CN107714746A - It is a kind of to prepare the method containing 11 kinds of panaxsaponin mixtures - Google Patents
It is a kind of to prepare the method containing 11 kinds of panaxsaponin mixtures Download PDFInfo
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- CN107714746A CN107714746A CN201711191350.0A CN201711191350A CN107714746A CN 107714746 A CN107714746 A CN 107714746A CN 201711191350 A CN201711191350 A CN 201711191350A CN 107714746 A CN107714746 A CN 107714746A
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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)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
- A61K36/258—Panax (ginseng)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7028—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
- A61K31/7034—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin
- A61K31/704—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin attached to a condensed carbocyclic ring system, e.g. sennosides, thiocolchicosides, escin, daunorubicin
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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
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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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The method containing 11 kinds of panaxsaponin mixtures is prepared the invention discloses a kind of, is comprised the following steps successively:Step 1:Take ginsenoside extract to be dissolved in water, then adjust pH value to 3 ~ 6, then add double-aqueous phase system and repeatedly extracted, the upper aqueous phase being obtained by extraction every time is merged;Step 2:Upper aqueous phase after the merging is subjected to low temperature and is concentrated into inorganic solvent, overall solution is obtained after adding appropriate purified water, adds the second organic acid of the first predetermined amount, 12 ~ 24h is then incubated under 80 ~ 100 DEG C of environment, and collect water insoluble active ingredient;Step 3:The water insoluble active ingredient is produced into the mixture containing 11 kinds of ginsenosides after drying, the technology realizes the low cost preparation of high content panaxsaponin mixture, is adapted to a large amount of productions.
Description
Technical field
The present invention relates to a kind of method for preparing panaxsaponin mixture, and in particular to one kind is prepared containing ginsenoside in 11
The method of mixture.
Background technology
Ginsenoside has been unequivocally established at present has the characteristics that bioactivity is notable, pharmacological action is unique.It is separated at present
The nearly 200 kinds of ginsenoside monomers identified, are broadly divided into three classes:Protopanaxadiol-type's saponin(e, protopanaxatriol type saponin(e and
Oleanolic acid type saponin, wherein 6 kinds of main saponin(es(Rg1、Re、Rb1、Rc、Rb2、Rd)Account for more than the 90% of total saposins, and its
Saponin contents such as his Rg3, Rg5, Rh2 and its low, this part saponin(e is referred to as ginsenoside, and ginsenoside was processing
Ginseng(That is red ginseng)Content is only ten a ten thousandths, or even less, but this part saponin(e really really has and significantly improved
The composition of immunity, antitumor pharmacological activity.
Existing market and correlative study mainly using prepare the ginsenosides of monomer ginsenoside or three kinds or so a kind of as
It is main, meanwhile, preparing ginsenoside mainly has 3 kinds of approach, sour conversion method, alkali conversion method and enzyme transforming process, and mainly to prepare one
Kind monomer ginsenoside is target.Enzyme transforming process has a mild condition, the features such as orientation conversion, but exist the transformation period compared with
It is long, the shortcomings of transformation efficiency is low.Sour conversion method generally selects hydrolyst of the strong acid as ginsenoside, transformation efficiency compared with
Height, but it is non-specific conversion to be present, it is serious to equipment corrosion the defects of.Alkali conversion method is needed in high temperature(More than 200 DEG C), it is high
Cracking conversion is carried out under the conditions of pressure, the method transformation efficiency is higher, but the also requirement to industrial equipment is very high, is unfavorable for industry
The application produced greatly.
Finding a kind of high efficiency raw material of the conversion containing a variety of ginsenosides and corresponding low cost and can have real
The conversion process of border industrialized production is significantly.
The content of the invention
It is an object of the present invention to disclose it is a kind of prepare the method containing 11 kinds of panaxsaponin mixtures, the technology not only improves
Transformation efficiency, and substantially increase the content of panaxsaponin mixture, while cost reduces, and is adapted to a large amount of productions, has
Highly important innovative value.
Realizing the technical scheme of the present invention for preparing the method containing 11 kinds of panaxsaponin mixtures is:
It is a kind of to prepare the method containing 11 kinds of panaxsaponin mixtures, comprise the following steps successively:
Step 1:Ginsenoside extract is taken, the ginsenoside extract contains 11 kinds of ginsenosides, with the first preset vol
Water the ginsenoside extract is completely dissolved, the first organic acid of the solution after the ginsenoside extract will be dissolved
PH value is adjusted to 3 ~ 6, double-aqueous phase system is then added and is extracted, upper aqueous phase is collected in extraction after completing, lower aqueous phase is added again
Enter the double-aqueous phase system and repeat extraction 2 ~ 4 times, then merge the upper aqueous phase being obtained by extraction every time;
Step 2:Upper aqueous phase after the merging is subjected to low temperature and is concentrated into inorganic solvent, is added in the inorganic solvent suitable
Overall solution is obtained after the purified water of amount, the second organic acid of the first predetermined amount is added in the overall solution, then 80 ~
12 ~ 24h is incubated under 100 DEG C of environment, and collects water insoluble active ingredient;
Step 3:The water insoluble active ingredient is produced into the mixture containing 11 kinds of ginsenosides after drying.
Further, the double-aqueous phase system be ethanol-ammonium sulfate-water, polyethylene glycol-ammonium sulfate-water, polyethylene glycol-
One kind in potassium hydrogen phosphate-water, acetone-potassium hydrogen phosphate-water or isopropanol-ammonium sulfate-aqueous systems.
Further, first organic acid is one in citric acid, aspartic acid, glutamic acid, ascorbic acid or acetic acid
Kind is a variety of.
Further, second organic acid is the one or more in citric acid, ascorbic acid or acetic acid.
Further, first preset vol is multiplied by 2 ~ 5L/Kg for the quality of the ginsenoside extract.
Further, after appropriate purified water being added in the inorganic solvent so that what the overall solution contained consolidates
The scale of construction is 25 ~ 35%.
Further, first predetermined amount is the 25 ~ 35% of the quality of the ginsenoside extract.
Further, extraction is using reactor extraction or Centrifugical extraction, it is preferred that extraction uses Centrifugical extraction, centrifugation extraction
Taking has the features such as two phase materials times of contact are short, and split-phase speed is fast, and amount retained is small in a device, and operation is wide compared to scope.
Further, the low temperature concentration is concentrated or is concentrated under reduced pressure using normal pressure, it is preferred that the low temperature concentration, which uses, to be subtracted
Pressure concentration, the boiling temperature that being concentrated under reduced pressure is water is reduced with the mode vacuumized evaporate the water drying, improve thickening efficiency.
Further, the drying uses vacuum dehydrating at lower temperature or freeze-drying, it is preferred that described dry low using vacuum
Temperature is dried, and vacuum dehydrating at lower temperature has that drying effect is good, the high feature of operating efficiency.
Further, the ginsenoside extract is extract of Radix Ginseng stem and leaf, ginseng root extract or American Ginseng extraction
One or more in thing, the extract of Radix Ginseng stem and leaf, ginseng root extract and American ginseng extract contain 11 kinds of ginsengs
Saponin(e, the ginsenoside extract can be obtained by commercially available mode, can also be prepared into according to certain technique
Arrive, extract of Radix Ginseng stem and leaf can be prepared using Chinese Pharmacopoeia technique, and ginseng root extract can use ethanol extraction work
Skill binding resin purifying process is prepared, and American ginseng extract is prepared into using ethanol extraction process binding resin purifying process
Arrive.
Further, the mass content of saponin(e is 25 ~ 35% in the ginsenoside extract.
Further, ginseng sapoglycoside Rg 3 content >=20% in the mixture for containing 11 kinds of ginsenosides, ginsenoside Rg 5
>=8%, ginsenoside Rk1 >=6%, ginseng saponin Rh 2 >=4%, 3beta,6alpha,12beta-Trihydroxydammar-20(21),24-diene-6-O-beta-D-glucopyranoside, ginsenoside Rh 1, ginsenoside Rh 3, ginseng
Saponin(e Rh4, ginsenoside Rk_2, ginsenoside aPPT and ginsenoside aPPD content summation >=9%.
Beneficial effects of the present invention are:
(1)The present invention is according to the design feature of ginsenoside composition, using two phase aqueous extraction system by protopanoxadiol constituents
Enriching and purifying is carried out, and catalyzing hydrolysis is carried out using weak acid and prepares ginsenoside, there is the characteristics of simple to operate and cost is cheap,
Preparation of industrialization panaxsaponin mixture preferably, at the same overcome strong acid hydrolysis and strong base catalyst hydrolysis needed for reaction environment will
Seek the high and high difficulty of equipment requirement.
(2)Transformation efficiency of the present invention is high, and it is used for the preparation of panaxsaponin mixture, and the molar yield of wherein saponin(e is
80-90%。
(3)The panaxsaponin mixture prepared by the inventive method, containing 11 kinds of ginsenosides, and content is higher, tool
The composition of immunity and antitumor action is improved, 11 kinds of composition collaborations play a role, and have the characteristics of better efficacy.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1:
50g extract of Radix Ginseng stem and leaf samples are weighed, are completely dissolved with 200ml water, add citric acid regulating solution pH to 4.0,
Polyethylene glycol-ammonium sulfate-water double aqueous phase system is added, is extracted, aqueous phase in collection, lower aqueous phase is repeated to extract by above-mentioned steps again
Take 2 times, a coextraction 3 times, aqueous phase in merging, the upper aqueous phase of merging is carried out into low temperature is concentrated into inorganic solvent, and moisturizing is extremely
100ml, add 15g citric acids, stirring, make to be completely dissolved, 20h be incubated under 90 DEG C of environment, after terminating collect water-insoluble into
Point, dried during water insoluble active ingredient is dried in vacuo, produce the mixture containing 11 kinds of ginsenosides, ginseng sapoglycoside Rg 3 contains
Amount >=21.3%, ginsenoside Rg 5 >=9.10%, ginsenoside Rk1 >=6.24%, ginseng saponin Rh 2 >=4.67%, other pole ginsengs
Saponin(e(Rk3、Rh1、Rh3、Rh4、Rk2、aPPT、aPPD)Content summation >=10.38%.
Embodiment 2:
50g extract of Radix Ginseng stem and leaf samples are weighed, are completely dissolved with 200ml water, addition glutamic acid regulation pH value of solution to 3.5,
Acetone-potassium hydrogen phosphate-water double aqueous phase system is added, is extracted, aqueous phase in collection, lower aqueous phase is repeated to extract by above-mentioned steps again
3 times, a coextraction 4 times, aqueous phase in merging, upper aqueous phase progress low temperature is concentrated into inorganic solvent, moisturizing to 100ml, adds 15g
Ascorbic acid, stirring, makes to be completely dissolved, 16h is incubated under 95 DEG C of environment, water insoluble active ingredient is collected after terminating, and water is insoluble
Property composition be dried in vacuo in dry, produce the mixture containing 11 kinds of ginsenosides, ginseng sapoglycoside Rg 3 content >=20.68%,
Ginsenoside Rg 5 >=9.52%, ginsenoside Rk1 >=6.18%, ginseng saponin Rh 2 >=4.29%, other pole ginsenosides(Rk3、
Rh1、Rh3、Rh4、Rk2、aPPT、aPPD)Content summation >=9.78%.
Embodiment 3:
100g American ginseng extract samples are weighed, are completely dissolved with 500ml water, add citric acid regulating solution pH to 3.5, are added
Isopropanol-ammonium sulfate-water double aqueous phase system, is extracted, aqueous phase in collection, and lower aqueous phase repeats extraction 3 times by above-mentioned steps again,
One coextraction 4 times, aqueous phase in merging, upper aqueous phase progress low temperature is concentrated into inorganic solvent, moisturizing to 250ml, adds 35g ice second
Acid, stirring, makes to be completely dissolved, 24h is incubated under 85 DEG C of environment, water insoluble active ingredient is collected after terminating, by water insoluble active ingredient
Dried in being dried in vacuo, produce the mixture containing 11 kinds of ginsenosides, ginseng sapoglycoside Rg 3 content >=22.43%, ginseng soap
Glycosides Rg5 >=10.42%, ginsenoside Rk1 >=6.83%, ginseng saponin Rh 2 >=6.78%, other pole ginsenosides(Rk3、Rh1、
Rh3、Rh4、Rk2、aPPT、aPPD)Content summation >=9.01%.
Embodiment 4:
100g ginseng root extract samples are weighed, are completely dissolved with 500ml water, acetic acid is added and adjusts pH value of solution to 3.0, add
Ethanol-ammonium sulfate-water double aqueous phase system, is extracted, aqueous phase in collection, lower aqueous phase again by above-mentioned steps repeat extraction 3 times, one
Coextraction 3 times, aqueous phase in merging, upper aqueous phase progress low temperature is concentrated into inorganic solvent, moisturizing to 250ml, adds 35g ice second
Acid, stirring, makes to be completely dissolved, 20h is incubated under 100 DEG C of environment, water insoluble active ingredient is collected after terminating, by water insoluble active ingredient
Dried in being dried in vacuo, produce the mixture containing 11 kinds of ginsenosides, ginseng sapoglycoside Rg 3 content >=21.83%, ginseng soap
Glycosides Rg5 >=11.04%, ginsenoside Rk1 >=6.31%, ginseng saponin Rh 2 >=6.09%, other pole ginsenosides(Rk3、Rh1、
Rh3、Rh4、Rk2、aPPT、aPPD)Content summation >=9.89%.
Embodiment 1, embodiment 2, embodiment 3 and embodiment 4 using two phase aqueous extraction system by protopanoxadiol class into
Divide and carry out enriching and purifying, and catalyzing hydrolysis is carried out using weak acid and prepares ginsenoside, the wherein molar yield of saponin(e is 80-
90%, there is the characteristics of simple to operate and cost is cheap, preparation of industrialization panaxsaponin mixture preferably, while overcome strong
Reaction environment needed for sour water solution and strong base catalyst hydrolysis requires the high and high difficulty of equipment requirement.
Claims (10)
1. a kind of prepare the method containing 11 kinds of panaxsaponin mixtures, it is characterised in that comprises the following steps successively:
Step 1:Ginsenoside extract is taken, the ginsenoside extract contains 11 kinds of ginsenosides, with the first preset vol
Water the ginsenoside extract is completely dissolved, the first organic acid of the solution after the ginsenoside extract will be dissolved
PH value is adjusted to 3 ~ 6, double-aqueous phase system is then added and is extracted, upper aqueous phase is collected in extraction after completing, lower aqueous phase is added again
Enter the double-aqueous phase system and repeat extraction 2 ~ 4 times, then merge the upper aqueous phase being obtained by extraction every time;
Step 2:Upper aqueous phase after the merging is subjected to low temperature and is concentrated into inorganic solvent, is added in the inorganic solvent suitable
Overall solution is obtained after the purified water of amount, the second organic acid of the first predetermined amount is added in the overall solution, then 80 ~
12 ~ 24h is incubated under 100 DEG C of environment, and collects water insoluble active ingredient;
Step 3:The water insoluble active ingredient is produced into the mixture containing 11 kinds of ginsenosides after drying.
2. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that the aqueous two-phase body
Be for ethanol-ammonium sulfate-water, polyethylene glycol-ammonium sulfate-water, polyethylene glycol-phosphorus potassium hydrogen phthalate-water, acetone-potassium hydrogen phosphate-water or
One kind in isopropanol-ammonium sulfate-aqueous systems.
3. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that described first is organic
Acid is the one or more in citric acid, aspartic acid, glutamic acid, ascorbic acid or acetic acid.
4. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that described second is organic
Acid is the one or more in citric acid, ascorbic acid or acetic acid.
5. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that described first is default
Volume is multiplied by 2 ~ 5L/Kg for the quality of the ginsenoside extract.
6. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that described inorganic molten
After appropriate purified water is added in agent so that the amount of solid that the overall solution contains is 25 ~ 35%.
7. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that described first is default
Measure 25 ~ 35% of the quality for the ginsenoside extract.
8. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that the ginsenoside
Extract is the one or more in extract of Radix Ginseng stem and leaf, ginseng root extract or American ginseng extract.
9. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that the ginsenoside
The mass content of saponin(e is 25-35% in extract.
10. the method containing 11 kinds of panaxsaponin mixtures is prepared according to claim 1, it is characterised in that described to contain 11 kinds
Ginseng sapoglycoside Rg 3 content >=20% in the mixture of ginsenoside, ginsenoside Rg 5 >=8%, ginsenoside Rk1 >=6%, ginseng soap
Glycosides Rh2 >=4%, 3beta,6alpha,12beta-Trihydroxydammar-20(21),24-diene-6-O-beta-D-glucopyranoside, ginsenoside Rh 1, ginsenoside Rh 3, Ginsenoside Rh4, ginsenoside Rk_2, ginseng soap
Glycosides aPPT and ginsenoside aPPD content summation >=9%.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109369744A (en) * | 2018-10-11 | 2019-02-22 | 浙江大学自贡创新中心 | A kind of method of sapindoside in aqueous two-phase extraction soapberry |
CN111018939A (en) * | 2019-12-16 | 2020-04-17 | 中国科学院青岛生物能源与过程研究所 | Rapid refining method of tea saponin |
CN112125947A (en) * | 2020-08-17 | 2020-12-25 | 赣州禾绿康健生物技术有限公司 | Method and equipment for removing plasticizer from ginsenoside extract |
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CN102133298A (en) * | 2010-12-03 | 2011-07-27 | 沈阳药科大学 | Two-aqueous-phase method for extracting total saponin from bittersweet herb |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109369744A (en) * | 2018-10-11 | 2019-02-22 | 浙江大学自贡创新中心 | A kind of method of sapindoside in aqueous two-phase extraction soapberry |
CN111018939A (en) * | 2019-12-16 | 2020-04-17 | 中国科学院青岛生物能源与过程研究所 | Rapid refining method of tea saponin |
CN112125947A (en) * | 2020-08-17 | 2020-12-25 | 赣州禾绿康健生物技术有限公司 | Method and equipment for removing plasticizer from ginsenoside extract |
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