylla.
Described desalination preferably uses ultrafiltration or dialysis, and ultrafiltration uses molecular cut off as 1000-100000's
Milipore filter desalination, dialysis use bag filter desalination of the molecular cut off for 1000-100000.
Described drying preferably spray drying or freeze-drying.
The gynosaponin that the present invention obtains, is detected through HPLC, and content is more than 98.5%.
Compared with prior art, advantages of the present invention：
1st, prior art is prepared in the method for gynosaponin using water extraction, because gynostemma pentaphylla active ingredient saponin in itself
With certain emulsification, foam can be produced, therefore excessive foam can be produced in extraction process, caused foam is on the one hand
It can be attached on medicinal raw material particle, and then have impact on being fully dissolved out for the effective-part of Gynostemma pentaphyllum, cause extraction time to extend, carry
The dosage of solvent is taken to increase；Another aspect foam can be also attached on extraction equipment, make extract solution coking, denaturation, and then influence
Drug effect.
Organic silicon modified by polyether, it is that polyether siloxane copolymers (letter made from polyether segment is added in siloxane molecule
Claim silicon ether copolymer).Polysiloxane-based defoamer has the features such as defoaming is rapid, and the suds time is grown and is safe and non-toxic, but it is difficult
Water is dissolved in, high temperature resistant, strong basicity resisting is poor, and polyethers defoamer good water solubility, high temperature resistant, strong basicity resisting is strong, but its antifoaming speed
It is all not satisfactory with the suds time, and organic silicon modified by polyether combines the advantages of polyethers is with both organic silicon defoamers, has
Nontoxic, harmless to strain, addition is few, is a kind of product of high performance-price ratio, and poly- silica is grafted on by condensation technology
Polyether chain is introduced on alkane chain, the advantages of with two class defoamers, turns into a kind of function admirable, what is had wide application prospects disappears
Infusion.In the molecule of silicon ether copolymer, siloxanes section is lipophilic group, and polyethers section is hydrophilic group.Polycyclic oxygen second in polyether segment
Alkane chain energy-conservation provides hydrophily and foaming characteristic, and PPOX chain energy-conservation provides hydrophobicity and penetration, to reducing surface tension
Play the role of stronger.Organic silicon modified by polyether is added in extraction, foam can be effectively eliminated, improve the clarity of extract solution,
Increase the dissolution rate of saponin so that impurity separation is more thorough, is more beneficial for subsequent handling operation.
2nd, prior art carry out gynosaponin extraction when, pre-treatment be typically all with water or ethanol etc. for solvent,
By heating extraction by active ingredient dissolution, and the present invention uses high pressure extraction, compared to heating extraction, is acted on by high pressure,
The compositions such as the organic acid contained in gynostemma pentaphylla, polyphenol, gynosaponin are fully dissolved out, beneficial to the processing of subsequent technique,
Beneficial to the yield for improving active component.
3rd, belong to gynostemma pentaphyllum total saponin to there are about more than 80 planting altogether, wherein 78 kinds are respectively designated as the-LXXV III of gypenoside I,
Wherein some is respectively ginsenoside Rb1, Rb3, Rd, and panoxadiol, 2 Alpha-hydroxy panoxadiols, 2 α, 19- dihydroxies
Base -12- deoxidation panoxadiols etc., the present invention passes through aqueous two-phase extraction so that the saponin of different structure is in different extraction phases
Distribution, add the dissolution rate of saponin.
4th, the gynosaponin content that prior art obtains is usually no more than 98%, and the present invention uses high pressure extraction and Shuan Shui
The combination of phase abstraction technique, production efficiency can be greatly improved, the resin used in prior art column chromatography is generally non-pole
Property resin, gynosaponin content 40-50% extract is can only obtain by once adsorbing；If using polar resin, warp
Cross once to adsorb and also can only obtain gynosaponin content 50% or so, wanting to obtain the gynosaponin of higher amount must lead to
2 times or more Adsorptions are crossed, so as to add process time and cost.Aqueous two phase extraction technique is as a kind of new
Isolation technics, have mild condition, it is easy to operate, be easy to the series of advantages such as amplification, separating capacity be strong, and use the present invention's
Technology combines, and the raising of matter occurs, can increase the content and extraction efficiency of gynosaponin, compared to water extraction or alcohol extracting rear pillar layer
Analysis, the time of the invention is short, and gynosaponin content is high.
5th, it is more environmentally-friendly present invention, avoiding the use of a large amount of organic solvents such as absolute ethyl alcohol, methanol.
Embodiment
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1：
A kind of method that gynosaponin is extracted from gynostemma pentaphylla, specifically comprises the following steps：
1) Feedstock treating：New fresh gynostemma pentaphylla is smashed；
2) high pressure extraction：The raw material after processing is put into pressure pan, adds the pure water of identical weight, added suitable
In the organic silicon modified by polyether of raw material weight 0.25%, 4kgf/cm is forced into2, make its pressure uniform, and 10min is kept, recover
Normal pressure, filtering, obtains extract solution；
3) separate：Gynostemma pentaphyllum Makino carries out aqueous two-phase extraction, obtains the upper phase of extraction and the lower phase of extraction, and aqueous two-phase extraction is used
Double-aqueous phase system be made up of polyethylene glycol, sodium hydroxide and water, quality percentage of the polyethylene glycol in the double-aqueous phase system
Than for 20%, mass percent of the sodium hydroxide in the double-aqueous phase system is 10%, and surplus is water, and the weight of polyethylene glycol is equal
Molecular weight is 1000-8000；
4) subsequent treatment：Phase in the extraction that step 3) is obtained, ultrafiltration use molecular cut off as 1000-100000's
Milipore filter desalination, concentration, spray drying, phase under the extraction that step 3) is obtained, add equivalent to the lower phase mass percent of extraction
10% sodium hydroxide, ultrafiltration use milipore filter desalination, concentration, spray drying of the molecular cut off for 1000-100000；
5) merge dried acquisition thing and obtain gynosaponin.
Embodiment 2：
A kind of method that gynosaponin is extracted from gynostemma pentaphylla, specifically comprises the following steps：
1) Feedstock treating：Gynostemma pentaphylla will be dried to crush；
2) high pressure extraction：The raw material after processing is put into pressure pan, adds the pure water of identical weight, added suitable
In the organic silicon modified by polyether of raw material weight 0.05%, 4kgf/cm is forced into2, make its pressure uniform, and 15min is kept, recover
Normal pressure, filtering, obtains extract solution；
3) separate：Gynostemma pentaphyllum Makino carries out aqueous two-phase extraction, obtains the upper phase of extraction and the lower phase of extraction, and aqueous two-phase extraction is used
Double-aqueous phase system be made up of polyethylene glycol, sodium hydroxide and water, quality percentage of the polyethylene glycol in the double-aqueous phase system
Than for 15%, mass percent of the sodium hydroxide in the double-aqueous phase system is 15%, and surplus is water, and the weight of polyethylene glycol is equal
Molecular weight is 1000-8000；
4) subsequent treatment：Phase in the extraction that step 3) is obtained, dialysis use molecular cut off as 1000-100000's
Bag filter desalination, concentration, freeze-drying, phase under the extraction that step 3) is obtained, add equivalent to the lower phase mass percent of extraction
5% sodium hydroxide, dialysis use bag filter desalination, concentration, freeze-drying of the molecular cut off for 1000-100000；
5) merge dried acquisition thing and obtain gynosaponin.
Embodiment 3：
A kind of method that gynosaponin is extracted from gynostemma pentaphylla, specifically comprises the following steps：
1) Feedstock treating：Gynostemma pentaphylla will be dried to crush；
2) high pressure extraction：The raw material after processing is put into pressure pan, adds the pure water of identical weight, added suitable
In the organic silicon modified by polyether of raw material weight 0.15%, 4kgf/cm is forced into2, make its pressure uniform, and 12min is kept, recover
Normal pressure, filtering, obtains extract solution；
3) separate：Gynostemma pentaphyllum Makino carries out aqueous two-phase extraction, obtains the upper phase of extraction and the lower phase of extraction, and aqueous two-phase extraction is used
Double-aqueous phase system be made up of polyethylene glycol, sodium hydroxide and water, quality percentage of the polyethylene glycol in the double-aqueous phase system
Than for 25%, mass percent of the sodium hydroxide in the double-aqueous phase system is 12%, and surplus is water, and the weight of polyethylene glycol is equal
Molecular weight is 1000-8000；
4) subsequent treatment：Phase in the extraction that step 3) is obtained, ultrafiltration use molecular cut off as 1000-100000's
Milipore filter desalination, concentration, freeze-drying, phase under the extraction that step 3) is obtained, add equivalent to the lower phase mass percent of extraction
10% sodium hydroxide, ultrafiltration use milipore filter desalination, concentration, freeze-drying of the molecular cut off for 1000-100000；
5) merge dried acquisition thing and obtain gynosaponin.
As a result：
Claims (2)
- A kind of 1. method that gynosaponin is extracted from gynostemma pentaphylla, it is characterised in that：Comprise the following steps：1) Feedstock treating：Gynostemma pentaphylla is crushed or smashed；2) high pressure extraction：The raw material after processing is put into pressure pan, adds the pure water of identical weight, add equivalent to original Expect weight 0.05-0.25% organic silicon modified by polyether, be forced into 4kgf/cm2, make its pressure uniform, and 10-15min is kept, Recover normal pressure, filtering, obtain extract solution；3) separate：Extract solution is obtained to step 2) and carries out aqueous two-phase extraction, obtains the upper phase of extraction and the lower phase of extraction, aqueous two-phase extraction Used double-aqueous phase system is made up of polyethylene glycol, sodium hydroxide and water, matter of the polyethylene glycol in the double-aqueous phase system Amount percentage is 15-25%, and mass percent of the sodium hydroxide in the double-aqueous phase system is 10-15%, and surplus is water, institute The weight average molecular weight for stating polyethylene glycol is 1000-8000；4) subsequent treatment：Phase in the extraction that step 3) is obtained, desalination, concentrate drying, phase under the extraction that step 3) is obtained, add Enter equivalent to the lower phase mass percent 5-10% sodium hydroxides of extraction, desalination, concentrate drying；5) merge dried acquisition thing and obtain gynosaponin.
- A kind of 2. method that gynosaponin is extracted from gynostemma pentaphylla according to claim 1, it is characterised in that：Described Gynostemma pentaphylla is fresh and/or dried gynostemma pentaphylla.
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| CN102232977A (en) * | 2011-05-06 | 2011-11-09 | 南京泽朗医药科技有限公司 | Method for extracting total saponins from pokeberry root |
| CN102366518A (en) * | 2011-10-17 | 2012-03-07 | 西北农林科技大学 | Method for ultrasonic assisted aqueous two-phase extraction of total dioscin |
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