CN110156864A - A kind of preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting - Google Patents
A kind of preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting Download PDFInfo
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- CN110156864A CN110156864A CN201910473950.9A CN201910473950A CN110156864A CN 110156864 A CN110156864 A CN 110156864A CN 201910473950 A CN201910473950 A CN 201910473950A CN 110156864 A CN110156864 A CN 110156864A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J17/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
- C07J17/005—Glycosides
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The present invention relates to the preparation methods of the black ginseng Rg3 of supercritical carbon dioxide extracting a kind of, accurately weigh red ginseng according to formula, are dissolved in dehydrated alcohol, wherein the mass ratio of red ginseng and dehydrated alcohol is in 1:(5-50) between；The solution dissolved is added in supercritical reaction kettle, under the conditions of certain temperature, pressure and dwell time, is quickly sprayed above-mentioned supercritical solution into PBS buffer solution by nozzle, simultaneously precipitating is dispersed, finally obtains ginseng sapoglycoside Rg 3.The nutritional ingredients such as the ginsenoside of noresidue solvent can be obtained in the method for the present invention, and highly-safe, preparation method is environmental-friendly, green, nontoxic, inexpensive；Process is simple, improves the extraction yield of organic principle, keeps content of ginsenoside high, can retain 90% or more and ginsenoside it is water-soluble in, substantially increase absorption of the human body to panaxoside, while being also conducive to long-term preservation, improve black ginseng absorption of nutrient ingredients ratio.
Description
Technical field
The invention belongs to black ginseng deep process technology fields, specifically, being related to a kind of black ginseng of supercritical carbon dioxide extracting
The preparation method of Rg3, a kind of black ginseng processing method improving content of ginsenoside.
Background technique
Ginseng can be used for reinforcing vital energy, veins takes off admittedly, reinforces the spleen to benefit the lung, promotes the production of body fluid to quench thirst, tranquilize the mind and promote the intelligence etc., be praised from ancient times to the present
For " king of herbal medicine ", it is widely applied by traditional medicine or even the whole world.In addition to as medicinal material, ginseng is also used for health care
Product, cosmetics, the fields such as food, ginseng will be used wider and wider.In recent years, various ginseng processed products are as function
Energy food applications are most commonly that white ginseng and red ginseng in cooking culture.Currently, black ginseng is a kind of new processing of ginseng
Product only possess some special knowledge in South Korea, and domestic research report seldom, and has no the product of batch production.
Modern medicine study shows: the bioactive ingredients of ginseng --- ginsenoside up to more than 40, and ginseng is by anti-
It is multiple to steam, dry and be manufactured into black ginseng, by active constituent contained by its process ginseng --- ginsenoside not only subtracts
It is few, it increased instead than white ginseng and red ginseng.Especially white ginseng, content is very low in red ginseng, and the high ingredient of active function has
It is improved.Therefore, it is necessary to study the higher black ginseng of functional component.
The raw material that South Korea processes black ginseng at present mostly uses water to join, and water ginseng raw material has certain seasonality, and not easy to maintain,
And red ginseng is used not to be subject to seasonal restrictions for raw material, and be easy to save.Therefore, it is also desirable to using red ginseng as the side of the black ginseng of Raw material processing
Method.
Black ginseng changes in steam in the process for exposing (boiling is repeated and dries) at branch more more, that is, ginseng
Carbohydrate (carbohydrate content: glucose, arabinose, xylose, rhamnose) plus water in the non-sugar of saponin(e glycocide (aglycome)
The chemical structure of decomposition reaction, saponin constituent changes, and produces new ingredient.Black ginseng is mainly characterized by depositing on a small quantity in red ginseng
Physiologically active ingredient ginseng sapoglycoside Rg 3 etc., Rg3 is effective biological core component, has anticancer, anti-hypertension is protected
Nervous system is protected, anticoagulant and anti-oxidation efficacy, the content in black ginseng are significantly higher than red ginseng, and the nutritive value of black ginseng is higher.
Currently, black ginseng processing technology is more at present, the method for mostly using solvent heating extraction.Height used in such methods
The bad stability of the warm condition ingredients such as the content of ginsenoside can be made to reduce, is easily denaturalized in process, is formed big
Floccule and sediment are measured, a large amount of losses of effective component are caused, and its activity is made also to decrease, ginsenoside in black ginseng
Water-soluble part only has 47.8%, is unfavorable for nutrition reservation.Meanwhile there is also solvent usage amounts for extraction method
Greatly, dissolvent residual, the disadvantages of extraction time is too long, and the minimal residue of organic solvent also have for human body it is bigger
Harm, greatly reduces the health-care effect to human body.Therefore, the content for how effectively improving water-soluble ginsenoside has become
For the hot spot of external Recent study.
Supercritical fluid is the fluid that temperature and pressure are in critical point or more, it has both liquid property and gaseousness
Matter, density is close with liquid, and viscosity and diffusion velocity and gas approach, and can never be dissolved into centainly to the dissolubility of substance
The dissolution of degree, this makes supercritical fluid technique have great operability.Supercritical carbon dioxide is as most common
Supercritical fluid is the reaction medium of the nontoxic, inertia of one kind and environmental sound.Due to its supercriticality have it is extremely excellent
Dissolubility, and when reducing its pressure, dissolubility can be reduced quickly, and can be vapored away without having hazardous solvent
Residual, therefore it has in terms of natural products extraction and greatly plays leeway.
The present invention is combined using supercritical extract etc. with conventional solvent extraction, is only spelled by simple circuit and elements
It connects, conditions or the parameter such as adjustment valve switch combination, flow velocity, extraction temperature and pressure, extraction kettle-separator-extraction kettle
Continuous extraction mode, which is extracted, is able to achieve supercritical fluid extraction Chinese-wolfberry nutritive ingredient, and low operation temperature, will not drop
The nutritive value of low activity substance, and organic solvent residual is not had, the health care for having played ginsenoside to greatest extent is made
With.
Summary of the invention
In view of the deficiencies of the prior art, the object of the invention abstract provides a kind of black ginseng Rg3's of supercritical carbon dioxide extracting
Preparation method, a kind of black ginseng deep working method improving content of ginsenoside.
In order to solve the above technical problems, the present invention adopts the following technical solutions: a kind of black ginseng of supercritical carbon dioxide extracting
The preparation method of Rg3, includes the following steps:
1) a certain amount of red ginseng is accurately weighed according to formula, be added into a certain amount of dehydrated alcohol, stirring dissolves it sufficiently, puts
Enter in ultrasonic oscillation device 5 minutes, after filtering, filtrate is put into refrigerator for use, wherein the mass ratio of red ginseng and dehydrated alcohol exists
Between 1:(5-50)；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, entering in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 15MPa-40MPa and temperature is between 313K-343K,
And pressure maintaining 20min -60min obtains supercritical solution；
3) above-mentioned supercritical solution is quickly sprayed by nozzle into PBS buffer solution, is dispersed simultaneously precipitating, guarantor can be obtained
Stay 90% or more water-soluble ginsenoside；
4) above-mentioned ginsenoside suspension, the as described black ginseng nutritional ingredient Rg3 are collected.
Basic idea of the present invention is: a certain amount of red ginseng accurately weighed according to formula, is dissolved in dehydrated alcohol, it will
The solution dissolved is added in supercritical reaction kettle, controls certain temperature and pressure, and pressure maintaining certain time, will by nozzle
Above-mentioned supercritical solution is quickly sprayed into PBS buffer solution, is dispersed simultaneously precipitating, is finally obtained 90% or more reservation and is dissolved in
The ginsenoside of water.The various enzymatic activitys and autodigestion that this method will not make black ginseng inherent keep content of ginsenoside high, pole
The earth improves black ginseng absorption of nutrient ingredients ratio.
The black ginseng application component Rg3 water-soluble.
The dosage of the cosolvent dehydrated alcohol is in CO2In molar fraction be calculated as 5% -30%.
The PBS buffer concentration is 0.01Mol/L, and pH value is equal to 7.2.
The nozzle diameter is between 100 μm -500 μm.
The CoQ10 nanoliposome prepared using the method for the invention, liposomal particle size is usually in 60nm-150nm
Between, number average bead diameter is about 100nm, and particle diameter distribution is narrow, and monodispersity is fine, and encapsulation rate can be up to 75% or more.
Compared with tradition extracts the method for ginseng sapoglycoside Rg 3, the advantage of the method for the present invention is mainly reflected in following side
Face:
1) environmental-friendly, green is nontoxic, inexpensive；
2) ginsenoside extraction yield is high, can retain 90% or more ginsenoside and it is water-soluble in；
3) it is extracted by extraction kettle-separation-extraction continuation mode, high production efficiency.
Specific embodiment
The present invention is further illustrated below by embodiment, is not intended to limit the scope of the invention.
Embodiment 1
A kind of black ginseng Rg3 of supercritical carbon dioxide extracting, following steps preparation:
1) 5 grams of a certain amount of red ginseng is accurately weighed by according to formula, it is added to absolute ethanol by mass parts 15%, stirring makes it
Solution is sufficiently dissolved and be prepared into, is put into ultrasonic oscillation device 5 minutes, filtered fluid is put into refrigerator for use；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, enter in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 20MPa and temperature is 323K, and pressure maintaining 40min must surpass
Critical Solution；
3) above-mentioned supercritical solution is quickly sprayed by the nozzle that diameter is 500 μm into PBS buffer solution, is dispersed and sinks
Analysis；
4) above-mentioned ginsenoside suspension, the as described Ginsenoside Rg3 are collected.
Its various enzyme will not activate, will not autodigestion, keep Rg3 content high, 92% solubility can be retained, mentioned significantly
High absorption of the human body to panaxoside, while being also conducive to long-term preservation, improve black ginseng absorption of nutrient ingredients ratio.
Embodiment 2
A kind of black ginseng Rg3 of supercritical carbon dioxide extracting, following steps preparation:
1) 5 grams of a certain amount of red ginseng is accurately weighed according to formula, it is added in dehydrated alcohol by mass fraction 10%, stirring makes
It sufficiently dissolves and is prepared into solution, is put into ultrasonic oscillation device 5 minutes, and filtered fluid is put into refrigerator for use；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, enter in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 20MPa and temperature is 333K, and pressure maintaining 30min must surpass
Critical Solution；
3) it is that 250 μm of nozzles are quickly sprayed into PBS buffer solution by diameter by above-mentioned supercritical solution, is dispersed and sinks
The soluble ginsenoside of reservation 95% can be obtained in analysis；
4) above-mentioned ginsenoside suspension, the as described Rg3 are collected.Black ginseng nutritional ingredient ginsenoside (Rg3) can be obtained,
Various enzymes will not activate, will not autodigestion, keep Rg3 content high, the suction for substantially increasing human body to panaxoside can be retained
It receives, while being also conducive to long-term preservation, improve black ginseng absorption of nutrient ingredients ratio.
Embodiment 3
A kind of black ginseng Rg3 of supercritical carbon dioxide extracting, following steps preparation:
1) 5 grams of red ginseng accurately are weighed according to formula, divides 20% to be added to absolute ethanol by quality it, stirring dissolves it sufficiently
And it is prepared into solution, it is put into ultrasonic oscillation device 5 minutes, filtered fluid is put into refrigerator for use；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, enter in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 25MPa and temperature is 328K, and pressure maintaining 50min must surpass
Critical Solution；
3) it is that 170 μm of nozzles are quickly sprayed into PBS buffer solution by diameter by above-mentioned supercritical solution, is dispersed and sinks
Analysis can be obtained and retain 90% or more water-soluble ginsenoside；
4) above-mentioned ginsenoside suspension is collected, Ginsenoside Rg3 can be obtained.Its various enzyme will not activate, and will not itself
Digestion keeps Rg3 content high, can retain 90% solubility, substantially increase absorption of the human body to panaxoside, while being also conducive to
Long-term preservation improves black ginseng absorption of nutrient ingredients ratio.
Embodiment 4
A kind of black ginseng Rg3 of supercritical carbon dioxide extracting, following steps preparation:
1) 5 grams of red ginseng accurately are weighed according to formula, it is added in dehydrated alcohol by mass fraction for 15%, stirring fills it
Divide and dissolve and be prepared into solution, is put into ultrasonic oscillation device 5 minutes, filtered fluid is put into refrigerator for use；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, enter in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 15MPa and temperature is 318K, and pressure maintaining 30min must surpass
Critical Solution；
3) it is that 500 μm of nozzles are quickly sprayed into PBS buffer solution by diameter by above-mentioned supercritical solution, is dispersed and sinks
The soluble ginsenoside of reservation 93.5% can be obtained in analysis；
4) above-mentioned ginsenoside suspension, the as described black ginseng nutritional ingredient Rg3 are collected.
Its various enzyme will not activate, will not autodigestion, keep Rg3 content high, 935% solubility can be retained, significantly
Absorption of the human body to panaxoside is improved, while being also conducive to long-term preservation, improves black ginseng absorption of nutrient ingredients ratio.
Claims (8)
1. a kind of preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting, it is characterised in that include the following steps:
1) a certain amount of red ginseng is accurately weighed according to formula, be added into a certain amount of dehydrated alcohol, stirring dissolves it sufficiently, puts
Enter in ultrasonic oscillation device 5 minutes, after filtering, filtrate is put into refrigerator for use, wherein the mass ratio of red ginseng and dehydrated alcohol exists
Between 1:(5-50)；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, entering in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 15MPa-40MPa and temperature is between 313K-343K,
And pressure maintaining 20min -60min obtains supercritical solution；
3) above-mentioned supercritical solution is quickly sprayed by nozzle into PBS buffer solution, is dispersed simultaneously precipitating, guarantor can be obtained
Stay 90% or more water-soluble ginsenoside；
4) above-mentioned ginsenoside suspension, the as described black ginseng nutritional ingredient Rg3 are collected.
2. the preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting according to claim 1, which is characterized in that anhydrous
The dosage of ethyl alcohol is in CO2In molar fraction be calculated as 5% -30%.
3. the preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting according to claim 1, which is characterized in that described
PBS buffer concentration is 0.01Mol/L, pH=7.2.
4. according to the method described in claim 1, it is characterized in that the nozzle diameter is between 100 μm -500 μm.
5. the preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting according to any one of claims 1 to 4, feature
It is, prepares as follows:
1) 5 grams of a certain amount of red ginseng is accurately weighed by according to formula, it is added to absolute ethanol by mass parts 15%, stirring makes it
Solution is sufficiently dissolved and be prepared into, is put into ultrasonic oscillation device 5 minutes, filtered fluid is put into refrigerator for use；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, enter in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 20MPa and temperature is 323K, and pressure maintaining 40min must surpass
Critical Solution；
3) above-mentioned supercritical solution is quickly sprayed by the nozzle that diameter is 500 μm into PBS buffer solution, is dispersed and sinks
Analysis；
4) above-mentioned ginsenoside suspension, the as described black ginseng nutriment Rg3 are collected.
6. the preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting according to any one of claims 1 to 4, feature
It is, prepares as follows:
1) 5 grams of a certain amount of red ginseng is accurately weighed according to formula, it is added in dehydrated alcohol by mass fraction 10%, stirring makes
It sufficiently dissolves and is prepared into solution, is put into ultrasonic oscillation device 5 minutes, and filtered fluid is put into refrigerator for use；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, enter in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 20MPa and temperature is 333K, and pressure maintaining 30min must surpass
Critical Solution；
3) it is that 250 μm of nozzles are quickly sprayed into PBS buffer solution by diameter by above-mentioned supercritical solution, is dispersed and sinks
Analysis；
4) above-mentioned ginsenoside suspension, the as described black ginseng nutriment Rg3 are collected.
7. the preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting according to any one of claims 1 to 4, feature
It is, prepares as follows:
1) 5 grams of red ginseng accurately are weighed according to formula, divides 20% to be added to absolute ethanol by quality it, stirring dissolves it sufficiently
And it is prepared into solution, it is put into ultrasonic oscillation device 5 minutes, filtered fluid is put into refrigerator for use；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, enter in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 25MPa and temperature is 328K, and pressure maintaining 50min must surpass
Critical Solution；
3) it is that 170 μm of nozzles are quickly sprayed into PBS buffer solution by diameter by above-mentioned supercritical solution, is dispersed and sinks
Analysis；
4) above-mentioned ginsenoside suspension is collected, Ginsenoside Rg3 can be obtained.
8. the preparation method of the black ginseng Rg3 of supercritical carbon dioxide extracting according to any one of claims 1 to 4, feature
It is, prepares as follows:
1) 5 grams of red ginseng accurately are weighed according to formula, it is added in dehydrated alcohol by mass fraction for 15%, stirring fills it
Divide and dissolve and be prepared into solution, is put into ultrasonic oscillation device 5 minutes, filtered fluid is put into refrigerator for use；
2) above-mentioned solution is placed in supercritical reaction kettle, opens carbon dioxide steel cylinder, carbon dioxide gas is cooled to through cold
After liquid, enter in reaction kettle after being pressurizeed by high-pressure pump, control pressure is 15MPa and temperature is 318K, and pressure maintaining 30min must surpass
Critical Solution；
3) it is that 500 μm of nozzles are quickly sprayed into PBS buffer solution by diameter by above-mentioned supercritical solution, is dispersed and sinks
Analysis；
4) above-mentioned ginsenoside suspension, the as described black ginseng nutritional ingredient Rg3 are collected.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111956677A (en) * | 2020-08-31 | 2020-11-20 | 延边大学 | Black ginseng extract for treating renal interstitial fibrosis, black ginseng quick-release pellet and application thereof |
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Application publication date: 20190823 |
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