CN116970290A - Cordyceps militaris pigment extract and preparation method and application thereof - Google Patents

Cordyceps militaris pigment extract and preparation method and application thereof Download PDF

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CN116970290A
CN116970290A CN202310774744.8A CN202310774744A CN116970290A CN 116970290 A CN116970290 A CN 116970290A CN 202310774744 A CN202310774744 A CN 202310774744A CN 116970290 A CN116970290 A CN 116970290A
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cordyceps militaris
extract
pigment
ethanol
pigment extract
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CN116970290B (en
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高益槐
王�忠
郑春源
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Alpha (fujian) Biotechnology Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9728Fungi, e.g. yeasts
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
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    • A23L3/3472Compounds of undetermined constitution obtained from animals or plants
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
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    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/40Colouring or decolouring of foods
    • A23L5/42Addition of dyes or pigments, e.g. in combination with optical brighteners
    • A23L5/43Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
    • A61K8/498Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/678Tocopherol, i.e. vitamin E
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0096Purification; Precipitation; Filtration
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    • C09K15/34Anti-oxidant compositions; Compositions inhibiting chemical change containing plant or animal materials of unknown composition
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    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
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    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/522Antioxidants; Radical scavengers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
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Abstract

The invention relates to a processing method of cordyceps militaris, in particular to a cordyceps militaris pigment extract, a preparation method and application thereof. The method comprises the following steps: extracting Cordyceps militaris powder with alcohol, and separating to obtain an alcohol extract solution and a Cordyceps militaris sediment; adding vitamin E, tea polyphenol and distilled water into the Cordyceps militaris sediment, heating to 55-60 ℃ for 20-30 min, and filtering to obtain a liquid extract; mixing the ethanol extraction solution and the liquid extraction solution, heating to 55-60 ℃ for 20-30 min, filtering to remove precipitate, and concentrating under reflux until the water content is 20% to obtain a Cordyceps militaris primary extract; centrifugal separation is carried out for 30-40 min in a changing magnetic field at 3000 r/min-4000 r/min, then supernatant is taken, and the Cordyceps militaris pigment extract is obtained through freeze drying. The invention can simultaneously improve the extraction rate and purity of the cordyceps militaris pigment by alcohol extraction and adding vitamin E and tea polyphenol and combining the action of a magnetic field.

Description

Cordyceps militaris pigment extract and preparation method and application thereof
Technical Field
The invention relates to a processing method of cordyceps militaris, in particular to a cordyceps militaris pigment extract, a preparation method and application thereof.
Background
Cordyceps militaris, also called Cordyceps militaris, belongs to the same genus as Cordyceps militaris, is also rich in bioactive substances, and has high medical and health-care effects. Modern scientific researches show that cordycepin is a nucleoside substance with antibacterial and antiviral activity, cordyceps militaris has good antibacterial and anti-inflammatory effects, and the main antibacterial component cordycepin in Cordyceps militaris has been proved to have inhibitory effects on staphylococci, streptococci, bacillus melitensis, bacillus anthracis, pig hemorrhagic septicemia bacillus and the like. Cordyceps militaris can synthesize carotenoid in the mycelium and fruiting body stages, and most of the synthesized carotenoid is rare water-soluble carotenoid and cordycepin. The cordycepin is used as a natural pigment, has various effects of anti-inflammatory, anti-cancer, anti-oxidation and the like, is soluble in water, has good coloring effect and has wider application space in cosmetics.
The extraction of Cordyceps militaris pigment is usually carried out by ethanol extraction, but most of the ethanol extraction substances are mixtures containing organic matters, so that the purity of the pigment is low, and separation and purification by means of resin, chromatographic columns and the like are needed, so that the pigment loss is high.
Disclosure of Invention
First, the technical problem to be solved
In order to solve the problems in the prior art, the invention provides a novel extraction method of the cordyceps militaris pigment extract, which can simultaneously improve the extraction rate and purity of the cordyceps militaris pigment by alcohol extraction, vitamin E and tea polyphenol are added, and the combination mode of magnetic field action.
Correspondingly, the invention also provides a novel cordyceps militaris pigment extract and application thereof, and the cordyceps militaris pigment extract has excellent coloring performance and stability.
(II) technical scheme
In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps:
the invention provides a preparation method of a cordyceps militaris pigment extract, which comprises the following steps:
s1 primary extraction: drying Cordyceps militaris until the water content is 10%, pulverizing into Cordyceps militaris powder, extracting with ethanol according to the weight ratio of Cordyceps militaris powder to ethanol of 1:20-1:30, and separating to obtain an ethanol extract solution and a Cordyceps militaris precipitate;
s2, adding vitamin E, tea polyphenol and distilled water into the cordyceps militaris sediment, heating to 55-60 ℃ for 20-30 min, and filtering to obtain a liquid extract; wherein, the weight ratio of the cordyceps militaris powder to the vitamin E to the tea polyphenol to the distilled water is 1:0.1-0.2:0.1-0.2:50-60;
s3, mixing the alcohol extraction solution and the liquid extraction solution, heating to 55-60 ℃ for 20-30 min, filtering to remove precipitate, and carrying out reflux concentration until the water content is 20% to obtain a cordyceps militaris primary extract;
s4, performing centrifugal separation on the cordyceps militaris primary extract in a changing magnetic field for 30-40 min at 3000-4000 r/min, taking supernatant, and performing freeze drying to obtain the cordyceps militaris pigment extract.
Firstly, alcohol extract and sediment are obtained through alcohol extraction, and vitamin E and tea polyphenol are added into the sediment to improve the extraction rate of pigment; after the alcohol extraction solution and the liquid extraction solution are mixed, the non-pigment substances can be continuously promoted to be settled by continuing heating so as to improve the purity; in addition, by performing centrifugal separation in a variable magnetic field, the adsorption of charges between the non-dye substance and dye molecule can be destroyed in the above-mentioned centrifugal speed range and centrifugal time, and the purity can be improved by centrifugal separation.
Alternatively, the varying magnetic field strength may range from 800 to 1200 gauss.
Non-pigment substances can be selectively separated within the variation range of the magnetic field intensity, so that the pigment yield is improved.
Optionally, the concentration of the ethanol is 70% -80%.
In a second aspect, the invention also provides the cordyceps militaris pigment extract prepared by the preparation method in any scheme.
In a third aspect, the invention also provides an application of the cordyceps militaris pigment extract in foods and cosmetics.
The cordyceps militaris pigment extract obtained by the invention has excellent stability of the pigment due to the tea polyphenol and the vitamin E, has good antibacterial function by combining the cordyceps militaris pigment, can be directly applied to food cosmetics, and reduces the use of antioxidants and preservatives in the food cosmetics.
(III) beneficial effects
The beneficial effects of the invention are as follows:
according to the extraction method of the cordyceps militaris pigment extract, the extraction rate and the purity of the cordyceps militaris pigment can be improved simultaneously by alcohol extraction, vitamin E and tea polyphenol are added, and the combination mode of the magnetic field effect;
the addition of vitamin E and tea polyphenol can promote the extraction of cordyceps militaris pigment, and the yield and purity are improved;
wherein, the changing magnetic field can generate eddy current to destroy the adsorption of non-pigment substances, charges of pigment molecules and the like, thereby improving the purity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
Example 1
The preparation method of the cordyceps militaris pigment extract comprises the following steps:
s1 primary extraction: drying Cordyceps militaris until the water content is 10%, pulverizing into Cordyceps militaris powder, mixing Cordyceps militaris powder with 75% ethanol at a weight ratio of 1:25, extracting with ethanol, and separating to obtain ethanol extract solution and Cordyceps militaris precipitate;
s2, adding vitamin E, tea polyphenol and distilled water into the cordyceps militaris sediment, heating to 58 ℃ for 25min, and filtering to obtain a liquid extract; wherein, the weight ratio of the Cordyceps militaris powder to the vitamin E to the tea polyphenol to the distilled water is 1:0.15:0.2:50;
s3, mixing the alcohol extraction solution and the liquid extraction solution, heating to 60 ℃ for 25min, filtering to remove precipitate, and concentrating under reflux until the water content is 20% to obtain a cordyceps militaris primary extract;
s4, performing centrifugal separation on the cordyceps militaris primary extract in a magnetic field with the variation of 800-1200 gauss at 3500r/min for 35min, taking supernatant, and performing freeze drying to obtain the cordyceps militaris pigment extract.
Example 2
The preparation method of the cordyceps militaris pigment extract comprises the following steps:
s1 primary extraction: drying Cordyceps militaris until the water content is 10%, pulverizing into Cordyceps militaris powder, mixing Cordyceps militaris powder with 80% ethanol at a weight ratio of 1:30, extracting with ethanol, and separating to obtain ethanol extract solution and Cordyceps militaris precipitate;
s2, adding vitamin E, tea polyphenol and distilled water into the cordyceps militaris sediment, heating to 60 ℃ for 30min, and filtering to obtain a liquid extract; wherein, the weight ratio of the Cordyceps militaris powder to the vitamin E to the tea polyphenol to the distilled water is 1:0.1:0.1:55;
s3, mixing the alcohol extraction solution and the liquid extraction solution, heating to 55 ℃ for 20-30 min, filtering to remove precipitate, and concentrating under reflux until the water content is 20% to obtain a Cordyceps militaris primary extract;
s4, performing centrifugal separation on the cordyceps militaris primary extract in a magnetic field with the variation of 800-1200 gauss at 3000r/min for 40min, taking supernatant, and performing freeze drying to obtain the cordyceps militaris pigment extract.
Example 3
The preparation method of the cordyceps militaris pigment extract comprises the following steps:
s1 primary extraction: drying Cordyceps militaris until the water content is 10%, pulverizing into Cordyceps militaris powder, mixing Cordyceps militaris powder with 70% ethanol at a weight ratio of 1:20, extracting with ethanol, and separating to obtain ethanol extract solution and Cordyceps militaris precipitate;
s2, adding vitamin E, tea polyphenol and distilled water into the cordyceps militaris sediment, heating to 55 ℃ for 20min, and filtering to obtain a liquid extract; wherein, the weight ratio of the Cordyceps militaris powder to the vitamin E to the tea polyphenol to the distilled water is 1:0.2:0.15:60;
s3, mixing the alcohol extraction solution and the liquid extraction solution, heating to 57 ℃ for 20-30 min, filtering to remove precipitate, and concentrating under reflux until the water content is 20% to obtain a Cordyceps militaris primary extract;
s4, performing centrifugal separation on the cordyceps militaris primary extract for 30min in a magnetic field with the variation of 800-1200 gauss at 4000r/min, taking supernatant, and performing freeze drying to obtain the cordyceps militaris pigment extract.
Comparative example 1
The preparation method of the cordyceps militaris pigment extract is the same as in example 1, and the difference is that: vitamin E and tea polyphenol are not added in the step S2.
Comparative example 2
The preparation method of the cordyceps militaris pigment extract is the same as in example 1, and the difference is that: in step S2, vitamin E is not added.
Comparative example 3
The preparation method of the cordyceps militaris pigment extract is the same as in example 1, and the difference is that: in the step S2, tea polyphenol is not added.
Comparative example 4
The preparation method of the cordyceps militaris pigment extract is the same as in example 1, and the difference is that: in step S3, no heat treatment is performed.
Comparative example 5
The preparation method of the cordyceps militaris pigment extract is the same as in example 1, and the difference is that: in step S4, no changing magnetic field is applied.
The pigment contents of the Cordyceps militaris pigment extracts prepared in examples 1 to 3 and comparative examples 1 to 5 were measured respectively.
The measuring method comprises the following steps: the absorption intensity of the sample at 455nm was measured by ultraviolet spectrophotometry, and the concentration of each sample was converted by measuring the absorption intensity of β -carotenoid at 455nm and formulating a standard curve.
Wherein, the samples are the Cordyceps militaris pigment extracts prepared in examples 1-3 and comparative examples 1-5, water is added to prepare a solution with the concentration of 10mg/L, and the solution with the same concentration of vitamin E and tea polyphenol is used as blank liquid for correction.
Wherein the yield is calculated as follows: the ratio of the Cordyceps militaris pigment extract to the Cordyceps militaris dried to the water content of 10%.
The content of the pigment in the Cordyceps militaris pigment extract obtained in each of the examples and comparative examples is shown in the following table after measurement and conversion:
from the above table it can be obtained: the invention can improve the purity of the pigment in the obtained product by adding vitamin E and tea polyphenol and applying a variable magnetic field.
The data of the yield can be obtained: vitamin E and tea polyphenol can improve the yield of products;
the heating treatment in step S3, as well as the application of a varying magnetic field, can significantly affect the yield of the product. Multiplying the yields and the content gives a total yield of pigment the yield of example 1 which is very significantly greater than that of comparative examples 1-5.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (5)

1. A preparation method of a cordyceps militaris pigment extract is characterized by comprising the following steps of: which comprises the following steps:
s1 primary extraction: drying Cordyceps militaris until the water content is 10%, pulverizing into Cordyceps militaris powder, extracting with ethanol according to the weight ratio of Cordyceps militaris powder to ethanol of 1:20-1:30, and separating to obtain an ethanol extract solution and a Cordyceps militaris precipitate;
s2, adding vitamin E, tea polyphenol and distilled water into the cordyceps militaris sediment, heating to 55-60 ℃ for 20-30 min, and filtering to obtain a liquid extract; wherein, the weight ratio of the cordyceps militaris powder to the vitamin E to the tea polyphenol to the distilled water is 1:0.1-0.2:0.1-0.2:50-60;
s3, mixing the alcohol extraction solution and the liquid extraction solution, heating to 55-60 ℃ for 20-30 min, filtering to remove precipitate, and carrying out reflux concentration until the water content is 20% to obtain a cordyceps militaris primary extract;
s4, performing centrifugal separation on the Cordyceps militaris primary extract at 3000-4000 r/min in a variable magnetic field for 30-40 min, taking supernatant, and performing freeze drying to obtain the Cordyceps sinensis pigment extract.
2. The method for preparing the cordyceps militaris pigment extract as claimed in claim 1, wherein: the varying magnetic field strength ranges from 800 to 1200 gauss.
3. The method for preparing the cordyceps militaris pigment extract as claimed in claim 1, wherein: the concentration of the ethanol is 70-80%.
4. A cordyceps militaris pigment extract prepared by the method of any one of claims 1-3.
5. A method for preparing Cordyceps militaris pigment extract as defined in claim 4, and its application in food and cosmetics.
CN202310774744.8A 2023-06-28 2023-06-28 Cordyceps militaris pigment extract and preparation method and application thereof Active CN116970290B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101492483A (en) * 2008-10-27 2009-07-29 东莞市生物技术研究所 Method for extraction and purification of cordycepin, and method for preparation of cordycepin dry powder
CN104447926A (en) * 2014-11-28 2015-03-25 哈尔滨墨医生物技术有限公司 Extraction method for cordycepin
CN108948785A (en) * 2018-10-16 2018-12-07 安徽祥康生物工程有限公司 The extracting method of pigment in a kind of Cordyceps militaris
CN109998983A (en) * 2019-05-14 2019-07-12 安发(福建)生物科技有限公司 A kind of moist lipstick of the extract containing Cordyceps militaris and preparation method thereof
CN111297918A (en) * 2020-05-04 2020-06-19 福州乾正药业有限公司 Composition of EGCG and cordyceps militaris extract and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101492483A (en) * 2008-10-27 2009-07-29 东莞市生物技术研究所 Method for extraction and purification of cordycepin, and method for preparation of cordycepin dry powder
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