CN109498515A - It is a kind of have effects that repair extracts of pinus koraiensis and its application - Google Patents
It is a kind of have effects that repair extracts of pinus koraiensis and its application Download PDFInfo
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- CN109498515A CN109498515A CN201811576851.5A CN201811576851A CN109498515A CN 109498515 A CN109498515 A CN 109498515A CN 201811576851 A CN201811576851 A CN 201811576851A CN 109498515 A CN109498515 A CN 109498515A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
- A61K8/9755—Gymnosperms [Coniferophyta]
- A61K8/9767—Pinaceae [Pine family], e.g. pine or cedar
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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Abstract
The invention discloses a kind of extracts of pinus koraiensis for having effects that repair and its applications.Korean pine seed extracting method of the invention includes drying, crushing, enzymatic hydrolysis, Microwave Extraction, suction filtration, rotary evaporation.Short with extraction time, extraction efficiency is high, utmostly retains thermal activity ingredient, and yield is high, and extracts the advantages of will not destroying the molecular structure of Korean pine seed.Korean pine seed extract produced by the present invention can effectively facilitate wound healing, hence it is evident that mitigate pain, can significantly reduce the incidence of inflammation and itch, be applied in cosmetics, have the effects that moisturize, repair, is anti-radiation, moisturizing.
Description
Technical field
The present invention relates to cosmetic fields, more particularly to a kind of extracts of pinus koraiensis for having effects that repair and its application.
Background technique
Korean pine (PinuskoraiensisSieb.etZucc.) it is main product in the rare tree in the Chinese Xiaoxinanlin Mountains.Korean pine
Seed be commonly called as Korean pine seed also known as Luo Songzi, korean pine seed, Pinus koraiensis etc..Just there is " korean pine seed temperature stomach in " Haiyao Bencao, Oversea Materia Medica " of the Tang Dynasty
Intestines, long term usage are made light of one's life by commiting suicide, and are promoted longevity " record.Ming Dynasty's Li Shizhen (1518-1593 A.D.) once gave very high evaluation to the medicinal of pine nut, he is in " book on Chinese herbal medicine
Detailed outline " in write: " korean pine seed, releases a Xin Luo pine nut, and smell is sweet small nontoxic;Joint wind is cured mainly, it is dizzy, remove dead flesh, bleach, dissipating
Aqueous vapor, moisturizing viscera, by wandering arthritis cold air, empty thin few gas tonifying for the deficiency, fertile the five internal organs dissipate all wind, wet stomach, and long term usage body is light, and macrobiosis is not
Always." modern study surface, containing there are many physiological activators of great Development volue, such as vitamin A, dimension life in Korean pine kernel
Plain E and a variety of unsaturated fatty acids needed by human, phosphatide, sterol, polysaccharide, flavones etc., it is edible or for functional food
Product, by ancient Chinese medicine doctor, the high praise of nutritionist.In people mind, pine nut is considered as " Longevity ", is the reason of the middle-aged and the old
Think the desirable material of health food and ladies' moistening skin beautifying.
However, less to application study of the Korean pine seed extract in cosmetics at present, there has been no relevant reports.The present invention
Inventor by a large amount of research and test, a kind of Korean pine seed extract for having effects that well to repair as a result has been made, from
And complete the present invention.
Summary of the invention
The purpose of the present invention is to provide a kind of Korean pine seed extracts, and are applied in cosmetics, play good
Repair.
A kind of preparation method of Korean pine seed extract, comprising the following steps:
(1) Korean pine seed dry, pulverize to the Korean pine powder of seeds that is sieved to obtain;
(2) Korean pine powder of seeds is taken, the sodium acetate-acetic acid buffer solution of pH4.0~5.5 is added, cellulase is added, carries out enzyme
Solution, obtains enzymolysis liquid;
(3) dehydrated alcohol is added into enzymolysis liquid, microwave-assisted extraction is carried out in microwave reactor, obtains extracting solution;
(4) extracting solution is filtered, filtrate rotary evaporation is removed into ethyl alcohol to get Korean pine seed extract;
The vigor that wherein step (2) digests cellulase used is 40-60U/mg, and dosage is by Korean pine seed powder: cellulase is
The ratio of 1g:100U.
In wherein some embodiments, drying described in step (1) be in baking oven 60 DEG C drying to constant weight, the mistake
Sieve was the sieving of 40-80 mesh.
In wherein some embodiments, the amount that buffer solution is added described in step (2) is 2-3 times of Korean pine seed weight,
The enzymatic hydrolysis is 1~2h of enzymatic hydrolysis in 50~60 DEG C of water-bath.
In wherein some embodiments, after dehydrated alcohol is added in step (3), in system the volume fraction of ethyl alcohol be 60~
80%.
In wherein some embodiments, Microwave Extraction condition in step (3) is microwave power 2-2.2KW/kg, at microwave
The reason time is 8~10min.
Another object of the present invention is to provide application of the Korean pine seed extract in cosmetics.
Korean pine seed extract of the present invention can be used as cosmetics and repair effect adding ingredient, be applied in cosmetics.
The dosage of the Korean pine seed extract, is calculated by mass percentage, and additive amount accounts for the 1-10wt% of cosmetics gross mass.Institute
The cosmetics stated can be the different dosage forms such as cream, lotion, facial mask, lipstick, toner.
A kind of lip-protecting lipstick containing above-mentioned Korean pine seed extract, is grouped as by the group of following mass percentage:
Tridecanol trimellitate 5-15%,
Hydrogenated rosins acid methyl esters 1-10%,
Double more -2 1-10% of acyl group adipate ester of-two glycerol,
Octyl dodecanol 5-20%,
Hydrogenated palm kernel oil 1-10%,
Polyethylene 1-5%,
Ceresine 1-3%,
Butyrospermum parkii (BUTYROSPERMUM PARKII) fruit rouge 0.1-3%,
Cera alba 0.1-3%,
Small candle sets (EUPHORBIA CERIFERA) wax 0.1-3%,
C12-15 alcohol benzoic ether 1-10%,
Microwax 0.1-3%,
Acrylic acid (ester) class/polydimethylsiloxanecopolymer copolymer 0.1-1%,
Ring five dimethyl silicone polymer 0.1-3%,
Pungent glycol 0.1-3%,
Titanium dioxide 0.1-1%,
Iron oxides 0.1-1%,
Mica 0.1-1%,
Korean pine seed extract 1-10% of the present invention,
Ethylhexyl palmitate surplus.
The present invention has the advantage that and the utility model has the advantages that
1. Korean pine seed extracting method of the present invention compares existing physical squeezing method (common law and spiral method) and extraction method
(water substitution), has the advantage that
(1) extraction time is short, and extraction efficiency is high, utmostly retains thermal activity ingredient, and the relatively existing water substitution of yield
It is higher;
(2) present invention is used and is first digested, then carries out Microwave Extraction to raw material, and on the one hand enzymatic hydrolysis can be starch and other biological matter
Etc. macromoleculars be converted to small molecule, be conducive to subsequent dissolution, another aspect microwave condition can substantially eliminate enzyme to extraction
The influence of Korean pine seed increases final Korean pine seed and extracts yield;And the molecular structure that will not destroy Korean pine seed is extracted, for red
The stability and functional characteristic of pine nut extract finished product have good protective effect.
2. the Korean pine seed extract that extracting method of the present invention obtains is applied in cosmetics, opened up as functional additive is repaired
Wide its use scope, Korean pine seed extract can effectively facilitate wound healing, hence it is evident that mitigate pain, can significantly reduce inflammation and scabies
The incidence itched, is applied in cosmetics, has the effects that moisturize, repairs, is anti-radiation, moisturizing.
3. and Korean pine seed is dual-purpose of drug and food medicinal material, be applied to cosmetics, safety it is guaranteed.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention will be made into one below
Step ground detailed description, embodiments of the present invention are not limited thereto, for not specifically specified technological parameter or condition, can refer to
Routine techniques carries out.
The cosmetics Chinese name of Korean pine seed extract of the present invention are as follows: Korean pine (PINUS KORAIENSIS) seed extracts
Object.
Embodiment 1
A kind of Korean pine seed extract chooses Korean pine seed as raw material, extracts to obtain by following steps:
(1) being placed in baking oven 60 DEG C drying to constant weight Korean pine seed dry, pulverize 40 meshes and obtains Korean pine powder of seeds;
(2) Korean pine powder of seeds is taken, the sodium acetate-acetic acid buffer solution of the pH4.0 of 3 times of Korean pine seed weight is added, cellulose is added
Enzyme digests 1h in 60 DEG C of water-bath, obtains enzymolysis liquid;
(3) dehydrated alcohol is added, so that the volume fraction of ethyl alcohol is 80% in system, carries out microwave-assisted leaching in microwave reactor
It mentions, microwave power 2KW/kg, microwave treatment time 10min obtains extracting solution;
(4) extracting solution is filtered, filtrate rotary evaporation removes ethyl alcohol to get Korean pine seed extract, yield 58.2%;
The vigor of cellulase used in above-mentioned enzymatic hydrolysis is 40U/mg, and dosage presses Korean pine seed powder: cellulase is the ratio of 1g:100U
Example calculates.
Embodiment 2
A kind of Korean pine seed extract chooses Korean pine seed as raw material, extracts to obtain by following steps:
(1) being placed in baking oven 60 DEG C drying to constant weight Korean pine seed dry, pulverize 80 meshes and obtains Korean pine powder of seeds;
(2) Korean pine powder of seeds is taken, the sodium acetate-acetic acid buffer solution of the pH5.5 of 2 times of Korean pine seed weight is added, cellulose is added
Enzyme digests 2h in 50 DEG C of water-bath, obtains enzymolysis liquid;
(3) dehydrated alcohol is added, so that the volume fraction of ethyl alcohol is 60% in system, carries out microwave-assisted leaching in microwave reactor
It mentions, microwave power 2.2KW/kg, microwave treatment time 8min obtains extracting solution;
(4) extracting solution is filtered, filtrate rotary evaporation removes ethyl alcohol to get Korean pine seed extract, yield 60.4%;
The vigor of cellulase used in above-mentioned enzymatic hydrolysis is 60U/mg, and dosage presses Korean pine seed powder: cellulase is the ratio of 1g:100U
Example calculates.
Embodiment 3
A kind of Korean pine seed extract chooses Korean pine seed as raw material, extracts to obtain by following steps:
(1) being placed in baking oven 60 DEG C drying to constant weight Korean pine seed dry, pulverize 60 meshes and obtains Korean pine powder of seeds;
(2) Korean pine powder of seeds is taken, the sodium acetate-acetic acid buffer solution of the pH5.0 of 2 times of Korean pine seed weight is added, cellulose is added
Enzyme digests 1h in 55 DEG C of water-bath, obtains enzymolysis liquid;
(3) dehydrated alcohol is added, so that the volume fraction of ethyl alcohol is 70% in system, carries out microwave-assisted leaching in microwave reactor
It mentions, microwave power 2.1KW/kg, microwave treatment time 9min obtains extracting solution;
(4) extracting solution is filtered, filtrate rotary evaporation removes ethyl alcohol to get Korean pine seed extract, yield 64.6%;
The vigor of cellulase used in above-mentioned enzymatic hydrolysis is 50U/mg, and dosage presses Korean pine seed powder: cellulase is the ratio of 1g:100U
Example calculates.
Comparative example 1
A kind of Korean pine seed extract chooses Korean pine seed as raw material, extracts to obtain by following steps:
1) by Korean pine seed, drying to constant weight in 60 DEG C of baking ovens, and 60 mesh are sieved to obtain Korean pine powder of seeds after crushing;
2) Korean pine powder of seeds 100g is taken, dehydrated alcohol is added, makes the volume fraction 70% of ethyl alcohol in system, adjusts microwave power
2.1KW/kg, the Microwave Extraction 9min in microwave reactor, obtains extracting solution;
3) extracting solution is filtered, filtrate rotary evaporation removes ethyl alcohol to get Korean pine seed extract;
This comparative example is 34.7% without enzymolysis step yield.
Comparative example 2
A kind of Korean pine seed extract chooses Korean pine seed as raw material, extracts to obtain by following steps:
The Korean pine powder of seeds 100g after grinding is accurately weighed, a certain proportion of water is added, adjustment solid-liquid ratio is 1:7.5g/ml, is mentioned
The extraction conditions of pH value 9,70 DEG C of Extracting temperature are taken, extraction time 2h is centrifuged 15min under the conditions of 4000r/min, sucks emulsification
Layer and water layer are dried under vacuum to constant weight under the conditions of 40 DEG C, this comparative example is extracted using water substitution, yield 50.4%.
Test 1 pair of Sjogren syndrome model mice salivary gland intervention effect test
Material: DPT vaccine is purchased from Beijing Tiantan Biological Products Co.ltd, lot number: 2018060402;Freund is complete
Adjuvant: SigmaUSA, lot number: 018k0619-81-2;Bioengineering Research Institute is built up in Coomassie brilliant blue kit, Nanjing, batch
Number: 20180618;Trizl:Invitrgen, USA, lot number: 0382739.
Animal selection: BALB/C mice 120, SPF grades, female, weight 20g or so.Purchased from Medical University Of Chongqing's reality
Test animal center
Experimental method
Animal is randomly divided into totally 5 groups, every group 30 by grouping.Blank control group, prednisone group, embodiment 1-3 group.Take 36 it is same
Mouse is planted, takes salivary gland under aseptic condition, after homogenate, 2171 μ g/ml of antigen concentration is measured, PBS buffer solution is added to be diluted to 1000 μ
G/ml, is added same volume Freund's complete adjuvant, and final concentration is 500 μ g/ml, every back of mice multi-point injection antigen, total amount
Only for 1ml/.Dorsal injection DPT vaccine 0.5ml simultaneously generates the salivary gland change similar to mankind SS and clinical manifestation spy
Point, starts to give that basic, normal, high dose delivery example 1-3 group is extract obtained, prednisone treats SS mouse for Yu Zaomo the 2nd day.
Any drug is not given in blank control group, daily normal raising, and embodiment group animal is low dose group (17gkg- 1·d- 1),
Middle dose group (34gkg- 1·d- 1), high dose group (68gkg- 1·d- 1), prednisone group gives prednisone 0.32mg/d filling
Stomach puts to death mouse and carries out evaluating drug effect after 4 weeks.
Saliva measures fixed: the cotton balls that dry weight is 5mg is made in sterile rayon balls, is put into the rear cheek of mouse, 5min
After take out, weigh on electronic balance.
Salivary secretion amount (mg)=cotton balls weight in wet base-cotton balls dry weight.
Each group mouse salivary changes in flow rate is relatively shown in Table 1.
Salivary flow compares and (is averaged) mg after 1 modeling of table 4 weeks
There is leaching in Korean pine seed extract low, middle and high dose groups obtained by embodiment 1-3 and prednisone group mouse submandibular gland salivary gland tissues
Bar cellular infiltration illustrates that Korean pine seed extract that Korean pine seed extracting method of the present invention obtains has and moisturizes effect.
Embodiment 4
The lip-protecting lipstick 1-3 and comparative example 3-4 formed as shown in table 2 is prepared, is grouped as by the group of following mass percentage:
Table 2
Test 2 crowds test on probation
Crowd's inclusion criteria: lip appearance dries up or even peels or cracking, cutis laxa, cheilogramma increase, the shrivelled dull nothing of lip color
Light, corners of the mouth cracking.
According to above crowd's inclusion criteria, case 250 are selected.Male 90, female 160;Age is average at 18~55 years old
34.8 years old, it is divided into 5 groups at random, every group of 50 people.
Application method: embodiment group applies sample made from lip-protecting lipstick 1-3 of the present invention, 1 day each 1 time sooner or later, smears every time
Uniform lip;Contrast groups apply sample made from comparative example 3-4.
Observation method: observing curative effect after two weeks, and lip is compact, and cheilogramma disappears, and lip color is ruddy glossy, and decortication disappears, nothing
Cracking is healing;Lip is compact, and cheilogramma is reduced, and the shrivelled decrease of lip color becomes ruddy, and decortication is reduced, and cracks gradually healing to have
Effect;Unchanged or exacerbation is invalid.
The results are shown in Table 3:
Table 3
The data recorded by table 3 are it is found that the lip-protecting lipstick 1-3 smearing affected part that the present invention is prepared, is used after two weeks, all shown
Effective out, cure rate is up to 60% or more (33/50*100%).Pair that Korean pine seed extract is made in enzymolysis processing is not carried out with addition
Ratio 3 and addition are compared using the comparative example 4 that Korean pine seed is made in water substitution, and cure rate is higher.
It is reacted according to subject, it is safe and non-stimulating using lip-protecting lipstick of the present invention, it has no adverse reaction, is that lip can be moistened,
Smooth fine lines can effectively facilitate lip wound healing, hence it is evident that improve the symptoms such as the shrivelled dimness of lip color, allow lip to become ruddy, dry and wet
Appropriateness, lubrication has light, old and young all to can be used;Especially there is the trier of lip inflammation, is used lip-protecting lipstick of the present invention two weeks
Afterwards, inflammation is also cured.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (9)
1. a kind of Korean pine seed extracting method, which comprises the following steps:
(1) Korean pine seed dry, pulverize to the Korean pine powder of seeds that is sieved to obtain;
(2) Korean pine powder of seeds is taken, the sodium acetate-acetic acid buffer solution of pH4.0~5.5 is added, cellulase is added, is digested
Obtain enzymolysis liquid;
(3) dehydrated alcohol is added, microwave-assisted extraction is carried out in microwave reactor, obtains extracting solution;
(4) extracting solution is filtered, filtrate rotary evaporation removes ethyl alcohol to get Korean pine seed extract;
The vigor that wherein step (2) digests the cellulase is 40-60U/mg, and dosage is by Korean pine seed powder: cellulase is
The ratio of 1g:100U calculates.
2. Korean pine seed extracting method according to claim 1, which is characterized in that drying described in step (1) is in baking
In case 60 DEG C drying to constant weight, it is described sieving be 40-80 mesh sieving.
3. Korean pine seed extracting method according to claim 1, which is characterized in that buffer solution is added described in (2) in step
Amount be 2-3 times of Korean pine seed weight, the enzymatic hydrolysis is 1~2h of enzymatic hydrolysis in 50~60 DEG C of water-bath.
4. Korean pine seed extracting method according to claim 1, which is characterized in that after dehydrated alcohol is added in step (3), body
The volume fraction of ethyl alcohol is 60~80% in system.
5. Korean pine seed extracting method according to claim 1, which is characterized in that the Microwave Extraction condition in step (3) is
Microwave power 2-2.2KW/kg, microwave treatment time are 8~10min.
6. the Korean pine seed extract that Korean pine seed extracting method according to claim 1-5 obtains.
7. application of the Korean pine seed extract according to claim 6 in cosmetics, which is characterized in that Korean pine seed extract
Dosage, be calculated by mass percentage, additive amount accounts for the 1-10wt% of cosmetics gross mass.
8. application according to claim 7, which is characterized in that the cosmetics are cream, lotion, facial mask, lipstick, makeup
Water.
9. a kind of lip-protecting lipstick containing Korean pine seed extract as claimed in claim 6, which is characterized in that by following quality hundred
The group of point content is grouped as:
Tridecanol trimellitate 5-15%,
Hydrogenated rosins acid methyl esters 1-10%,
Double more -2 1-10% of acyl group adipate ester of-two glycerol,
Octyl dodecanol 5-20%,
Hydrogenated palm kernel oil 1-10%,
Polyethylene 1-5%,
Ceresine 1-3%,
Butyrospermum parkii (BUTYROSPERMUM PARKII) fruit rouge 0.1-3%,
Cera alba 0.1-3%,
Small candle sets (EUPHORBIA CERIFERA) wax 0.1-3%,
C12-15 alcohol benzoic ether 1-10%,
Microwax 0.1-3%,
Acrylic acid (ester) class/polydimethylsiloxanecopolymer copolymer 0.1-1%,
Ring five dimethyl silicone polymer 0.1-3%,
Pungent glycol 0.1-3%,
Titanium dioxide 0.1-1%,
Iron oxides 0.1-1%,
Mica 0.1-1%,
Korean pine seed extract 1-10% as claimed in claim 6,
Ethylhexyl palmitate surplus.
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Application publication date: 20190322 |