CN105963153A - Active composition containing copper peptide and cosmetic or skin care product - Google Patents

Active composition containing copper peptide and cosmetic or skin care product Download PDF

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Publication number
CN105963153A
CN105963153A CN201610566190.2A CN201610566190A CN105963153A CN 105963153 A CN105963153 A CN 105963153A CN 201610566190 A CN201610566190 A CN 201610566190A CN 105963153 A CN105963153 A CN 105963153A
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China
Prior art keywords
skin care
cosmetics
care item
copper peptides
emulsion
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CN201610566190.2A
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Chinese (zh)
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CN105963153B (en
Inventor
黄亚东
刘凌雪
项琪
肖巧学
何金莲
李德发
钟宇
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GUANGZHOU JIYUAN BIO-TECHNOLOGY Co Ltd
Medical And Biological Technology Research And Development Center Jinan Univ G
Guangzhou Realong Biological Technology Co Ltd
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GUANGZHOU JIYUAN BIO-TECHNOLOGY Co Ltd
Medical And Biological Technology Research And Development Center Jinan Univ G
Guangzhou Realong Biological Technology Co Ltd
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Priority to CN201610566190.2A priority Critical patent/CN105963153B/en
Publication of CN105963153A publication Critical patent/CN105963153A/en
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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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • A61K8/068Microemulsions
    • 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
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/368Carboxylic acids; Salts or anhydrides thereof with carboxyl groups directly bound to carbon atoms of aromatic rings
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/733Alginic acid; Salts thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • 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
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

Abstract

The invention discloses an active composition containing copper peptide and a cosmetic or skin care product. The active composition containing copper peptide is prepared from the following components in percentage by weight: 0.001-2 percent of copper peptide, 1-5 percent of vitamin E, 0.1-10 percent of chitin oligosaccharide, 0.1-2 percent of 4-MSK, 0.1-5 percent of algal polysaccharides, 6-30 percent of emulsifier, 0-10 percent of co-emulsifier, 0.1-0.8 percent of stabilizer, 0-10 percent of excipient and the balance of water. The active composition and the cosmetic or skin care product have the effects of promoting cell reproduction, remarkably moisturizing and moistening, delaying senescence and the like.

Description

Comprise the active compound of copper peptides and cosmetics or skin care item
Technical field
The invention belongs to cosmetic field, be specifically related to a kind of active compound comprising copper peptides and Cosmetics or skin care item.
Background technology
Aging is the degeneration change that body is respectively organized, organ dysfunction increases with the age and occurs, and is machine The general performance of the various biochemical reaction of body, is that the many factors such as inside and outside environmental pollution, psychentonia are total to The result of same-action.Aging is the inexorable law of life process, is inevitable, but slow down aging But it is possible.
Along with the raising of people's living standard, people also begin to after meeting basic clothing, food, lodging and transportion--basic necessities of life demand Pay close attention to the demand of the aspect such as attractive in appearance of other aspects especially body, appearance, wherein allow skin keep year The light thing that many people dream of especially.Today in development in science and technology, it is achieved probability Also improving, anti-aging cosmetics is the most increasingly paid close attention to by people.
Anti-aging cosmetics in the market is a feast for the eyes, very different, the most often there is many Problem.Such as, some product, because containing such as the unstable materials such as vitamin C, is difficult to long storage time, If changing the most in time, easily produce allergy;The most such as, some product because of containing can make thinning of skin, Injure tissue, make erythrosis, cause the side effect such as chemical burn fruit acid and can not be long-term Use.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of active compound comprising copper peptides and change Cosmetic or skin care item.The active compound of the present invention and cosmetics or skin care item have promotion cell proliferation And significantly replenishing water and preserving moisture and anti-ageing effect of waiting for a long time.
For achieving the above object, a first aspect of the present invention provides a kind of comprise copper peptides active group Compound, it includes each component of following percentage by weight: 0.001-2% copper peptides, 1-5% vitamin E, 0.1-10% chitin oligosaccharide, 0.1-2%4-MSK (4-methoxysalicylic acid potassium), 0.1-5% Sargassum polysaccharides, 6-30% emulsifying agent, 0-10% co-emulsifier, 0.1-0.8% stabilizer and 0-10% figuration Agent, surplus is water.
Preferably, described in comprise the active compound of copper peptides, it includes following percentage by weight Each component: 0.5-1.5% copper peptides, 2-4% vitamin E, 1-3% chitin oligosaccharide, 0.5-1.5%4-MSK, 1-3% Sargassum polysaccharides, 8-12% emulsifying agent, 1-2.5% co-emulsifier, 0.3-0.5% Stabilizer and 5-7% excipient, surplus is water.
Preferably, described emulsifying agent is octadecanoid acid and/or glyceryl monostearate.
Preferably, described co-emulsifier is glycerol.
Preferably, described stabilizer is lecithin or soybean lecithin.
Preferably, described excipient is mannose and/or lactose.
A second aspect of the present invention provides the lyophilizing of a kind of aforementioned active compound comprising copper peptides Emulsion or Spray dried products.
A third aspect of the present invention provides the lyophilizing of a kind of aforementioned active compound comprising copper peptides Emulsion or the preparation method of Spray dried products, described in comprise copper peptides active compound include as Each component of lower percentage by weight: 0.001-2% copper peptides, 1-5% vitamin E, 0.1-10% first Shell element oligosaccharide, 0.1-2%4-MSK, 0.1-5% Sargassum polysaccharides, 6-30% emulsifying agent, 0-10% help Emulsifying agent, 0.1-0.8% stabilizer and 0-10% excipient, surplus is water;
Described preparation method comprises the steps:
(1) by vitamin E, emulsifying agent, co-emulsifier and stabilizer mix homogeneously post-heating to complete CL, obtains oil phase;Copper peptides, chitin oligosaccharide, 4-MSK and Sargassum polysaccharides are mixed After be dissolved in water, obtain aqueous phase;
(2) under agitation aqueous phase is added drop-wise in oil phase, obtains emulsion mixture;
(3) gained emulsion mixture is processed through homogenizing, obtain the Asia of a diameter of 100-300nm Microemulsion;
(4) in gained submicron emulsion, add excipient, lyophilization or spray drying and prepare lyophilizing breast Agent or Spray dried products.
Preferably, described in step (1), mix homogeneously post-heating is to be heated to by fat-soluble ingredient 60~80 DEG C, the most also system is cooled to 30~40 DEG C, and with System is stirred by the stir speed (S.S.) of 10000-18000r/min, forms oil phase.
Preferably, described in step (2), the stir speed (S.S.) of stirring is 15000-20000r/min.
Preferably, homogenizing described in step (3) processes is to be carried out by high pressure Microfluidizer.
Preferably, described in step (4), cryodesiccated condition is: successively through-20 DEG C in freeze dryer Pre-freeze 120min ,-80 DEG C of pre-freeze 30min ,-55 DEG C of vacuum freezings, to being dried, obtain freeze-dried emulsion.
Preferably, described in step (4) be spray-dried condition be: feed rate be 2-5ml/min, It is spray-dried under the conditions of nozzle diameter 0.5-1mm, obtains Spray dried products.
A fourth aspect of the present invention provides a kind of cosmetics or skin care item, described cosmetics or skin care item bag Include freeze-dried emulsion or the Spray dried products of the aforementioned active compound comprising copper peptides.
Preferably, the preparation type of described cosmetics or skin care item is water preparation, cream, Emulsion, gel Agent or film former.
Preferably, in described cosmetics or skin care item, described in comprise the active compound of copper peptides The content of freeze-dried emulsion or Spray dried products is 0.1-30wt%, more preferably 10-20wt%.
Preferably, described cosmetics or skin care item also include alcohols, oil preparation, pH adjusting agent and antioxygen One or more in agent.
Preferably, one or more in ethanol, glycerol and 1,3 butylene glycol of described alcohols.
Preferably, described oil preparation one in fatty acid, higher alcohol, liquid paraffin and silicone oil or Multiple.
Preferably, described pH adjusting agent is citric acid-sodium citrate or lactic acid-sodium lactate.
Preferably, one or more in nicotiamide, riboflavin and nicotinic acid of described antioxidant.
Preferably, described cosmetics or skin care item also include can be used for being re-dubbed of cosmetics or skin care item Point, described in be re-dubbed be selected from metallothionein, L-ascorbic acid, chitin and derivant thereof, Chitosan, astaxanthin, HIRULOG, dicoumarol, acenocoumarol, Radix Notoginseng flavone, arasaponin With one or more in Aloe extract.
Preferably, described compounding composition accounts for described cosmetics or the 0.1%-20% of skin care item gross mass, More preferably 0.1%-10%.
The present invention achieves following beneficial effect:
1, the active compound that the present invention comprises copper peptides makes freeze-dried emulsion or Spray dried products, A diameter of 100-300nm, particle is evenly distributed, good stability, and more existing commercially available prod is easier to wear Transdermal, enters intracellular performance whitening skin and preserving moisture, toxin expelling and the effect of defying age.The research and development of the present invention Personnel experiments prove that the compositions of the present invention has promotion cell proliferation and significantly really Replenishing water and preserving moisture and the effect of defying age, be embodied in stimulation collagen and formed with elastin, tightly The effects such as real skin and minimizing microgroove, recovery skin repair ability, removing heavy metal.
2, the compositions of the present invention comprises 4-methoxysalicylic acid potassium (4-MSK), can activating skin Outer layer horny layer, and then strengthen the action and efficacy of the composition such as copper peptides, vitamin E, improve product Permeability.
3, the active targeting of the product utilization submicron emulsion of the present invention and passive targeting feature, more Fast and efficiently copper peptides etc. is had the effective ingredient moistened with repair and is delivered to target cell, Play targeting effectiveness.
4, the freeze-dried emulsion of the present invention or Spray dried products, its submicron emulsion structure considerably increases indigo plant The stability of the compositions such as the most oxidized, hydrolysis such as copper victory peptide, the stability of product the most of the present invention is better than With copper peptides and vitamin E be main pharmacodynamics composition general formulation such as cream agent, emulsion agent etc..
Accompanying drawing explanation
Fig. 1 (A) is shown that the molecular formula of copper peptides;Fig. 1 (B) is shown that copper peptides Molecular structure model.
Fig. 2 (A)-(D) is to moisten moisture-keeping efficacy in embodiment 6 to evaluate Visia skin of face imaging Result figure, wherein, Fig. 2 (A) be product use before, Fig. 2 (B) be product use after;Figure 2 (C) are before product uses, and Fig. 2 (D) is after product uses.
Fig. 3 is the knot of the product anteroposterior diameter severe edema due to hypofunction of the spleen shunting vector that experimenter uses the present invention in embodiment 7 Really comparison diagram, wherein, before left and right cheek block diagram is the most all followed successively by use, use 10d, Use 20d, use 30d and use the data of 40d.
Fig. 4 is the result pair of moisture content of skin before and after experimenter uses the product of the present invention in embodiment 7 Than figure, wherein, before left and right cheek and right and left eyes angle block diagram are the most all followed successively by use, use 10d, use 20d, use 30d and the data of use 40d.
Fig. 5 (A) and (B) are that in embodiment 7, white-skinned face function evaluates Visia skin of face imaging Result figure, wherein, Fig. 5 (A) is before product uses, and Fig. 5 (B) is after product uses.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with concrete real Execute example, and referring to the drawings, the present invention is described in further detail.
First aspect present invention provides a kind of active compound comprising copper peptides, and it includes following weight Each component of amount percentage ratio: 0.001-2% copper peptides, 1-5% vitamin E, 0.1-10% chitin Oligosaccharide, 0.1-2%4-MSK, 0.1-5% Sargassum polysaccharides, 6-30% emulsifying agent, 0-10% help emulsifying Agent, 0.1-0.8% stabilizer and 0-10% excipient, surplus is water.
Wherein, victory peptide also known as polypeptide or peptide, be simpler than protein structure, led to by 2-16 aminoacid Cross the small molecule compound that peptide is bonded.In human body, various physiological processes are nearly all by specifically The polypeptide of aminoacid sequence composition or protein regulation, and peptide is in biological growth, growth and metabolism In play an important role.In the natural aging and nursing process of skin, victory peptide plays an important role, Such as the synthesis of cell proliferation, inflammation, chromogenesis and albumen and regulation and control etc..Along with people are to self skin The further understanding of skin microstructure and mechanism, the victory peptide of various structures be introduced in skin nursing and then It is widely used in cosmetics and skin care item.
Described copper peptides is prior art term, wins peptide also known as copper, is abbreviated as GHK-Cu, its point Minor and structural model thereof are respectively as shown in Fig. 1 (A) and Fig. 1 (B), due to contained in its molecule Copper ion soluble in water in blue and gain the name.Copper peptides is considered as real meaning beauty treatment victory peptide First ancestor, finds that it is highly effective to treatment wound and skin injury the earliest.American Loren in 1973 Pickart is isolated one copper bond aminoacid GHK complex in human serum, i.e. GHK-Cu, It is a kind of by three aminoacid (Glycyl-Histidyl-Lysine) and copper ion (Copper) institute group The complex become.Thereafter it is found that GHK-Cu is expelled to wound surface not only can reduce cicatrix Tissue generates, moreover it is possible to stimulate skin self-heal.Additionally, research finds that GHK-Cu can promote nerve Tissue and angiogenesis, the growth of immunity-associated cell, divide and break up, promotes difference extracellular matrix The expression of component, and then wound healing can be effectively facilitated.Along with deepening continuously of research, copper peptides Start progress into the visual field of people and be applied in cosmetics and skin care item.
Chitin and chitosan is to be widely present in crustacean shell, insecticide shell and fungal cell wall In a class natural polysaccharide, preferably natural in deep-sea shrimp and Eriocheir sinensis, be application gene engineering extract High molecular cellulose.Due to unique material characteristic of " the two-way strong adsorption " of chitin, have Detoxicating, lock water, repair the effect such as impaired skin and allergy skin and be described as " the 6th life by science Key element ", the most also regarded as functional immune material by American-European Zhong government.
Described chitin oligosaccharide (chitooligosaccharides, COS) is to be gathered by chitin and shell A class low polymerization degree (n is typically at 2-20) water-soluble aminosaccharide that sugar produces after hydrolysis Compound, is the general name of chitin oligomer.COS relative molecular mass is less, gathers than macromole shell Sugar, chitin etc. are more easily absorbed by the skin, and with this cream made, frost class cosmetics can be by pore etc. Directly penetrate into inside skin, can effectively nurse one's health skin, play whitening and moisten effect.It was found that relatively divide The COS of protonatomic mass 1500~3000 has excellent water solublity, and its moisture absorption and moisture-retaining capacity are above shell Polysaccharide, sodium lactate, glycerol etc., and fungistatic effect is notable.
4-methoxysalicylic acid potassium (4-MSK) is the compound similar with salicylic acid structure, studies table Bright 4-MSK has the ability that correction Keratinocyte differentiation is unbalance, and for causing skin black Generation and release two aspects of element are respectively provided with protection effect, can be effectively improved the formation of mottle and freckle, For one of more remarkable whitening composition.
The present inventor is surprised to find that in R&D process: above-mentioned several active component are according to one Fixed ratio, is prepared as multiple for skin repair, the cosmetic of whitening skin and preserving moisture by adding other adjuvant Product preparation, definite ingredients, in addition to significant defying age, whitening skin and preserving moisture effect, be also equipped with wrinkle removal, Antiinflammatory, antioxidation, maintenance, the multiple efficacies such as skin of waking up, and safety have no adverse reaction, and have wide Market application foreground.Rear it has been investigated that, 4-MSK can activating skin outermost layer horny layer, Jin Erzeng The action and efficacy of the strong composition such as copper peptides, vitamin E, the permeability of raising product, and submicron emulsion There is the feature of active targeting and passive targeting, can be more fast and efficiently copper peptides It is delivered to target cell etc. having the effective ingredient moistened with repair, plays targeting effectiveness.
Preferably, described in comprise the active compound of copper peptides, it includes following percentage by weight Each component: 0.5-1.5% copper peptides, 2-4% vitamin E, 1-3% chitin oligosaccharide, 0.5-1.5%4-MSK, 1-3% Sargassum polysaccharides, 8-12% emulsifying agent, 1-2.5% co-emulsifier, 0.3-0.5% Stabilizer and 5-7% excipient, surplus is water.
Preferably, described emulsifying agent is octadecanoid acid and/or glyceryl monostearate.
Preferably, described co-emulsifier is glycerol.
Preferably, described stabilizer is lecithin or soybean lecithin.
Preferably, described excipient is mannose and/or lactose.
A second aspect of the present invention provides the lyophilizing of a kind of aforementioned active compound comprising copper peptides Emulsion or Spray dried products.
A third aspect of the present invention provides the lyophilizing of a kind of aforementioned active compound comprising copper peptides Emulsion or the preparation method of Spray dried products, described in comprise copper peptides active compound include as Each component of lower percentage by weight: 0.001-2% copper peptides, 1-5% vitamin E, 0.1-10% first Shell element oligosaccharide, 0.1-2%4-MSK, 0.1-5% Sargassum polysaccharides, 6-30% emulsifying agent, 0-10% help Emulsifying agent, 0.1-0.8% stabilizer and 0-10% excipient, surplus is water;
Described preparation method comprises the steps:
(1) by vitamin E, emulsifying agent, co-emulsifier and stabilizer mix homogeneously post-heating to complete CL, obtains oil phase;Copper peptides, chitin oligosaccharide, 4-MSK and Sargassum polysaccharides are mixed After be dissolved in water, obtain aqueous phase;
(2) under agitation aqueous phase is added drop-wise in oil phase, obtains emulsion mixture;
(3) gained emulsion mixture is processed through homogenizing, obtain the Asia of a diameter of 100-300nm Microemulsion;
(4) in gained submicron emulsion, add excipient, lyophilization or spray drying and prepare lyophilizing breast Agent or Spray dried products.
Wherein, when co-emulsifier content and excipient content are 0, in step (1) and (4) Save addition co-emulsifier and the operation of excipient accordingly.Preferably, mix described in step (1) Uniformly post-heating is fat-soluble ingredient to be heated to 60~80 DEG C, the most also by body System is cooled to 30~40 DEG C, and system is stirred with the stir speed (S.S.) of 10000-18000r/min, Form oil phase.
Preferably, described in step (2), the stir speed (S.S.) of stirring is 15000-20000r/min.
Preferably, homogenizing described in step (3) processes is to be carried out by high pressure Microfluidizer.
Preferably, described in step (4), cryodesiccated condition is: successively through-20 DEG C in freeze dryer Pre-freeze 120min ,-80 DEG C of pre-freeze 30min ,-55 DEG C of vacuum freezings, to being dried, obtain freeze-dried emulsion.
Preferably, described in step (4) be spray-dried condition be: feed rate be 2-5ml/min, It is spray-dried under the conditions of nozzle diameter 0.5-1mm, obtains Spray dried products.
A fourth aspect of the present invention provides a kind of cosmetics or skin care item, described cosmetics or skin care item bag Include freeze-dried emulsion or the Spray dried products of the aforementioned active compound comprising copper peptides.
Preferably, the preparation type of described cosmetics or skin care item is water preparation, cream, Emulsion, gel Agent or film former.
Preferably, in described cosmetics or skin care item, described in comprise the active compound of copper peptides The content of freeze-dried emulsion or Spray dried products is 0.1-30wt%, more preferably 10-20wt%.
Preferably, described cosmetics or skin care item also include alcohols, oil preparation, pH adjusting agent and antioxygen One or more in agent.
Preferably, one or more in ethanol, glycerol and 1,3 butylene glycol of described alcohols.
Preferably, described oil preparation one in fatty acid, higher alcohol, liquid paraffin and silicone oil or Multiple.
Preferably, described pH adjusting agent is citric acid-sodium citrate or lactic acid-sodium lactate.
Preferably, one or more in nicotiamide, riboflavin and nicotinic acid of described antioxidant.
Preferably, described cosmetics or skin care item also include can be used for being re-dubbed of cosmetics or skin care item Point, described in be re-dubbed be selected from metallothionein, L-ascorbic acid, chitin and derivant thereof, Chitosan, astaxanthin, HIRULOG, dicoumarol, acenocoumarol, Radix Notoginseng flavone, arasaponin With one or more in Aloe extract.
Preferably, described compounding composition accounts for described cosmetics or the 0.1%-20% of skin care item gross mass, More preferably 0.1%-10%.
Specific embodiment is presented herein below, and the most if no special instructions, reagent used is city Sell the reagent of analytical pure rank.
Prepared by 1 one kinds of freeze-dried emulsions comprising copper peptides active compound of embodiment
1, the percentage by weight of each component is as shown in table 1:
Table 1 comprises each component of the freeze-dried emulsion of copper peptides active compound
Composition Content (%)
Copper peptides 1
Vitamin E 3
Chitin oligosaccharide 2
Sargassum polysaccharides 2
4-MSK 1
Glycerol 2.5
Glyceryl monostearate 2
Octadecanoid acid 8
Mannitol 5
Lecithin 0.5
Ultra-pure water Surplus
2, the preparation method of freeze-dried emulsion:
(1) by fat such as vitamin E, glycerol, glyceryl monostearate, octadecanoid acid and lecithin Soluble components Hybrid Heating to 70 DEG C, is cooled to 35 DEG C and in stir speed (S.S.) is after being completely dissolved Oil phase is formed under the conditions of 10000-18000r/min;By copper peptides, chitin oligosaccharide, 4-MSK It is dissolved in water after mixing with Sargassum polysaccharides, obtains aqueous phase;(2) in 15000-20000r/min stir speed (S.S.) Lower aqueous phase is added drop-wise in oil phase, obtains O/W type emulsion mixture;
(3), after gained emulsion mixture being processed by high pressure Microfluidizer homogenizing, obtain straight Footpath size is the submicron emulsion of 100-300nm;
(4) in gained submicron emulsion add mannitol, in freeze dryer in-20 DEG C of pre-freeze 120min ,-80 DEG C After pre-freeze 30min, again through-55 DEG C of vacuum lyophilizations, obtain freeze-dried emulsion.
Prepared by 2 one kinds of Spray dried products comprising copper peptides active compound of embodiment
1, the percentage by weight of each component is as shown in table 2:
Table 2 comprises each component of the Spray dried products of copper peptides active compound
Composition Content (%)
Copper peptides 1
Vitamin E 3
Chitin oligosaccharide 2
Sargassum polysaccharides 2
4-MSK 1
Glycerol 2.5
Glyceryl monostearate 2
Octadecanoid acid 8
Lecithin 0.5
Ultra-pure water Surplus
2, the preparation method of Spray dried products:
(1) by fat such as vitamin E, glycerol, glyceryl monostearate, octadecanoid acid and lecithin Soluble components Hybrid Heating to 70 DEG C, is cooled to 35 DEG C and in stir speed (S.S.) is after being completely dissolved Oil phase is formed under the conditions of 10000-18000r/min;By copper peptides, chitin oligosaccharide, 4-MSK It is dissolved in water after mixing with Sargassum polysaccharides, obtains aqueous phase;
(2) under 15000-20000r/min stir speed (S.S.), aqueous phase is added drop-wise in oil phase, obtains O/W Type emulsion mixture;
(3), after gained emulsion mixture being processed by high pressure Microfluidizer homogenizing, obtain straight Footpath size is the submicron emulsion of 100-300nm;
(4) by gained submicron emulsion feed rate be 2-5ml/min, nozzle diameter 0.5-1mm condition Under be spray-dried, obtain Spray dried products.
Embodiment 3 one kinds comprises the astringent of copper peptides active compound
1, the percentage by weight of each composition is as shown in table 3:
The percentage by weight of each composition of table 3 astringent
Composition Content (%)
Embodiment 1 or 2 product 20
Epigallocatechin gallate (EGCG) 0.15
Lactic acid 0.1
Sodium lactate 0.3
Ethanol 10
Sorbitol 5
Glycerol 1
Methyl hydroxybenzoate 0.1
Distilled water Surplus
2, preparation method: epigallocatechin gallate (EGCG) is dissolved according to formula ratio in table 3 Ethanol is made alcohol mixed solution;Embodiment 1 obtained freeze-drying Emulsion or embodiment 2 gained are sprayed Desciccate is sequentially added into Sorbitol, lactic acid, sodium lactate, nipalgin after dissolving with appropriate distilled water Methyl ester and glycerol, add above-mentioned alcohol mixed solution, stir after mix homogeneously, supplements residue double Steam water and get final product.
Embodiment 4 one kinds comprises emollient cream of copper peptides active compound
1, the percentage by weight of each composition is as shown in table 4:
The percentage by weight of each composition of table 4 emollient cream
2, preparation method: according to formula ratio in table 4 by isopropyl palmitate, octadecanol, titanium dioxide Titanium, propolis, Parleam, methyl hydroxybenzoate and ethyl hydroxybenzoate mix after being heated to 70 DEG C, As oil phase;By embodiment 1 obtained freeze-drying Emulsion or embodiment 2 gained Spray dried products, nicotinoyl Amine and collagen protein dissolve with appropriate distilled water, add oil phase after supplementing residue distilled water mix homogeneously, Stir and get final product.In final emollient cream product, the percentage by weight of each composition is shown in Table 4.
Embodiment 5 comprises the active compound of the copper peptides proliferation function to promoting application on human skin epidermis cell
By be in exponential phase Hacat cell (Hacat cell be purchased from Wuhan University's Chinese Typical Representative Culture collection center, CCTCC) with containing 10%FBS, (FBS is purchased from Hangzhou Ilex purpurea Hassk.[I.chinensis Sims biology work Journey Materials Co., Ltd) DMEM culture medium (DMEM culture medium be purchased from Gibco company of the U.S.) Cellar culture converges to 80%-90%, uses 0.25% trypsinization, with 1 × 105The cell number of individual/ml Mesh is inoculated in 96 orifice plates, after cultivating 24h, changes plasma-free DMEM medium and cultivates, will after 24h The embodiment 1 that concentration is 100,50,25,12.5,6.25 μ g/mL it is separately added into after culture medium sucking-off And the submicron emulsion prepared by embodiment 2, each concentration sets 3 multiple holes, and blank group is six multiple holes. Put into incubator after administration to continue to cultivate 24h, add 10 μ l MTT (0.5mg/ml), in incubator After hatching 4h, solution add 150 μ l DMSO, after vibration under 570nm wavelength in sucking-off hole Detection absorbance OD value.
Cell proliferation rate %=(administration group OD value/blank group OD value-1) × 100%, result It is shown in Table 5.
Table 5 Hacat cell proliferation rate (%) (n=3,)
Note: administration group compares with Normal group significant difference p < 0.05.
As shown in Table 5, embodiment 1,2 product is 6.25-100 μ g/mL in administration concentration In the range of Hacat cell all had had significant proliferation effect, and there is certain concentration dependent;I.e. with The increase of administration concentration, its cell proliferation rate increases the most therewith.
Embodiment 6 comprises the moisture-keeping efficacy evaluation of the freeze-dried emulsion of copper peptides active compound
Recipient site test can not use any product (cosmetics or topical drug) for first 2 days~3 days, 1h~3h can not contact water.Before experiment, experimenter needs unification clear water to clean face.Clean method For by dry medicated napkin wiped clean.
Experimenter face test zone is bilateral cheek (nose and the intersection point of outer canthus) and the bilateral corners of the mouth At outer 2cm.Pilot region area at least 3cm × 3cm, should be standard compliant before official testing Sit quietly in room at least 20min, it is impossible to drinks water and beverage, keeps light state.Period operator's meeting Carry out exchanging and fill in skin evaluation and test table with regard to subjects skin's situation with experimenter.Reality is carried out after 30min Test front skin test (skin moisture content, percutaneous water loss amount, it is thus achieved that initial basis value), survey Examination terminates the rear same day according to product requirement uniform application product, and 7,14,28 days after smearing pay a return visit Carry out corresponding skin test, and carry out tested before and after compare.
Visia dermal imaging shows, the situation using skin peeling after embodiment 1 product to fall bits substantially changes Kind, skin rubefaction situation also makes moderate progress, and result is shown in Fig. 2 (A)-(D).
Before and after using experimenter, skin is analyzed (being shown in Table 6), and result display uses lyophilized powder After, As time goes on, being dried of skin, peel, play the integrations such as bits and red blood streak and become in declining Gesture, symptom significantly improves (p < 0.01).Moist degree, smoothness, skin pliability, skin are tight Cause degree and skin transparent feel all have lifting in various degree, wherein with moist degree the most substantially (p < 0.05).
Table 6 skin evaluation (n=33,)
It is dried Decortication Play bits Red blood streak
Before using 3.60±0.40 1.60±0.68 2.40±0.51 1.40±0.24
Use latter 7 days 2.20±0.37 0.60±0.40 1.40±0.24 1.40±0.24
Use latter 14 days 2.40±0.24 0.80±0.49 1.80±0.58 1.40±0.40
Use latter 28 days 1.20±0.20 0.20±0.20 1.20±0.20 1.20±0.20
From Fig. 2 (A)-(D) and the experimental result of table 6, copper peptides lyophilized powder is to being dried Property skin there is significant moisturizing and skin barrier function repairing effect, it is possible to promote skin significantly Cutin moisture, reduces percutaneous water loss amount, makes the moist degree of skin, glossiness increase, skin The lifting of skin moisture makes skin it is thus possible to break away from dry, pruritus, the symptom of decortication.
Embodiment 7 comprises the senile-resistant efficacy evaluation of the Spray dried products of copper peptides active compound
Meet into set condition experimenter temperature be 20 DEG C~22 DEG C, humidity be the survey of 40%~60% Test ring border carries out real-time dynamic monitoring.Recipient site test can not use any product in first 2 days~3 days Product (cosmetics or topical drug), 1h~3h can not contact water.Before experiment, experimenter is unified with clear Water cleaning face (clean method is by dry medicated napkin wiped clean), is meeting mark before official testing Sit quietly in accurate room (temperature: 20 DEG C~22 DEG C, humidity: 40%~60%) at least 20min, Do not drink water and beverage.Experimenter face test zone is experiment septum reset left and right cheek, the corners of the mouth, canthus And the region such as forehead.Pilot region area at least 3cm × 3cm.
Experiment starts first to measure the blank value of 30min after facial cleansing, then press product requirement consumption, Use step, embodiment 2 product is spread evenly across face.In use 10d after product, 20d, 30d, 40d pay a return visit and carry out face shots and detection through the severe edema due to hypofunction of the spleen with VISIA face-image analyser The shunting index such as vector, skin elasticity.
Finding the detection of experimenter's percutaneous water loss amount, change over time uses skin after product Water loss rate presents downward trend, the total percutaneous water loss recorded for the 20th, 30 days after using Measure, compared with before use product, there is statistical significance (p < 0.05).The lower petition of surrender of percutaneous water loss amount Bright skin barrier function obtains and recovers to a certain extent, and lock water function promotes, and strengthens the moisturizing of dry skin Effect, concrete outcome is shown in Fig. 3.In figure 3, percutaneous water loss amount unit is g/h/m2(n=9,), wherein, * p < 0.05, * * p < 0.01 compared with before use.Test result indicate that, use The moisture of skin can be effectively improved before and after embodiment 2 product for skin, there is significantly guarantor Wet function.
To subjects skin's elastomeric check find: its R2 value (without the springback capacity of skin during negative pressure with have The ratio of maximum tension amount during negative pressure, ratio is more bordering on 1, illustrates that elasticity is the best) change is reflected in survey In the examination cycle, Experimental Area skin elasticity increases in time, and its R2 value increases the most therewith, specifically ties Fruit sees Fig. 4 and Fig. 5 (A)-(B).In the diagram, moisture content of skin unit be U (n=9,), Wherein, * p < 0.05, * * p < 0.01 compared with before use.Test result indicate that, use embodiment 2 Before and after product, skin elasticity substantially increases, and the product of the present invention has significant anti-senescence function.
It should be noted that aforementioned preferably embodiment is carry out as a example by astringent and emollient cream Illustrate, but technical scheme is applicable to cosmetics and the skin care item of all conventionally forms, and It is not limited with detailed description of the invention enumerated supra.
Separately, the present invention has also carried out other serial experiments, such as stability test comparative experiments, experiment knot Fruit shows that the stability of product of the present invention is better than with copper peptides and vitamin E for main pharmacodynamics composition General formulation such as cream agent, emulsion agent etc..
Particular embodiments described above, is carried out the purpose of the present invention, technical scheme and beneficial effect Further describe it should be understood that the foregoing is only the specific embodiment of the present invention, Be not limited to the present invention, all within the spirit and principles in the present invention, any amendment of being made, Equivalent, improvement etc., should be included within the scope of the present invention.

Claims (13)

1. the active compound comprising copper peptides, it is characterised in that include following weight hundred Each component of proportion by subtraction: 0.001-2% copper peptides, 1-5% vitamin E, 0.1-10% chitin are oligomeric Sugar, 0.1-2%4-MSK, 0.1-5% Sargassum polysaccharides, 6-30% emulsifying agent, 0-10% co-emulsifier, 0.1-0.8% stabilizer and 0-10% excipient, surplus is water.
The active compound comprising copper peptides the most according to claim 1, it is characterised in that Each component including following percentage by weight: 0.5-1.5% copper peptides, 2-4% vitamin E, 1-3% Chitin oligosaccharide, 0.5-1.5%4-MSK, 1-3% Sargassum polysaccharides, 8-12% emulsifying agent, 1-2.5% Co-emulsifier, 0.3-0.5% stabilizer and 5-7% excipient, surplus is water.
The active compound comprising copper peptides the most according to claim 1 and 2, its feature Being, described emulsifying agent is octadecanoid acid and/or glyceryl monostearate;And/or,
Described co-emulsifier is glycerol;And/or,
Described stabilizer is lecithin or soybean lecithin;And/or,
Described excipient is mannose and/or lactose.
The freeze-dried emulsion of the active compound comprising copper peptides the most according to claim 1 or Spray dried products.
5. the freeze-dried emulsion of the active compound comprising copper peptides as claimed in claim 4 Or the preparation method of Spray dried products, it is characterised in that described in comprise the active component of copper peptides Thing includes each component of following percentage by weight: 0.001-2% copper peptides, 1-5% vitamin E, 0.1-10% chitin oligosaccharide, 0.1-2%4-MSK, 0.1-5% Sargassum polysaccharides, 6-30% emulsifying agent, 0-10% co-emulsifier, 0.1-0.8% stabilizer and 0-10% excipient, surplus is water;
Described preparation method comprises the steps:
(1) by vitamin E, emulsifying agent, co-emulsifier and stabilizer mix homogeneously post-heating to complete CL, obtains oil phase;Copper peptides, chitin oligosaccharide, 4-MSK and Sargassum polysaccharides are mixed After be dissolved in water, obtain aqueous phase;
(2) under agitation aqueous phase is added drop-wise in oil phase, obtains emulsion mixture;
(3) gained emulsion mixture is processed through homogenizing, obtain the Asia of a diameter of 100-300nm Microemulsion;
(4) in gained submicron emulsion, add excipient, lyophilization or spray drying and prepare lyophilizing breast Agent or Spray dried products.
Preparation method the most according to claim 5, it is characterised in that
Mix homogeneously post-heating described in step (1) is fat-soluble ingredient to be heated to 60~80 DEG C, more The most also system is cooled to 30~40 DEG C, and stirring with 10000-18000r/min Mix speed system to be stirred, form oil phase;And/or,
Described in step (2), the stir speed (S.S.) of stirring is 15000-20000r/min;And/or,
It is to be carried out by high pressure Microfluidizer that homogenizing described in step (3) processes;And/or,
Described in step (4), cryodesiccated condition is: successively through-20 DEG C of pre-freezes in freeze dryer 120min ,-80 DEG C of pre-freeze 30min ,-55 DEG C of vacuum freezings, to being dried, obtain freeze-dried emulsion;
The condition being spray-dried described in step (4) is: be 2-5ml/min, nozzle at feed rate It is spray-dried under the conditions of bore 0.5-1mm, obtains Spray dried products.
7. cosmetics or skin care item, it is characterised in that described cosmetics or skin care item include as The freeze-dried emulsion of the active compound comprising copper peptides described in claim 4 or Spray dried products.
Cosmetics the most according to claim 7 or skin care item, it is characterised in that described cosmetic The preparation type of product or skin care item is water preparation, cream, Emulsion, gel or film former.
Cosmetics the most according to claim 7 or skin care item, it is characterised in that described cosmetic In product or skin care item, described in comprise copper peptides active compound freeze-dried emulsion or be spray-dried produce The content of thing is 0.1-30wt%, more preferably 10-20wt%.
10. according to the cosmetics described in any one of claim 7-9 or skin care item, it is characterised in that Described cosmetics or skin care item also include the one in alcohols, oil preparation, pH adjusting agent and antioxidant Or it is multiple.
11. cosmetics according to claim 10 or skin care item, it is characterised in that
One or more in ethanol, glycerol and 1,3 butylene glycol of described alcohols;And/or,
One or more in fatty acid, higher alcohol, liquid paraffin and silicone oil of described oil preparation;With / or,
Described pH adjusting agent is citric acid-sodium citrate or lactic acid-sodium lactate;And/or,
One or more in nicotiamide, riboflavin and nicotinic acid of described antioxidant.
12. according to the cosmetics described in any one of claim 7-9 or skin care item, it is characterised in that Described cosmetics or skin care item also include the compounding composition that can be used for cosmetics or skin care item, described compounding Composition is selected from metallothionein, L-ascorbic acid, chitin and derivant thereof, chitosan, shrimp green grass or young crops Element, HIRULOG, dicoumarol, acenocoumarol, Radix Notoginseng flavone, arasaponin and Aloe extract In one or more.
13. cosmetics according to claim 12 or skin care item, it is characterised in that described multiple It is made into and point accounts for described cosmetics or the 0.1%-20% of skin care item gross mass, more preferably 0.1%-10%.
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