CN104546657B - Method for extracting cosmetics used active matters from cordyceps sinensis - Google Patents

Method for extracting cosmetics used active matters from cordyceps sinensis Download PDF

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CN104546657B
CN104546657B CN201410740160.XA CN201410740160A CN104546657B CN 104546657 B CN104546657 B CN 104546657B CN 201410740160 A CN201410740160 A CN 201410740160A CN 104546657 B CN104546657 B CN 104546657B
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water
cordyceps sinensis
extracting
glycerine
cordyceps
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CN104546657A (en
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林河妹
马廉正
袁裕泉
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YICHANG SHANCHENGSHUIDU CORDYCEPS Co.,Ltd.
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Guangdong HEC Pharmaceutical
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Abstract

The invention discloses a method for extracting cosmetics used active matters from cordyceps sinensis, wherein the method is further suitable for extracting active matters from cordyceps sinensis mycelia. The method comprises the following steps: adding pulverized cordyceps sinensis or cordyceps sinensis mycelia and water into an extraction device, heating through water bath, and extracting for the first time; extracting a powder for the second time by using the mixture of glycerol and water; concentrating the obtained extracts in vacuum rotationally, centrifuging and filtering with a microfiltration membrane in sequence; and adding an appropriate amount of a polyol to obtain a final extract. The extract obtained by adopting the method is free from sensitizing organic solvent residue, is improved in the aspects of deterioration and precipitation during storage and is improved in the compatibility with the formula of the cosmetics.

Description

A kind of extracting method of Cordyceps sinensis active matter used for cosmetic
Technical field
The present invention relates to a kind of field of traditional Chinese medicine extraction, refer in particular to a kind of for the Cordyceps sinensis active matter in cosmetics or winter The extracting method of worm summer grass mycelia active thing.
Background technology
Cordyceps sinensis is a kind of rare traditional Chinese medicine of China, is classified as Chinese three big tonics together with ginseng, pilose antler.Early in one The Seventh Five-Year Plan 7 years《The new compilation of materia medica》In just have " Cordyceps sinensis Gan Pingbao lung, kidney-nourishing, mend marrow, hemostasis and phlegm, phthisical cough, control diaphragm disease All good " record.The traditional Chinese medical science thinks, Chinese caterpillar fungus enters lung kidney two warp, can tonifying lung cloudy, and can kidney-replenishing, cure mainly kidney deficiency, impotence and seminal emission, Soreness of waist and knee joint, eak after being ill, chronic cough is weak, phthisical cough phlegm blood, and spontaneous sweating etc., is that uniquely one kind can balance simultaneously, adjust the moon The Chinese medicine of sun.And cordyceps mycelia is the stroma of Cordyceps sinensis, there is the composition similar to Cordyceps sinensis, and the containing of active matter Amount is very high.At present, Cordyceps sinensis and its mycelium are mainly used in health care, food aspect, in the fortune of the beauty industry such as cosmetics With little, but their active component Cordyceps sinensis polysaccharide, cordycepic acid, superoxide dismutase and amino acid of being rich in etc. have well Cosmetic result.
Considerably less with regard to the report of Cordyceps sinensis and the extracting method of cordyceps mycelia active material, through the present invention at present The long-term experiment of people finds, prior art all has some shortcomings.
Patent publication No. CN 101928352A obtains single having by steps such as water backflow, concentration, filtration, column chromatographies Effect composition.For cosmetic field, the composition such as amino acid in cordyceps mycelia, polysaccharide, adenosine and cordycepic acid all has U.S. Hold effect of skin care, the cordyceps mycelia in the method is not comprehensively utilized.
Number of patent application CN 93112049.7 disclose with ethanol or acetone soak 7-10 days, filtration, reduced pressure concentration side The method that method prepares the extract of Cordceps militaris, this process takes oversize, is unfavorable for industrialized production.
Number of patent application CN 200710030010.X and CN 201110004151.0 discloses by heating acidolysis, pulverizing Ultrasonic, the step such as filter, concentrate and prepare the activity extract of cordyceps mycelia, but there is the irritant gas of extract band in the method After taste and Ultrasonic Pulverization, extract easily separates out the problem of particle precipitation in storing process.
Number of patent application CN 201310303417.0 discloses the technique by adding solvent heating extraction, filter, drying Prepare cordyceps mycelia extract.Application number CN 201010017125.7, application number CN 201010017125.7 China specially Profit discloses prepares cordyceps mycelia freeze-dried powder by ultrasonic extraction, thickening filtration, freeze-drying.The extraction of these methods preparation Thing is pressed powder, and with liquid extraction liquid phase ratio, being added into cosmetics has insoluble granule, the especially cosmetics of water aqua type, Also easily separate out and form precipitation.
Content of the invention
It is an object of the invention to provide a kind of extracting method of Cordyceps sinensis active matter used for cosmetic, also it is simultaneously suitable for the winter The extraction of worm summer grass fermentation mycelium, this method is simple and reliable, is avoided that relevant material separates out and forms precipitation, improves such The quality of cosmetics.The extract that the method obtains is applied to the cosmetics of the formulations such as cream, emulsion, aqua, especially suitable Cosmetics in water aqua type.
For reaching above-mentioned purpose, the invention provides a kind of preparation method of cordyceps extracting liquid used for cosmetic, comprise Following steps:
(1) Cordyceps sinensis or cordyceps mycelia powder and water is 1 in mass ratio:20~30 ratio mixing, 20~ In 100 DEG C of water-baths, constant temperature stirring extraction was filtered after 30~100 minutes;
(2) after filtering, solid adds the glycerine of same step (1) aqueous phase homogenous quantities to be extracted with the mixed liquor of water, 20~ In 100 DEG C of water-baths, constant temperature stirring extraction was filtered after 30~100 minutes, merged the body of the filtrate extracted twice, wherein glycerine and water Long-pending ratio is 1:20~50;
(3) by after through being concentrated in vacuo to Chinese caterpillar fungus or erinaceus mycelium powder quality 10~50 times of the filtrate of step (2) gained, from Filter after the heart, by filtrate and glycerine in mass ratio 1:0.5~3 mixes, and final extract is obtained.
In some embodiments, the granularity of cordyceps mycelia powder is 40~100 mesh.
In some embodiments, the filtration in step (3) is to be processed using 0.22um filter membrane.
In some embodiments, the rotating speed of centrifugation is 6000~12000r/min.
Main advantages of the present invention are:
Amino acid is extracted from Chinese caterpillar fungus or its mycelium by this method, polysaccharide, adenosine mainly become with Chinese caterpillar funguses such as cordycepic acids Comprehensive recovery rate is divided to maintain higher level.In addition the method being provided using the present invention, not only increase in extract Chinese caterpillar fungus or The solubility of each active matter of its mycelium, and solve Cordyceps sinensis and its mycelia extract in refrigeration, heating process Separate out the FAQs of precipitation because activity concentration is too high, and in 4 DEG C, 25 DEG C of room temperature, 45 DEG C and subzero 18 DEG C of constant temperature shapes Can stablize more than 6 months under state, solution keeps clear, no precipitation and macroscopic foreign matter separate out, with cosmetics its The compatibility of his raw material is good, adds as raw material in suitable cosmetics.
Specific embodiment
Described below is the preferred embodiment of the present invention, and what the present invention was protected is not limited to the following side of being preferable to carry out Formula.It should be pointed out that for a person skilled in the art on the basis of this innovation and creation design, some deformation of making and Improve, broadly fall into protection scope of the present invention.
In the embodiment of the present invention, Cordyceps sinensis is obtained from commercially available.Mycelium is to be fermented by hair spore (Cs-C-Q80) by China Obtain with artificial culture.Realized by following condition in the embodiment of the present invention:
Experiment condition:After Cordyceps sinensis is extracted with water after pulverizing, residue alcohol and water mixed liquor carries out second extraction, extracts Liquid is through concentrating, centrifugation, filter after, by extract and the polyalcohol such as glycerine, 1,3-BDO, 1,2-PD or ethanol, second The mixing such as acid (adopts same material) in each embodiment, be statically placed in the environment of 45 DEG C, 4 DEG C, subzero 18 DEG C and 25 DEG C of room temperature Under, under the corresponding time period, whether the smell of observation extract, color change, pH value change and have the aspects such as material precipitation Judge the stability of extract.
Residue after extraction obtains its quality using freeze-drying, Cordyceps sinensis before extraction after quality difference value and winter used The ratio of worm summer grass original quality is worth to the recovery rate of extract.
Embodiment 1
(1) weigh 20.0g Cordyceps sinensis is dried and be crushed to 40 mesh, powder and water are 1 in mass ratio:20 ratio mixing, In 20 DEG C of water-baths, constant temperature stirring is filtered after extracting 30 minutes;
(2) after filtering, solid adds the glycerine of same step (1) aqueous phase homogenous quantities and the mixed liquor of water, permanent in 20 DEG C of water-baths Temperature stirring is filtered after extracting 30 clocks, merges the filtrate extracted twice, wherein glycerine and the volume ratio of water are 1:20;
(3) filter vacuum of (2) gained is concentrated into 10 times of Cordyceps sinensis powder quality, then through 6000r/min centrifugation Cross 0.22um filter membrane after 20 minutes to process, filtrate and glycerine are with 1:0.5 mass ratio mixing, obtains final Cordyceps sinensis and extracts Liquid.The effective component extraction rate of this embodiment is 83.61%, and extract is carried out stability experiment.Respectively use 1,2- butanediol, 1,3-BDO, 1,2- pentanediol replaces glycerine to carry out testing as a comparison, and it the results are shown in Table 1.
Table 1 stability experiment result
Embodiment 2
(1) weigh 20.0g Cordyceps sinensis is dried and be crushed to 100 mesh, powder and water are 1 in mass ratio:30 ratio mixing, In 100 DEG C of water-baths, constant temperature stirring is filtered after extracting 100 minutes;
(2) after filtering, solid adds the glycerine of same step (1) aqueous phase homogenous quantities and the mixed liquor of water, in 100 DEG C of water-baths Constant temperature stirring is filtered after extracting 100 clocks, merges the filtrate extracted twice, wherein glycerine and the volume ratio of water are 1:50;
(3) filter vacuum of (2) gained is concentrated into 50 times of Cordyceps sinensis powder quality, then through 12000r/min centrifugation Cross 0.22um filter membrane after 20 minutes to process, filtrate and glycerine are with 1:3 mass ratio mixing, obtains final cordyceps extracting liquid. The effective component extraction rate of this embodiment is 90.32%, and extract is carried out stability experiment.Respectively use 1,2- butanediol, 1, 3- butanediol, 1,2- pentanediol replaces glycerine to be tested, and as a comparison, it the results are shown in Table 2.
Table 2 stability experiment result
Embodiment 3
(1) weigh 20.0g Cordyceps sinensis is dried and be crushed to 60 mesh, powder and water are 1 in mass ratio:25 ratio mixing, In 80 DEG C of water-baths, constant temperature stirring is filtered after extracting 80 minutes;
(2) after filtering, solid adds the glycerine of same step (1) aqueous phase homogenous quantities and the mixed liquor of water, permanent in 80 DEG C of water-baths Temperature stirring is filtered after extracting 80 clocks, merges the filtrate extracted twice, wherein glycerine and the volume ratio of water are 1:30;
(3) filter vacuum of (2) gained is concentrated into 30 times of Cordyceps sinensis powder quality, then through 8000r/min centrifugation Cross 0.22um filter membrane after 20 minutes to process, filtrate and glycerine are with 1:1 mass ratio mixing, obtains final cordyceps extracting liquid. The effective component extraction rate of this embodiment is 92.08%, and extract is carried out stability experiment.Respectively use 1,2- butanediol, 1, 3- butanediol, 1,2- pentanediol replaces glycerine to be tested, and as a comparison, it the results are shown in Table 3.
Table 3 stability experiment result
Embodiment 4
(1) weigh 20.0g Cordyceps sinensis is dried and be crushed to 80 mesh, powder and water are 1 in mass ratio:28 ratio mixing, In 60 DEG C of water-baths, constant temperature stirring is filtered after extracting 60 minutes;
(2) after filtering, solid adds the glycerine of same step (1) aqueous phase homogenous quantities and the mixed liquor of water, permanent in 60 DEG C of water-baths Temperature stirring is filtered after extracting 60 clocks, merges the filtrate extracted twice, wherein glycerine and the volume ratio of water are 1:40;
(3) filter vacuum of (2) gained is concentrated into 40 times of Cordyceps sinensis quality, then is centrifuged 20 points through 10000r/min Cross 0.22um filter membrane after clock to process, filtrate and glycerine are with 1:2 mass ratio mixing, obtains final cordyceps extracting liquid.This is real The effective component extraction rate applying example is 89.66%, and extract is carried out stability experiment.Replaced with ethanol, acetone, acetic acid respectively Glycerine is tested, and as a comparison, it the results are shown in Table 4.
Table 4 stability experiment result
Embodiment 5
(1) weigh 20.0g cordyceps sinensis mycelium powder is dried and be broken to 50 mesh, powder and water are 1 in mass ratio:22 ratio Mixing, constant temperature stirring in 50 DEG C of water-baths is filtered after extracting 50 minutes;
(2) after filtering, solid adds the glycerine of same step (1) aqueous phase homogenous quantities and the mixed liquor of water, permanent in 50 DEG C of water-baths Temperature stirring is filtered after extracting 50 clocks, merges the filtrate extracted twice, wherein glycerine and the volume ratio of water are 1:25;
(3) filter vacuum of (2) gained is concentrated into 25 times of cordyceps sinensis mycelium powder end quality, then through 8000r/ Min crosses 0.22um filter membrane after being centrifuged 20 minutes and processes, and filtrate and glycerine are with 1:1.5 mass ratio mixing, obtains the final worm summer in winter Careless mycelia extract.The effective component extraction rate of this embodiment is 91.58%, and extract is carried out stability experiment.Respectively Glycerine is replaced to be tested with ethanol, acetone, acetic acid, it the results are shown in Table 5 as a comparison.
Table 5 stability experiment result

Claims (3)

1. a kind of extracting method of Cordyceps sinensis active matter used for cosmetic is it is characterised in that comprise the steps of:
(1) Cordyceps sinensis or cordyceps mycelia powder and water is 1 in mass ratio:20~30 ratio mixing, at 20~100 DEG C In water-bath, constant temperature stirring extraction was filtered after 30~100 minutes;
(2) after filtering, solid adds the glycerine of same step (1) aqueous phase homogenous quantities to be extracted with the mixed liquor of water, 20~100 In DEG C water-bath, constant temperature stirring extraction was filtered after 30~100 minutes, merged the filtrate extracted twice, wherein the volume ratio of glycerine and water For 1:20~50;
(3) by after through being concentrated in vacuo to Chinese caterpillar fungus or erinaceus mycelium powder quality 10~50 times of the filtrate of (2) gained, mistake after centrifugation Filter, by filtrate and glycerine in mass ratio 1:0.5~3 mixes, and final extract is obtained.
2. extracting method according to claim 1 it is characterised in that in step (1) Chinese caterpillar fungus or erinaceus mycelium powder granularity For 40~100 mesh.
3. extracting method according to claim 1 it is characterised in that step (3) in filter be using 0.22um filter membrane at Reason.
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TWI744668B (en) * 2019-07-19 2021-11-01 克一股份有限公司 Production method and application of rice protein extract extracted from cordyceps militaris ferment
CN113133951B (en) * 2020-01-19 2023-06-09 克一股份有限公司 Production method for extracting rice protein extract from cordyceps militaris fermentation product and application of rice protein extract
CN112656718A (en) * 2021-02-03 2021-04-16 现代百朗德生物科技(江苏)有限公司 Whitening mask containing cordyceps sinensis extract

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1189532A (en) * 1997-01-25 1998-08-05 杨国祥 Prodn. tech. of natural plant perfume for cigarette
JP2003292429A (en) * 2002-04-01 2003-10-15 Noevir Co Ltd Skin care preparation
CN102641235A (en) * 2012-05-18 2012-08-22 通德集团有限公司 Rhodiola crenulata essence with skin softening and anti-wrinkle effects

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1189532A (en) * 1997-01-25 1998-08-05 杨国祥 Prodn. tech. of natural plant perfume for cigarette
JP2003292429A (en) * 2002-04-01 2003-10-15 Noevir Co Ltd Skin care preparation
CN102641235A (en) * 2012-05-18 2012-08-22 通德集团有限公司 Rhodiola crenulata essence with skin softening and anti-wrinkle effects

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Denomination of invention: Method for extracting cosmetics used active matters from cordyceps sinensis

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Denomination of invention: A method for extracting active substance of Cordyceps sinensis for cosmetics

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