CN106309466A - Cordyceps cicadae cordycepin preparation and extraction process - Google Patents
Cordyceps cicadae cordycepin preparation and extraction process Download PDFInfo
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- CN106309466A CN106309466A CN201610687872.9A CN201610687872A CN106309466A CN 106309466 A CN106309466 A CN 106309466A CN 201610687872 A CN201610687872 A CN 201610687872A CN 106309466 A CN106309466 A CN 106309466A
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- cordyceps cicadae
- cicadae shing
- cordycepin
- cordyceps
- extracting
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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
- A61K31/7042—Compounds having saccharide radicals and heterocyclic rings
- A61K31/7052—Compounds having saccharide radicals and heterocyclic rings having nitrogen as a ring hetero atom, e.g. nucleosides, nucleotides
- A61K31/706—Compounds having saccharide radicals and heterocyclic rings having nitrogen as a ring hetero atom, e.g. nucleosides, nucleotides containing six-membered rings with nitrogen as a ring hetero atom
- A61K31/7064—Compounds having saccharide radicals and heterocyclic rings having nitrogen as a ring hetero atom, e.g. nucleosides, nucleotides containing six-membered rings with nitrogen as a ring hetero atom containing condensed or non-condensed pyrimidines
- A61K31/7076—Compounds having saccharide radicals and heterocyclic rings having nitrogen as a ring hetero atom, e.g. nucleosides, nucleotides containing six-membered rings with nitrogen as a ring hetero atom containing condensed or non-condensed pyrimidines containing purines, e.g. adenosine, adenylic acid
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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
- A61K36/06—Fungi, e.g. yeasts
- A61K36/062—Ascomycota
- A61K36/066—Clavicipitaceae
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- Life Sciences & Earth Sciences (AREA)
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- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention relates to the field of edible mushrooms. A cordyceps cicadae cordycepin preparation comprises the following materials: less than 10% of sporocarp of cordyceps cicadae, more than 90% of stroma of cordyceps cicadae and 5% of a binding agent, and the sum of the three components is 100%. The invention further relates to a cordyceps cicadae cordycepin extracting process. The cordyceps cicadae cordycepin preparation has the beneficial effects that the materials are easy to get, the extracting process is simple, and an extract is prepared into a pharmaceutically defined preparation with a conventional galenic pharmacy method.
Description
Technical field
The present invention relates to edible fungi field, particularly relate to a kind of Cordyceps cicadae Shing cordycepin preparation and extraction process.
Background technology
Cordycepin (cordycepin), also known as Cordycepin, Cordycepin, cordycepin, is Cordyceps and pupa worm
(especially ucleosides) main active in grass, is also first nucleoside antibiotics separated from fungus.Cordyceps
The medicine of a kind of natural origin of element, has the same benefit of negative and positive and two-ways regulation total balance of the body that in traditional Chinese medical science medical knowledge, Cordyceps is the same
Function；It is more preferable due to the purer effect of composition in terms of hepatoprotective, guarantor kidney, lung moistening, and strongly invigorating QI and blood, can eliminate and can not control now
The diseases such as dysmenorrhea more, migraine, hyperosteogeny.In terms of doctor trained in Western medicine medical knowledge angle cordycepin have antitumor, defying age, antibacterial,
Antiviral, immunomodulating, improve metabolism, remove the multiple pharmacological effect such as free radical, have good potential applicability in clinical practice.Mesh
The research of front cordycepin is existing is just becoming an extremely active field in pharmaceutical chemistry, defying age, beauty treatment, field of health care products.Worm
Grass element (Cordycepin) is the analog of adenosine.Nineteen fifty-one, the Cunningham etc. of Germany is from the culturing filtrate of Cordyceps militaris (L.) Link.
Separate and find cordycepin.Cordycepin content in wild cordyceps is atomic, and the cordycepin of present institute is generally individually
Extract from the Cordyceps militaris (L.) Link. of fermentation.The purity that current domestic natural extract (fermentation) the is originated cordycepin more than 99% may be used
To commercially produce.Modern study finds Cordyceps cicadae Shing CI-5N, CI-P and CI-A Han cordycepin.Galactomannan
(galactomannan), by D-MANNOSE (D-mannose) and D-galactose D-galactose) form with 4:3 ratio.Therefore such as
What extracts cordycepin from Cordyceps cicadae Shing becomes those skilled in the art's urgent problem.
Summary of the invention
In order to solve above-mentioned technical problem, an object of the present invention is to provide a kind of Cordyceps cicadae Shing cordycepin preparation, this
The two of the purpose of invention are to provide the technique that a kind of method simply extracts cordycepin from Cordyceps cicadae Shing.
In order to realize above-mentioned first goal of the invention, present invention employs following technical scheme:
A kind of Cordyceps cicadae Shing cordycepin preparation, is made up of the material of following components:
Cordyceps cicadae Shing sporophore is less than 10%
Cordyceps cicadae Shing Stroma is more than 90%
Binding agent 5%
Three's component and be 100%.
In order to realize above-mentioned second goal of the invention, present invention employs following technical scheme:
A kind of Cordyceps cicadae Shing process for extracting cordycepin, comprises the following steps:
1) Cordyceps cicadae Shing sporophore is proportionally crushed to after 100-300 mesh with Cordyceps cicadae Shing Stroma mix；
2) by step 1) in obtain mixture acetone stirring immersion carry out ungrease treatment, after stratification collect third
Ketone；
3) to step 2) in the leftover materials vacuum drying that obtains obtain mixture except acetone；
4) by step 3) in the mixture that obtains and normal saline extract in the ratio of 1:10-1:5 and obtain filtrate 1-3 time；
5) to step 4) filtrate that obtains carries out pressure filtration, upper ion exchange column, first uses sodium dihydrogen phosphate eluting,
When being washed till effluent OD value less than 1.2, change sodium dihydrogen phosphate eluting, when the rapidly rising of effluent OD value and reach 1.5
Time above, start to collect eluent, stop collecting when being down to 1.2 to eluent OD value；
6) by step 5) liquid concentration collected to paste, add HPC or the CMC mixing of 5%, make preparation.
Preferably, step 1) in Cordyceps cicadae Shing sporophore and Cordyceps cicadae Shing Stroma exist through dehumidifying, dried moisture Control
Less than 7%, then pulverize with pulverizer, cross 100-300 mesh sieve.
Preferably, step 2) in the acetone consumption of defat control through step 1) mixture that obtains 5-
10 times amount, degreasing time controlled at 20-30 hour.
Preferably, step 3) in vacuum drying pressure be not less than 0.1Mpa, the vacuum drying time controls at 10-20
Hour.
Preferably, step 4) in extract at a temperature of 60-90 DEG C, extraction time is 15-20h.
Preferably, step 5) in carry out pressure filtration, eluent sodium dihydrogen phosphate flow velocity with 5-10 micron filter element
Controlling at 12000--15000ml/h, disodium hydrogen phosphate flow speed control is at 5000--7000ml/h.
Preferably, step 6) in thickening temperature below 90 DEG C concentrate.
Preferably, step 6) preparation that obtains is tablet, granule or capsule.Meet the multiple need of user
Ask.
The present invention have raw material be easy to get, extraction process simple, and extract made medicament by available conventional formulation method
The beneficial effect of the preparation in definition.
Detailed description of the invention
With instantiation, the present invention is described further below:
Embodiment 1:
A kind of Cordyceps cicadae Shing process for extracting cordycepin and preparation are prepared (granule), depletion Periostracum cicadae sporophore 100g, Cordyceps cicadae Shing
Stroma 900g, is crushed to 100 mesh respectively, first carries out ungrease treatment according to 5 times of acetone after mixing, and stirring is soaked 20 hours, stands
Collecting acetone after layering, leftover materials carry out vacuum drying and remove acetone, 20 hours drying times, vacuum 0.1Mpa, and vacuum is done
Carrying out extracting 1 time with normal saline (0.9%) 1:5 according to powder at 60 degrees Celsius by the powder of mixing after dry, extraction time is 15
Hour, merging filtrate, carry out pressure filtration, upper ion exchange column with 5 microns of filter elements, first use sodium dihydrogen phosphate eluting, wash
De-flow velocity controls at 12000--15000ml/h, when being washed till effluent OD value less than 1.2, changes sodium dihydrogen phosphate eluting,
Eluent flow rate controls at 5000--7000ml/h.When effluent OD value rises rapidly and when reaching more than 1.5, start to collect
Eluent, stops collecting when being down to 1.2 to eluent OD value.Collect liquid under 80 degree celsius temperature, be concentrated into paste, add 5%
HPC, mixing, carry out wet granulation with granulator, after having pelletized in 60 degrees Celsius of baking ovens after drying, enter according to 5g/ bag
Luggage bag.
Embodiment 2:
A kind of Cordyceps cicadae Shing process for extracting cordycepin and preparation are prepared (granule), depletion Periostracum cicadae sporophore 300g, Cordyceps cicadae Shing
Stroma 700g, is crushed to 300 mesh respectively, first carries out ungrease treatment according to 8 times of acetone after mixing, and stirring is soaked 25 hours, stands
Collecting acetone after layering, leftover materials carry out vacuum drying and remove acetone, 15 hours drying times, vacuum 0.1Mpa, and vacuum is done
Carrying out extracting 2 times with normal saline (0.9%) 1:6 according to powder at 70 degrees Celsius by the powder of mixing after dry, extraction time is 20
Hour, merging filtrate, carry out pressure filtration, upper ion exchange column with 10 microns of filter elements, first use sodium dihydrogen phosphate eluting, wash
De-flow velocity controls at 12000--15000ml/h, when being washed till effluent OD value less than 1.2, changes sodium dihydrogen phosphate eluting,
Eluent flow rate controls at 5000--7000ml/h.When effluent OD value rises rapidly and when reaching more than 1.5, start to collect
Eluent, stops collecting when being down to 1.2 to eluent OD value.Collect liquid under 70 degree celsius temperature, be concentrated into paste, add 5%
CMC, mixing, carry out wet granulation with granulator, after having pelletized in 60 degrees Celsius of baking ovens after drying, enter according to 5g/ bag
Luggage bag.
Embodiment 3:
A kind of Cordyceps cicadae Shing process for extracting cordycepin and preparation are prepared (tablet), depletion Periostracum cicadae sporophore 200g, golden cicada beggar
Seat 800g, is crushed to 100 mesh respectively, first carries out ungrease treatment according to 5 times of acetone after mixing, and stirring is soaked 20 hours, stands and divides
Collecting acetone after Ceng, leftover materials carry out vacuum drying except acetone, 20 hours drying times, vacuum 0.1Mpa, vacuum drying
After carry out extracting 1 time according to powder and normal saline (0.9%) 1:5 at 60 degrees Celsius by the powder of mixing, extraction time is 15 little
Time, merging filtrate, carry out pressure filtration, upper ion exchange column with 5 microns of filter elements, first use sodium dihydrogen phosphate eluting, eluting
Flow velocity controls at 12000--15000ml/h, when being washed till effluent OD value less than 1.2, changes sodium dihydrogen phosphate eluting, washes
De-flow velocity controls at 5000--7000ml/h.When effluent OD value rises rapidly and when reaching more than 1.5, start collection and wash
De-liquid, stops collecting when being down to 1.2 to eluent OD value.Collect liquid under 80 degree celsius temperature, be concentrated into paste, add 5%
HPC, mixing, carry out wet granulation with granulator, dried in 60 degrees Celsius of baking ovens after having pelletized, carry out according to 2g/ sheet
Tabletting, according to 60/bottled bottle.
Embodiment 4:
A kind of Cordyceps cicadae Shing process for extracting cordycepin and preparation are prepared (tablet), depletion Periostracum cicadae sporophore 400g, golden cicada beggar
Seat 600g, is crushed to 300 mesh respectively, first carries out ungrease treatment according to 8 times of acetone after mixing, and stirring is soaked 25 hours, stands and divides
Collecting acetone after Ceng, leftover materials carry out vacuum drying except acetone, 15 hours drying times, vacuum 0.1Mpa, vacuum drying
After carry out extracting 2 times according to powder and normal saline (0.9%) 1:6 at 70 degrees Celsius by the powder of mixing, extraction time is 20 little
Time, merging filtrate, carry out pressure filtration, upper ion exchange column with 10 microns of filter elements, first use sodium dihydrogen phosphate eluting, eluting
Flow velocity controls at 12000--15000ml/h, when being washed till effluent OD value less than 1.2, changes sodium dihydrogen phosphate eluting, washes
De-flow velocity controls at 5000--7000ml/h.When effluent OD value rises rapidly and when reaching more than 1.5, start collection and wash
De-liquid, stops collecting when being down to 1.2 to eluent OD value.Collect liquid under 70 degree celsius temperature, be concentrated into paste, add 5%
CMC, mixing, carry out wet granulation with granulator, dried in 60 degrees Celsius of baking ovens after having pelletized, carry out according to 2g/ sheet
Tabletting, according to 60/bottled bottle.
Embodiment 5:
A kind of Cordyceps cicadae Shing process for extracting cordycepin and preparation are prepared (capsule), depletion Periostracum cicadae sporophore 200g, golden cicada beggar
Seat 800g, is crushed to 100 mesh respectively, first carries out ungrease treatment according to 5 times of acetone after mixing, and stirring is soaked 20 hours, stands and divides
Collecting acetone after Ceng, leftover materials carry out vacuum drying except acetone, 20 hours drying times, vacuum 0.1Mpa, vacuum drying
After carry out extracting 1 time according to powder and normal saline (0.9%) 1:5 at 60 degrees Celsius by the powder of mixing, extraction time is 15 little
Time, merging filtrate, carry out pressure filtration, upper ion exchange column with 5 microns of filter elements, first use sodium dihydrogen phosphate eluting, eluting
Flow velocity controls at 12000--15000ml/h, when being washed till effluent OD value less than 1.2, changes sodium dihydrogen phosphate eluting, washes
De-flow velocity controls at 5000--7000ml/h.When effluent OD value rises rapidly and when reaching more than 1.5, start collection and wash
De-liquid, stops collecting when being down to 1.2 to eluent OD value.Collect liquid under 80 degree celsius temperature, be concentrated into paste, add 5%
HPC, mixing, carry out wet granulation with granulator, dried in 60 degrees Celsius of baking ovens after having pelletized, carry out according to 1g/ grain
Fill, according to 60/bottled bottle.
Embodiment 6:
A kind of Cordyceps cicadae Shing process for extracting cordycepin and preparation are prepared (capsule), depletion Periostracum cicadae sporophore 300g, golden cicada beggar
Seat 700g, is crushed to 300 mesh respectively, first carries out ungrease treatment according to 8 times of acetone after mixing, and stirring is soaked 25 hours, stands and divides
Collecting acetone after Ceng, leftover materials carry out vacuum drying except acetone, 15 hours drying times, vacuum 0.1Mpa, vacuum drying
After carry out extracting 2 times according to powder and normal saline (0.9%) 1:6 at 70 degrees Celsius by the powder of mixing, extraction time is 20 little
Time, merging filtrate, carry out pressure filtration, upper ion exchange column with 10 microns of filter elements, first use sodium dihydrogen phosphate eluting, eluting
Flow velocity controls at 12000--15000ml/h, when being washed till effluent OD value less than 1.2, changes sodium dihydrogen phosphate eluting, washes
De-flow velocity controls at 5000--7000ml/h.When effluent OD value rises rapidly and when reaching more than 1.5, start collection and wash
De-liquid, stops collecting when being down to 1.2 to eluent OD value.Collect liquid under 70 degree celsius temperature, be concentrated into paste, add 5%
CMC, mixing, carry out wet granulation with granulator, dried in 60 degrees Celsius of baking ovens after having pelletized, carry out according to 1g/ grain
Fill, according to 60/bottled bottle.
Claims (9)
1. a Cordyceps cicadae Shing cordycepin preparation, it is characterised in that be made up of the material of following components:
Cordyceps cicadae Shing sporophore is less than 10%
Cordyceps cicadae Shing Stroma is more than 90%
Binding agent 5%
Three's component and be 100%.
2. a Cordyceps cicadae Shing process for extracting cordycepin, it is characterised in that comprise the following steps:
1) Cordyceps cicadae Shing sporophore is proportionally crushed to after 100-300 mesh with Cordyceps cicadae Shing Stroma mix；
2) by step 1) in obtain mixture acetone stirring immersion carry out ungrease treatment, after stratification collect acetone；
3) to step 2) in the leftover materials vacuum drying that obtains obtain mixture except acetone；
4) by step 3) in the mixture that obtains and normal saline extract in the ratio of 1:10-1:5 and obtain filtrate 1-3 time；
5) to step 4) filtrate that obtains carries out pressure filtration, upper ion exchange column, and first use sodium dihydrogen phosphate eluting, be washed till
When effluent OD value is less than 1.2, change sodium dihydrogen phosphate eluting, when the rapidly rising of effluent OD value and reach more than 1.5
Time, start to collect eluent, stop collecting when being down to 1.2 to eluent OD value；
6) by step 5) liquid concentration collected to paste, add HPC or the CMC mixing of 5%, make preparation；
Wherein, step 1) in Cordyceps cicadae Shing sporophore less than 10%, Cordyceps cicadae Shing Stroma is more than 90%.
A kind of Cordyceps cicadae Shing process for extracting cordycepin the most according to claim 2, it is characterised in that step 1) in golden cicada beggar
Entity and Cordyceps cicadae Shing Stroma, are then pulverized with pulverizer through dehumidifying, dried moisture Control below 7%, cross 100-300
Mesh sieve.
A kind of Cordyceps cicadae Shing process for extracting cordycepin the most according to claim 2, it is characterised in that step 2) in defat third
Ketone consumption controls in step 1) the 5-10 times amount of the mixture arrived, degreasing time controlled at 20-30 hour.
A kind of Cordyceps cicadae Shing process for extracting cordycepin the most according to claim 2, it is characterised in that step 3) middle vacuum drying
Pressure is not less than 0.1Mpa, and the vacuum drying time controlled at 10-20 hour.
A kind of Cordyceps cicadae Shing process for extracting cordycepin the most according to claim 2, it is characterised in that step 4) at 60-90
Extracting at a temperature of DEG C, extraction time is 15-20h.
A kind of Cordyceps cicadae Shing process for extracting cordycepin the most according to claim 2, it is characterised in that step 5) middle 5-10 is micro-
Rice filter element carries out pressure filtration, and eluent sodium dihydrogen phosphate flow speed control is at 12000--15000ml/h, disodium hydrogen phosphate flow velocity
Control at 5000--7000ml/h.
A kind of Cordyceps cicadae Shing process for extracting cordycepin the most according to claim 2, it is characterised in that step 6) in 90 DEG C with
Under thickening temperature concentrate.
A kind of Cordyceps cicadae Shing process for extracting cordycepin the most according to claim 2, it is characterised in that step 6) preparation that obtains
For tablet, granule or capsule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610687872.9A CN106309466A (en) | 2016-08-18 | 2016-08-18 | Cordyceps cicadae cordycepin preparation and extraction process |
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| CN201610687872.9A CN106309466A (en) | 2016-08-18 | 2016-08-18 | Cordyceps cicadae cordycepin preparation and extraction process |
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ID=57744121
Family Applications (1)
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| CN201610687872.9A Pending CN106309466A (en) | 2016-08-18 | 2016-08-18 | Cordyceps cicadae cordycepin preparation and extraction process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496141A (en) * | 2019-09-10 | 2019-11-26 | 杭州华东医药集团新药研究院有限公司 | A kind of pharmaceutical composition containing cordyceps sinensis |
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| CN101200481A (en) * | 2006-12-15 | 2008-06-18 | 河南农业大学 | Technique for extracting cordycepin from artificial Chinese caterpillar fungus culture medium residue |
| CN101229199A (en) * | 2008-01-15 | 2008-07-30 | 重庆和润生物工程有限公司 | Integrative extract method of multi-active ingredient in cordyceps militaris mycelium |
| CN104490941A (en) * | 2014-12-17 | 2015-04-08 | 李豫杰 | Cordyceps cicadae extract improving immunity, resisting tumor, improving renal function and promoting sleep |
| KR20160122469A (en) * | 2015-04-14 | 2016-10-24 | 고려대학교 산학협력단 | Method for producing cordycepin comprising of adding algal or protein medium |
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2016
- 2016-08-18 CN CN201610687872.9A patent/CN106309466A/en active Pending
Patent Citations (4)
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| CN101200481A (en) * | 2006-12-15 | 2008-06-18 | 河南农业大学 | Technique for extracting cordycepin from artificial Chinese caterpillar fungus culture medium residue |
| CN101229199A (en) * | 2008-01-15 | 2008-07-30 | 重庆和润生物工程有限公司 | Integrative extract method of multi-active ingredient in cordyceps militaris mycelium |
| CN104490941A (en) * | 2014-12-17 | 2015-04-08 | 李豫杰 | Cordyceps cicadae extract improving immunity, resisting tumor, improving renal function and promoting sleep |
| KR20160122469A (en) * | 2015-04-14 | 2016-10-24 | 고려대학교 산학협력단 | Method for producing cordycepin comprising of adding algal or protein medium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110496141A (en) * | 2019-09-10 | 2019-11-26 | 杭州华东医药集团新药研究院有限公司 | A kind of pharmaceutical composition containing cordyceps sinensis |
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