CN107970265A - A kind of method for extracting Folium Notoginseng glycoside - Google Patents
A kind of method for extracting Folium Notoginseng glycoside Download PDFInfo
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- CN107970265A CN107970265A CN201711460348.9A CN201711460348A CN107970265A CN 107970265 A CN107970265 A CN 107970265A CN 201711460348 A CN201711460348 A CN 201711460348A CN 107970265 A CN107970265 A CN 107970265A
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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
- 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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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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 invention discloses a kind of method for extracting Folium Notoginseng glycoside, this method is using the dry notoginseng haulm of common salt aqueous solution immersion, then through extraction, decolorization, recrystallization and etc., obtain the few Folium Notoginseng glycoside product of impurity content, the method of the present invention cleaning, cost is low, easy to operate, with short production cycle, pigment is few, extract yield is high, suitable for industrialized production and marketing application.
Description
Technical field
The present invention relates to a kind of industrialized preparing process that Folium Notoginseng glycoside is extracted from dry notoginseng haulm.
Background technology
Pseudo-ginseng also known as pseudo-ginseng, the famous pharmacy man Li Shizhen (1518-1593 A.D.) of the Ming Dynasty are called " invaluable ".The application of pseudo-ginseng has long
History.In 1578 Christian eras, Li Shizhen (1518-1593 A.D.) is in its immortal monumental work《Compendium of Materia Medica》In recorded pseudo-ginseng " this medicine begin when near, southern people
Key medicine is created with for gold in army, cloud has outstanding service ";" be the medicine of yangming syncope the moon blood system, therefore all blood disease can be controlled ".As traumatic injury,
Specific medicament promoting blood circulation and removing blood stasis is known far and wide in through the country.In addition to treating the special efficacy of traumatic injury, pseudo-ginseng, which also has, to be nourished by force
Strong effect.Modern pharmacology research shows that pseudo-ginseng has hyperlipidemia, hypercoagulable blood, hypertension, arrhythmia cordis etc. obvious
Preventive and therapeutic action.
Pseudo-ginseng aerial part principle active component sanchi leaf total saposins are that " Folium Notoginseng glycoside " main pharmacological has calm peace
God, analgesia, lipid-loweringing etc..Central nervous system has remarkable effect, and can resist excited caused by central stimulant caffeine
Effect.Folium Notoginseng glycoside can be supplied by improving cerebrum blood, and nutrition and adjusting nerve, make every regulatory function of nervous system extensive
It is multiple to coordinate, so as to recover physiological sleep to treat neurasthenia, moreover it is possible to strengthen corticocerebral inhibitory action, and make under cortex
The excitability of rise reduces and rises and support angst resistance effect, available for treating generalized anxiety disorder.Folium Notoginseng glycoside is fallen asleep to shortening
Time, extends the length of one's sleep, reduces awakening number, improves headache, dizziness, palpitaition, weak all preferable.
The effect of reducing blood lipid:Folium Notoginseng glycoside can significantly reduce the content of serum total cholesterol and serum triglyceride, this
Effect is related with panoxadiol type saponin component contained therein.It is reported that early in nineteen eighty-three, just there has been scholar in China to three
Seven cauline leaf glucosides carried out research, and saponin(e of the document report in Folium Notoginseng glycoside at that time has following several:Ginsenoside Rb1,
Rb3, Re, 20 (R)-ginsenoside-Rg3,20 (R)-ginsenoside-Rh2s etc., gypenoside Ⅸ and notoginsenoside Fa, Fc, Fe
Totally seven kinds.
With the development of social progress and science and technology, people are higher and higher to living standard requirement, Folium Notoginseng glycoside
Development and utilization is also increasingly taken seriously, and has preferable utility value in health products and pharmaceutical industry.Before higher market
Scape.
At present, the method for extracting Folium Notoginseng glycoside is very much, and due to being influenced by traditional handicraft, it is multiple that these methods have operation
Miscellaneous, the shortcomings of input cost is high, accessory substance is more, shade deviation, it is unfavorable for industrialized production.
There are the following problems in the method prior art or conventional method of extracting Folium Notoginseng glycoside from dry notoginseng haulm:
(1)At present, column, solvent extraction such as methanol, second were carried with water more than the method for extraction Folium Notoginseng glycoside from dry notoginseng haulm
Alcohol or methanol-water, ethanol water are Extraction solvent;Due to the property of these solvent polarities, the various impurity of Folium Notoginseng glycoside are extracted together
Out, difficulty is increased to follow-up column chromatography, and impurity cannot be controlled effectively;Product quality is reduced, increase is extracted into
This;
(2)In the extracting method of most of document patent reports, need to carry out necessary column chromatography processing after the completion of extraction, to life
Produce for enterprise, column chromatography adds production cycle and production cost;In industrial production, when adding industrialized production into
This control.
The content of the invention
It is an object of the invention to provide a kind of method for extracting Folium Notoginseng glycoside, this method cleaning, cheap, extraction bar
Part is not harsh, accessory substance is less, pigment is few, extract yield is higher, and method is simply controllable, with short production cycle, is adapted to industry metaplasia
Produce Folium Notoginseng glycoside.
The purpose of the present invention is achieved through the following technical solutions:
(1)Using dry notoginseng haulm as raw material, immersion raw material, filtering are heated with common salt aqueous solution, filter residue adds common salt aqueous solution,
Soak 1~2 time repeatedly, merging filtrate, extraction is stirred to filtrate with petroleum ether, stratification, water is mutually mutually overlapping with petroleum ether
Extract 1 time again, collect water phase;
(2)Above-mentioned water is mutually extracted with n-butanol-isopropanol mixed liquor, continuous extraction 2~3 times, collects and merge organic phase,
Concentration organic phase obtains Folium Notoginseng glycoside crude product, and total saponin content is more than 45% in Folium Notoginseng glycoside;
(3)Folium Notoginseng glycoside crude product methanol-acetone mixed liquor is dissolved by heating, is subsequently cooled to -5~-10 DEG C, standing sedimentation
12-24h, filtering, adds decolorising agent in filtrate, is placed at 40~45 DEG C and carries out decolorization, filter, and filtrate revolving is drained yellow
Color crystal Folium Notoginseng glycoside.
The step(1)In at 50~60 DEG C soak 4~6h;The mass concentration of salt in water is in common salt aqueous solution
5~8%.
The n-butanol-isopropanol mixed liquor is n-butanol and isopropanol by volume 4~6:1 ratio is mixed to prepare.
The methanol-acetone mixed liquor is methanol and acetone by volume 3~5:1 ratio is mixed to prepare.
The step(3)Middle heating-up temperature is 50~60 DEG C.
The decolorising agent is activated carbon and neutral alumina, and the mass ratio of activated carbon and neutral alumina is 2~3:1, three
The mass ratio of aesculin crude product and decolorising agent is 4~6:1.
Advantage of the present invention and technique effect:
(1)Contain the material such as substantial amounts of arasaponin and panaxoside, polysaccharide, lipid, chlorophyll in notoginseng haulm;The present invention
The characteristics of having been dissolved in water using arasaponin;Notoginseng haulm is soaked using water as primary solvent;It is to incite somebody to action to add salt
Cell in notoginseng haulm forms hyperosmosis, realizes the rapid extraction of active ingredient;
(2)The solution of immersion adds petroleum ether extraction, and more than 90% lipid and pigment are extracted out, and active ingredient is difficult
It is dissolved in petroleum ether, this extraction reaches preliminary separating-purifying effect;
(3)Extracted using n-butanol-isopropanol mixed liquor, various arasaponins and panaxoside extraction are separated;
The crude product of Folium Notoginseng glycoside is obtained after concentration, various active ingredient total contents are more than 45%;
(4)After crude product methanol and acetone mixture dissolving, cooling-sedimentation, separates out a large amount of polysaccharide and partial impurities, filtrate warp
The decolorization of activated carbon and neutral alumina is crossed, obtains the Folium Notoginseng glycoside that active ingredient total content is more than 80%.
Embodiment
The present invention is described in further detail below by embodiment, but the scope of the present invention is not limited in described
Hold.
Embodiment 1:The method of this extraction Folium Notoginseng glycoside carries out according to the following steps:
(1)The drying sanchi leaf that 5kg is cut into 1-2cm segments is added in 50L pots, adds 40L common salt aqueous solutions(Salt is in water
Mass concentration be 5%)When heating immersion 4 is small under the conditions of 60 DEG C, filtering, filter residue adds the salt of the mass concentration 5% of 35L
When aqueous solution heating immersion 5 is small, filtering;Filter residue adds the common salt aqueous solution 35L of mass concentration 5%, when heating immersion 6 is small, mistake
Filter, merges filtrate 105L three times;
(2)The extraction processing of salt infusion and the preparation of Folium Notoginseng glycoside crude product
Above-mentioned 105L filtrates are added in extractor, adding petroleum ether 21L, (petroleum ether dosage is five points of filtrate totality accumulated amount
One of) stirring extraction, stratification, water is mutually with petroleum ether mutually repeatedly extraction 1 time, collection water phase;Petroleum ether layer is separated to concentrate back
Receive petroleum ether;Water is mutually placed in extractor, adding n-butanol-isopropanol mixed liquor 30L, (n-butanol is with isopropanol volume ratio
4:1), continuous extraction 2 times, collect and merge organic phase 55L, and water layer is discharged into cesspool;Organic phase is concentrated at decompression, 75 DEG C and drained
Obtain 1015g Folium Notoginseng glycoside crude products, total saponin content 37.16%, recovery rate 7.5%;
(3)The preparation of Folium Notoginseng glycoside
By 1015g Folium Notoginseng glycosides crude product 3L methanol-acetone mixed liquors(Methanol-acetone mixed liquor is methanol and acetone by volume
Than 3:1 ratio is mixed to prepare)Dissolved by heating at 60 DEG C, be subsequently cooled to -5 DEG C, standing sedimentation 20h, filtering, adds in filtrate
Add decolorising agent(Decolorising agent is activated carbon and neutral alumina, and the mass ratio of activated carbon and neutral alumina is 2:1)253g, is placed in
Carried out at 40 DEG C decolorization 2 it is small when, filtering, filtrate revolving drains to obtain yellow crystals Folium Notoginseng glycoside 453g, total through censorship content
Saponin content is 78.8%.Yield 95.01%.
Embodiment 2:The method of this extraction Folium Notoginseng glycoside carries out according to the following steps:
(1)The drying sanchi leaf 10kg for being cut into 1-2cm segments is added in 100L pots, adds 80L common salt aqueous solutions(Salt is in water
In mass concentration be 6%)When heating immersion 6 is small under the conditions of 50 DEG C, filtering, filter residue adds the food of the mass concentration 6% of 70L
When saline solution heating immersion 5 is small, filtering;Filter residue adds the common salt aqueous solution 60L of mass concentration 6%, when heating immersion 6 is small,
Filtering, merges filtrate 205L three times;
(2)The extraction processing of salt infusion and the preparation of Folium Notoginseng glycoside crude product
205L filtrates are added in extractor, add petroleum ether 45L extractions, stratification, water mutually is mutually repeated to extract with petroleum ether
Take 1 time, collect water phase;Water is mutually placed in extractor, adds n-butanol-isopropanol mixed liquor 60L (n-butanol and isopropyl alcohol
Product ratio is 5:1), continuous extraction 2 times, collect organic phase 115L, and water layer is discharged into cesspool;Organic phase is dense at decompression, 75 DEG C
2023g Folium Notoginseng glycoside crude products, total saponin content 38.23%, recovery rate 7.7% are drained to obtain in contracting;
(3)The preparation of Folium Notoginseng glycoside
By 2023g Folium Notoginseng glycosides crude product 6L methanol-acetone mixed liquors(Methanol-acetone mixed liquor is methanol and acetone by volume
Than 4:1 ratio is mixed to prepare)Dissolved by heating at 50 DEG C, be subsequently cooled to -8 DEG C, standing sedimentation 15h, filtering, adds in filtrate
Enter decolorising agent(Decolorising agent is activated carbon and neutral alumina, and the mass ratio of activated carbon and neutral alumina is 2.5:1)410g,
(decolorising agent is activated carbon and neutral alumina, and the mass ratio of activated carbon and neutral alumina is 2:1), it is placed at 45 DEG C and is taken off
When color processing 2 is small, filtering, filtrate revolving drains to obtain yellow crystals Folium Notoginseng glycoside 912.5g, is through censorship content total saponin content
77.56%.Yield 91.5%.
Embodiment 3:The method of this extraction Folium Notoginseng glycoside carries out according to the following steps:
(1)The drying sanchi leaf 10kg for being cut into 1-2cm segments is added in 100L pots, adds 80L common salt aqueous solutions(Salt exists
Mass concentration in water is 8%)When heating immersion 5 is small under the conditions of 55 DEG C, filtering;Filter residue adds 70L mass concentrations 8%
When common salt aqueous solution heating immersion 6 is small, filtering;Merge 2 filtrates;
(2)The extraction processing of salt infusion and the preparation of Folium Notoginseng glycoside crude product
Above-mentioned filtrate is added in extractor, adds petroleum ether 40L extractions, stratification, water mutually is mutually repeated to extract with petroleum ether
Take 1 time, collect water phase;Water is mutually placed in extractor, adds n-butanol-isopropanol mixed liquor 50L (n-butanol and isopropyl alcohol
Product ratio is 6:1), continuous extraction 2 times, collect organic phase, and water layer is discharged into cesspool;Organic phase is concentrated at decompression, 75 DEG C and taken out
Do to obtain Folium Notoginseng glycoside crude product, total saponin content 35.43%, recovery rate 7.8%;
(3) preparation of Folium Notoginseng glycoside
By Folium Notoginseng glycoside crude product methanol-acetone mixed liquor 5L methanol-acetone mixed liquors(Methanol-acetone mixed liquor be methanol and
Acetone by volume 5:1 ratio is mixed to prepare)Dissolved by heating at 55 DEG C, be subsequently cooled to -10 DEG C, standing sedimentation 12h, mistake
Filter, adds decolorising agent in filtrate(Decolorising agent is activated carbon and neutral alumina, and the mass ratio of activated carbon and neutral alumina is
3:1), the mass ratio of Folium Notoginseng glycoside crude product and decolorising agent is 6:1;Be placed at 43 DEG C carry out decolorization 2 it is small when, filtering, filtrate
Revolving drains to obtain yellow crystals Folium Notoginseng glycoside, is 79.82% through censorship content total saponin content.Yield 93.47%.
Claims (7)
- A kind of 1. method for extracting Folium Notoginseng glycoside, it is characterised in that carry out according to the following steps:(1)Using dry notoginseng haulm as raw material, immersion raw material, filtering are heated with common salt aqueous solution, filter residue adds salt water-soluble Liquid, soaks 1~2 time, merging filtrate, is stirred filtrate extraction, stratification, water is mutually with petroleum ether phase with petroleum ether repeatedly Extraction 1 time is repeated, collects water phase;(2)Above-mentioned water is mutually extracted with n-butanol-isopropanol mixed liquor, continuous extraction 2~3 times, it is organic to collect merging Phase, concentration organic phase obtain Folium Notoginseng glycoside crude product;(3)Folium Notoginseng glycoside crude product methanol-acetone mixed liquor is dissolved by heating, is subsequently cooled to -5~-10 DEG C, standing sedimentation 12-24h, filtering, decolorising agent is added in filtrate, is placed at 40~45 DEG C and carries out decolorization, is filtered, and filtrate revolving is drained Yellow crystals Folium Notoginseng glycoside.
- 2. the method for extraction Folium Notoginseng glycoside according to claim 1, it is characterised in that:Salt is in water in common salt aqueous solution Mass concentration be 5~8%.
- 3. the method for extraction Folium Notoginseng glycoside according to claim 1, it is characterised in that:N-butanol-isopropanol mixed liquor is N-butanol and isopropanol by volume 4~6:1 ratio is mixed to prepare.
- 4. the method for extraction Folium Notoginseng glycoside according to claim 1, it is characterised in that:Methanol-acetone mixed liquor is first Alcohol and acetone by volume 3~5:1 ratio is mixed to prepare.
- 5. the method for extraction Folium Notoginseng glycoside according to claim 1, it is characterised in that:Step(3)Middle heating-up temperature is 50~60 DEG C.
- 6. the method for extraction Folium Notoginseng glycoside according to claim 1, it is characterised in that:Decolorising agent is activated carbon and neutrality The mass ratio of aluminium oxide, activated carbon and neutral alumina is 2~3:1, the mass ratio of Folium Notoginseng glycoside crude product and decolorising agent is 4~6: 1。
- 7. the method for extraction Folium Notoginseng glycoside according to claim 1, it is characterised in that:Step(1)In at 50~60 DEG C 4~6h of lower immersion.
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Cited By (1)
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CN109134562A (en) * | 2018-10-26 | 2019-01-04 | 宁县恒瑞康生物科技有限公司 | A kind of aesculin purification process |
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