CN105535080A - Process for producing total flavonoids of radix astragali with microwave technology - Google Patents
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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)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
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- 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
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- 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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- 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 relates to the technical field of radix astragali medicine extraction, in particular to a process for producing total flavonoids of radix astragali with a microwave technology. The method includes the steps that dry radix astragali is taken, cleaned, dried and smashed, water is added, the solution is extracted with microwaves for two times, extract liquor is merged and stands to be cooled, a natural plant extract liquor clarifying agent KBT-ZTC is added, and the crude extract liquor stands and then is rotationally evaporated and concentrated to obtain a crude extract product; ethyl alcohol is added into the crude extract product, the extract product is stirred and stands for precipitation, supernate is removed through centrifugation to obtain precipitate, and the pure total flavonoids of radix astragali are obtained through macroporous adsorptive resin, silica gel column, ODS open column and medium-pressure column separation and purification technologies in sequence. Cells rupture due to microwave radiation, so that extracellular solvent enters the cells easily, more total flavonoids are dissolved, the yield of the total flavonoids is increased, and macromolecule impurities such as protein, nucleic acid and starch in the total flavonoids of radix astragali can be effectively removed through the introduced clarifying and impurity removing process.
Description
Technical field
The invention belongs to Radix Astragali extract drugs technical field, particularly relate to the technique utilizing microwave technology to produce Radix Astragali total flavones.
Background technology
The Radix Astragali is fabaceous, sweet in the mouth, and slightly warm in nature returns lung, spleen channel, there is tonifying Qi and lifting yang, beneficial taste consolidating superficial resistance, inducing diuresis to remove edema, promote the production of body fluid nourish blood, expelling pus and toxin by strengthening QI, the effect such as expelling pus and promoting granulation.Radix Astragali total flavones is one of secondary metabolite formed in Radix Astragali growth course, has various biological activity; In recent years, food safety and health food enjoy the favor of people, and Radix Astragali total flavones also becomes studied focus gradually.The chemical composition analysis of the Radix Astragali shows mainly containing flavonoid and soaping agents, and research shows the regulatory function that total flavones is useful to human physiological metabolism, for its exploitation illustrate bright prospects.Along with the increase of social pressure, the sharply outburst of cardiovascular and cerebrovascular disease, and flavone has Tumor suppression, anti-inflammation detumescence, reduces the functions such as blood fat, is therefore valued by the people gradually and studies.
Current water extraction is the traditional method extracting Chinese medicine flavone, and water extraction method is simple, easy to operation, but energy consumption is comparatively large, and extracting method is unstable, extracts the flavone purity obtained not high, how containing impurity such as protein, nucleic acid, starch.The present invention is in order to the Radix Astragali flavone yield solving above-mentioned water extraction and extract is not high, extract the large problem of energy consumption, according to the physicochemical property of effective ingredient most of in Radix Astragali total flavones and in order to cost-saving, introduce clarifier dedoping step and multiple stage separation adsorption, impurity in effective removing ingredient, reduce the energy consumption of leaching process because needing pyroprocess to produce, and extractive technique technological process is tended towards stability, method is reproducible.
Summary of the invention
The object of the invention is to overcome the shortcomings such as existing medicinal extraction Radix Astragali total flavones purity, extraction ratio are low, a kind of technique utilizing water extraction technology to produce Radix Astragali total flavones is provided.
Actualizing technology scheme of the present invention is, a kind of technique utilizing zymolysis technique to produce Radix Astragali total flavones, and be raw material with the Radix Astragali, it is characterized in that, the method step comprises:
1) crude extract obtains: dry astragalus root raw material 1kg, cleaning, dry, pulverize after add 3 ~ 6 times of water, be 80 ~ 150W at microwave power, carry out extraction 1 ~ 1.5h under the condition of pH=6 ~ 7, extracts 2 times, merge extractive liquid, is standing obtains crude extract;
2) concentration and evaporation: add natural botanical extraction liquid clarifier KBT-ZTC in the crude extract that step 1) obtains, addition is 5 ~ 10g/L, and after leaving standstill 20 ~ 30min, rotary evaporation concentrates crude extract, obtains extractum crude product;
3) dissolve remove impurity: in step 2) add ethanol in the extractum crude product that obtains, stir extractum and dissolve, staticly settle, centrifugal segregation supernatant is precipitated thing, precipitate add again ethanol carry out stirrings after standing, centrifugal collecting precipitate;
4) macroporous adsorptive resins separation and purification: macroporous adsorptive resins on precipitate step 3) obtained, carries out eluting with ethanol water, collects eluent and concentrating under reduced pressure oven dry, obtains crude extract I;
5) silicagel column separation and purification: step 4) is dried crude extract I silicagel column upper after dissolve with ethanol obtained, carry out eluting with the chloroformic solution containing methanol, collection yellow green eluent is also air-dry, obtains crude extract II;
6) with the open column separating purification of ODS: the crude extract II that step 5) the is obtained open post of ODS upper after dissolve with ethanol, carry out eluting with ethanol water, collect yellow green eluent and concentrating under reduced pressure oven dry, obtain crude extract III;
7) with in compression leg separation and purification: the upper compression leg of crude extract III that step 6) is obtained, use ethanol water eluting, from going out peak, collect eluent, stop after declining to peak collecting, eluent concentrating under reduced pressure are dried, and obtain crude extract IV;
8) filtering for crystallizing: crude extract IV dissolve with methanol that step 7) is obtained, crystallization is carried out with slowly adding water after membrane filtration, stir while adding and stop stirring to during the yellow floccule of appearance, leave standstill 20-50min, filter paper filtering, volatilized by the yellow medicine stayed on filter paper, collecting the yellow medicine after volatilizing both had been Radix Astragali total flavones.
As further qualifications of the present invention, described cleaning is for using clean water 2 ~ 3 times; Described pulverizing is that astragalus membranaceus powder is broken to 50 ~ 100 orders.
As further qualifications of the present invention, it is the extractum of 1.0 ~ 1.50 that crude extract is evaporated to water proportion d by described rotary evaporation simmer down to.
As further qualifications of the present invention, in described step 3), the addition of ethanol is 2 ~ 5 times of volumes of extractum.
As further qualifications of the present invention, described natural botanical extraction liquid clarifier KBT-ZTC is the clarifier that You Ke Lier bio tech ltd produces.
As further restriction of the present invention, containing the chloroformic solution that the chloroformic solution of methanol is containing 1 ~ 5% methanol in described step 5).
As further restriction of the present invention, the ethanol water in described step 4), step 6), step 7) is the ethanol water of 60 ~ 80%.
As further restriction of the present invention, the filter sizes in described step 9) is 0.35 ~ 0.5 μm.
The present invention achieves following substantial advance and outstanding effect:
Start with medicinal Astragalis, high-quality Radix Astragali total flavones is extracted through series of processes, on the basis of microwave action, introduced plant Chinese medicine clarification technique realizes the extraction purification of high-quality Radix Astragali total flavones, because microwave radiation causes surface of Plant callus cell to occur hole and crackle, the outer solvent of born of the same parents easily enters in cell, dissolve more total flavones, in born of the same parents, total flavones is also easily released, effectively improve the yield of total flavones, and the clarification dedoping step introduced efficiently can remove the protein in Radix Astragali total flavones, nucleic acid, the macromole impurity such as starch, and in conjunction with macroporous adsorptive resins, silicagel column, the open post of ODS, middle compression leg separating and purifying technology, improve extracts active ingredients productive rate in Radix Astragali total flavones, method Radix Astragali total flavones extraction ratio after improvement is 1.3 ~ more than 1.9mg/g, the Radix Astragali total flavones obtained can be used for regulating animal immune in veterinary clinic, antiviral, the chemoprophylaxis treatments such as antibiosis.
Radix Astragali total flavones of the present invention is admixed in the feed for nursing of animal according to certain ratio, a meal is fed in three meals in a day, the immunity of animal can be significantly improved, sickness rate has been reduced to 20.5% from initial 32%, the health realizing animal is raised, reduce the treatment of antibiotic, hormonal medicaments, realize ecological raising, improve livestock-raising economic worth.
Detailed description of the invention
Following examples describe the present invention and utilize microwave technology to produce the technique of Radix Astragali total flavones, and these descriptions are not be further limited content of the present invention, and all reagent used in following examples are all bought by commercial means.
embodiment 1
The present embodiment is with the dry Radix Astragali for raw material, and preparation method step comprises:
1) crude extract obtains: dry astragalus root raw material 1kg, cleaning, dry, pulverize after add 5 times of water (cleaning for by clean water 3 times, pulverize as astragalus membranaceus powder is broken to 50 orders), under microwave power be 150W, pH=7 condition, carry out extraction 1h, extract 2 times;
2) concentration and evaporation: add the natural botanical extraction liquid clarifier KBT-ZTC produced by Ke Lier bio tech ltd in the crude extract that step 1) obtains, addition is 5g/L, after leaving standstill 30min, rotary evaporation concentrates crude extract, is the extractum of 1.50, obtains extractum crude product to water proportion d;
3) remove impurity is dissolved: in step 2) add ethanol in the extractum crude product that obtains, the addition of ethanol is 5 times of volumes of extractum, stirs extractum and dissolves, staticly settle, centrifugal segregation supernatant is precipitated thing, and precipitate adds ethanol again to carry out leaving standstill after stirring, centrifugal collecting precipitate;
4) macroporous adsorptive resins separation and purification: macroporous adsorptive resins on precipitate step 3) obtained, carries out eluting with ethanol water, collects eluent and concentrating under reduced pressure oven dry, obtains crude extract I;
5) silicagel column separation and purification: step 4) is dried crude extract I silicagel column upper after dissolve with ethanol obtained, be that the chloroformic solution containing 15% methanol carries out eluting with the chloroformic solution containing methanol, collect yellow green eluent also air-dry, obtain crude extract II;
6) with the open column separating purification of ODS: the crude extract II that step 5) the is obtained open post of ODS upper after dissolve with ethanol, carry out eluting with ethanol water, collect yellow green eluent and concentrating under reduced pressure oven dry, obtain crude extract III;
7) with in compression leg separation and purification: the upper compression leg of crude extract III that step 6) is obtained, use ethanol water eluting, from going out peak, collect eluent, stop after declining to peak collecting, eluent concentrating under reduced pressure are dried, and obtain crude extract IV;
8) f filtering for crystallizing: crude extract IV dissolve with methanol that step 7) is obtained, crystallization is carried out with slowly adding water after membrane filtration, stir while adding and stop stirring to during the yellow floccule of appearance, leave standstill 20min, filter paper filtering, volatilized by the yellow medicine stayed on filter paper, collecting the yellow medicine after volatilizing both had been Radix Astragali total flavones.
Ethanol water in step 4), step 6), step 7) is the ethanol water of 60%, and the filter sizes in step 8) is 0.4 μm.
Originally be the extraction ratio of embodiment Radix Astragali total flavones be 1.3mg/g.
embodiment 2
1) crude extract obtains: dry astragalus root raw material 1kg, cleaning, dry, pulverize after add 6 times of water (cleaning be for by clean water 2 times, pulverize as astragalus membranaceus powder is broken to 100 orders), extraction 1.5h is carried out under microwave power is 80W, pH=6 condition, extract 2 times, merge extractive liquid, leaves standstill and cools, and obtains crude extract;
2) concentration and evaporation: add the natural botanical extraction liquid clarifier KBT-ZTC produced by Ke Lier bio tech ltd in the crude extract that step 1) obtains, addition is 10g/L, after leaving standstill 20min, rotary evaporation concentrates crude extract, is the extractum of 1.0, obtains extractum crude product to water proportion d;
3) remove impurity is dissolved: in step 2) add ethanol in the extractum crude product that obtains, the addition of ethanol is 2 times of volumes of extractum, stirs extractum and dissolves, staticly settle, centrifugal segregation supernatant is precipitated thing, and precipitate adds ethanol again to carry out leaving standstill after stirring, centrifugal collecting precipitate;
4) macroporous adsorptive resins separation and purification: macroporous adsorptive resins on precipitate step 3) obtained, carries out eluting with ethanol water, collects eluent and concentrating under reduced pressure oven dry, obtains crude extract I;
5) silicagel column separation and purification: step 4) is dried crude extract I silicagel column upper after dissolve with ethanol obtained, be that the chloroformic solution containing 1% methanol carries out eluting with the chloroformic solution containing methanol, collect yellow green eluent also air-dry, obtain crude extract II;
6) with the open column separating purification of ODS: the crude extract II that step 5) the is obtained open post of ODS upper after dissolve with ethanol, carry out eluting with ethanol water, collect yellow green eluent and concentrating under reduced pressure oven dry, obtain crude extract III;
7) with in compression leg separation and purification: the upper compression leg of crude extract III that step 6) is obtained, use ethanol water eluting, from going out peak, collect eluent, stop after declining to peak collecting, eluent concentrating under reduced pressure are dried, and obtain crude extract IV;
8) f filtering for crystallizing: crude extract IV dissolve with methanol that step 7) is obtained, crystallization is carried out with slowly adding water after membrane filtration, stir while adding and stop stirring to during the yellow floccule of appearance, leave standstill 50min, filter paper filtering, volatilized by the yellow medicine stayed on filter paper, collecting the yellow medicine after volatilizing both had been Radix Astragali total flavones.
Ethanol water in step 4), step 6), step 7) is the ethanol water of 80%.Filter sizes in described step 8) is 0.5 μm.
Originally be the extraction ratio of embodiment Radix Astragali total flavones be 1.6mg/g.
embodiment 3
1) crude extract obtains: dry astragalus root raw material 1kg, cleaning, dry, pulverize after add 3 times of water (cleaning be for by clean water 3 times, pulverize as astragalus membranaceus powder is broken to 75 orders), extraction 1.2h is carried out under microwave power is 120W, pH=6.5 condition, extract 2 times, merge extractive liquid, leaves standstill and cools, and obtains crude extract;
2) concentration and evaporation: add the natural botanical extraction liquid clarifier KBT-ZTC produced by Ke Lier bio tech ltd in the crude extract that step 1) obtains, addition is 7.5g/L, after leaving standstill 25min, rotary evaporation concentrates crude extract, is the extractum of 1.20, obtains extractum crude product to water proportion d;
3) remove impurity is dissolved: in step 2) add ethanol in the extractum crude product that obtains, the addition of ethanol is 3 times of volumes of extractum, stirs extractum and dissolves, staticly settle, centrifugal segregation supernatant is precipitated thing, and precipitate adds ethanol again to carry out leaving standstill after stirring, centrifugal collecting precipitate;
4) macroporous adsorptive resins separation and purification: macroporous adsorptive resins on precipitate step 3) obtained, carries out eluting with ethanol water, collects eluent and concentrating under reduced pressure oven dry, obtains crude extract I;
5) silicagel column separation and purification: step 4) is dried crude extract I silicagel column upper after dissolve with ethanol obtained, be that the chloroformic solution containing 3% methanol carries out eluting with the chloroformic solution containing methanol, collect yellow green eluent also air-dry, obtain crude extract II;
6) with the open column separating purification of ODS: the crude extract II that step 5) the is obtained open post of ODS upper after dissolve with ethanol, carry out eluting with ethanol water, collect yellow green eluent and concentrating under reduced pressure oven dry, obtain crude extract III;
7) with in compression leg separation and purification: the upper compression leg of crude extract III that step 6) is obtained, use ethanol water eluting, from going out peak, collect eluent, stop after declining to peak collecting, eluent concentrating under reduced pressure are dried, and obtain crude extract IV;
8) f filtering for crystallizing: crude extract IV dissolve with methanol that step 7) is obtained, crystallization is carried out with slowly adding water after membrane filtration, stir while adding and stop stirring to during the yellow floccule of appearance, leave standstill 30min, filter paper filtering, volatilized by the yellow medicine stayed on filter paper, collecting the yellow medicine after volatilizing both had been Radix Astragali total flavones.
Ethanol water in step 4), step 6), step 7) is the ethanol water of 70%.Filter sizes in described step 8) is 0.35 μm.
Originally be the extraction ratio of embodiment Radix Astragali total flavones be 1.9mg/g.
application Example 1
Radix Astragali total flavones is admixed in the feed for nursing of pig according to certain ratio and (is added 5g Radix Astragali total flavones in the feedstuff of 1kg), a meal is fed in three meals in a day, the immunity of animal can be significantly improved, sickness rate has been reduced to 18.5% from initial 30%, the health realizing animal is raised, reduce the treatment of antibiotic, hormonal medicaments, realize ecological raising, improve livestock-raising economic worth.
application Example 2
Radix Astragali total flavones is admixed in the feed for nursing of cattle according to certain ratio and (is added 9g Radix Astragali total flavones in the feedstuff of 1kg), a meal is fed in three meals in a day, the immunity of animal can be significantly improved, sickness rate has been reduced to 20.5% from initial 32%, the health realizing animal is raised, reduce the treatment of antibiotic, hormonal medicaments, realize ecological raising, improve livestock-raising economic worth.
The above embodiment of the present invention scheme is only can not limit the present invention to explanation of the present invention, scope of the present invention is indicated in claim, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, is all considered to be and is included in the scope of claims.
The present invention is through multidigit Radix Astragali total flavones and extracts processing staff's long-term work experience accumulation, and created by creative work, it is in the leaching process at actual Radix Astragali total flavones, it is 1.3 ~ more than 1.9mg/g that the method can obtain Radix Astragali total flavones extraction ratio, and the Radix Astragali total flavones obtained can be used in veterinary clinic chemoprophylaxis treatments such as animal immune adjustment, antiviral, antibiosis.
Claims (9)
1. utilize microwave technology to produce a technique for Radix Astragali total flavones, be raw material with the Radix Astragali, it is characterized in that, the method step comprises:
1) crude extract obtains: dry astragalus root raw material 1kg, cleaning, dry, pulverize after add 3 ~ 6 times of water, be 80 ~ 150W at microwave power, carry out extraction 1 ~ 1.5h under the condition of pH=6 ~ 7, extracts 2 times, merge extractive liquid, is standing obtains crude extract;
2) concentration and evaporation: add natural botanical extraction liquid clarifier KBT-ZTC in the crude extract that step 1) obtains, addition is 5 ~ 10g/L, and after leaving standstill 20 ~ 30min, rotary evaporation concentrates crude extract, obtains extractum crude product;
3) dissolve remove impurity: in step 2) add ethanol in the extractum crude product that obtains, stir extractum and dissolve, staticly settle, centrifugal segregation supernatant is precipitated thing, precipitate add again ethanol carry out stirrings after standing, centrifugal collecting precipitate;
4) macroporous adsorptive resins separation and purification: macroporous adsorptive resins on precipitate step 3) obtained, carries out eluting with ethanol water, collects eluent and concentrating under reduced pressure oven dry, obtains crude extract I;
5) silicagel column separation and purification: step 4) is dried crude extract I silicagel column upper after dissolve with ethanol obtained, carry out eluting with the chloroformic solution containing methanol, collection yellow green eluent is also air-dry, obtains crude extract II;
6) with the open column separating purification of ODS: the crude extract II that step 5) the is obtained open post of ODS upper after dissolve with ethanol, carry out eluting with ethanol water, collect yellow green eluent and concentrating under reduced pressure oven dry, obtain crude extract III;
7) with in compression leg separation and purification: the upper compression leg of crude extract III that step 6) is obtained, use ethanol water eluting, from going out peak, collect eluent, stop after declining to peak collecting, eluent concentrating under reduced pressure are dried, and obtain crude extract IV;
8) filtering for crystallizing: crude extract IV dissolve with methanol that step 7) is obtained, crystallization is carried out with slowly adding water after membrane filtration, stir while adding and stop stirring to during the yellow floccule of appearance, leave standstill 20-50min, filter paper filtering, volatilized by the yellow medicine stayed on filter paper, collecting the yellow medicine after volatilizing both had been Radix Astragali total flavones.
2. the technique utilizing microwave technology to produce Radix Astragali total flavones according to claim 1, is characterized in that, described cleaning is for using clean water 2 ~ 3 times; Described pulverizing is that astragalus membranaceus powder is broken to 50 ~ 100 orders.
3. the technique utilizing microwave technology to produce Radix Astragali total flavones according to claim 1, it is characterized in that, it is the extractum of 1.0 ~ 1.50 that crude extract is evaporated to water proportion d by described rotary evaporation simmer down to.
4. the technique utilizing microwave technology to produce Radix Astragali total flavones according to claim 1, it is characterized in that, in described step 3), the addition of ethanol is 2 ~ 5 times of volumes of extractum.
5. the technique utilizing microwave technology to produce Radix Astragali total flavones according to claim 1, it is characterized in that, in described step 1), enzyme liquid composition is a kind of or their compositions in hemicellulase, fungal amylase, cellulase.
6. the technique utilizing microwave technology to produce Radix Astragali total flavones according to claim 1, it is characterized in that, described natural botanical extraction liquid clarifier KBT-ZTC is the clarifier that You Ke Lier bio tech ltd produces.
7. the technique utilizing microwave technology to produce Radix Astragali total flavones according to claim 1, is characterized in that, containing the chloroformic solution that the chloroformic solution of methanol is containing 1 ~ 5% methanol in described step 5).
8. the technique utilizing microwave technology to produce Radix Astragali total flavones according to claim 1, it is characterized in that, the ethanol water in described step 4), step 6), step 7) is the ethanol water of 60 ~ 80%.
9. the technique utilizing microwave technology to produce Radix Astragali total flavones according to claim 1, it is characterized in that, the filter sizes in described step 9) is 0.35 ~ 0.5 μm.
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| CN104958349A (en) * | 2015-06-29 | 2015-10-07 | 兰捷 | Method for extracting high-purity total flavanone from stragalus membranaceus |
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| CN104958349A (en) * | 2015-06-29 | 2015-10-07 | 兰捷 | Method for extracting high-purity total flavanone from stragalus membranaceus |
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Application publication date: 20160504 |