CN107184427A - A kind of cooperative compositions and application containing polyglutamic acid and hyaluronic acid - Google Patents
A kind of cooperative compositions and application containing polyglutamic acid and hyaluronic acid Download PDFInfo
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- CN107184427A CN107184427A CN201710250848.3A CN201710250848A CN107184427A CN 107184427 A CN107184427 A CN 107184427A CN 201710250848 A CN201710250848 A CN 201710250848A CN 107184427 A CN107184427 A CN 107184427A
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/88—Polyamides
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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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/20—Halogens; Compounds thereof
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- A—HUMAN NECESSITIES
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- 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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/23—Sulfur; Selenium; Tellurium; Compounds thereof
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- A—HUMAN NECESSITIES
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- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
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- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
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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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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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- 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
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Abstract
The invention discloses a kind of cooperative compositions containing polyglutamic acid and hyaluronic acid and application, the composition includes the composition of following parts by weight：5 30 parts of hyaluronic acid, 1 10 parts of polyglutamic acid, 1 20 parts of compound；The compound includes recombined human hyaluronidase（PH20）, sodium chloride, calcium chloride, magnesium sulfate.Hyaluronic acid by the invention has anti-inflammatory bacteriostatic activity and moisturizing repair；Polyglutamic acid：With superpower moisture-retaining capacity, adsorptivity, biodegradability；Compound has safe and efficient percutaneous absorbability；Therefore this composition has more preferable moisturizing, antibacterial and excellent percutaneous permeability, and a variety of cooperative effects can rationally prevent and solve skin problem, make the more beautiful health of skin.
Description
Technical field
The present invention relates to skin care applications, more particularly to a kind of cooperative compositions containing polyglutamic acid and hyaluronic acid
And the preparation method of various formulations.
Background technology
It is reported that, polyglutamic acid (γ-PGA) is a kind of water-soluble, biodegradable, use microbial fermentation without toxicity
Boiomacromolecule made from method, it is a kind of sticking material, is found first in " natto ".γ-PGA are a kind of special
The natural polymer of anion, be using the glutamic acid of left and right optical activity as cell cube, through acyl between alpha-amido and γ-carboxyl
The homotype polyamide polypeptide that amine key knot is constituted, γ-PGA molecular weight is from 5 ten thousand to 2 megadaltons.Special molecule
Structure, makes it have extremely strong moisture-retaining capacity, can effectively increase the moisture-retaining capacity of skin, promotes skin health, its is superpower
Moisture-retaining capacity is better than common moisturizing ingredient, is the biotechnology NMF of a new generation.γ-PGA also have superpower simultaneously
Adsorptivity and biodegradability, catabolite are non-harmful glutamic acid, are a kind of excellent environment-friendly type macromolecule materials, can
As water-loss reducer, adsorbent for heavy metal, flocculant, sustained release agent and pharmaceutical carrier etc., in cosmetics, food, medicine etc.
Industry has very big commercial value and social value.
Modern medicine study shows that human flora's imbalance, pathogenic bacteria grow, and can cause endocrine dysfunction, in vivo poison
Element increases and can not discharged in time, and be inflamed reaction with skin surface in vivo, so that the toxin expelling burden of skin has been aggravated, when
Between it is long will endanger the function of skin, skin is unable to eupnea and metabolism, will form chloasma, acne, and skin will
Dry, lack moisture and oil, it is intense darkness without light.The hyaluronic acid of activation is without anaphylaxis by common hyaluronic acid using safety
The shearing of recombined human hyaluronidase, then by a special processing technology processing after, form activation segment, become magical
Almost " guaranteeing to cure mucocutaneous all kinds of diseases and ailments " bioactive materials.Inflammation is source of ten thousand diseases, is also the main of beauty and aging
Reason, the hyaluronic acid after activation is combined with extracellular CD44 and TLR4 acceptors, can promote mucocutaneous secretion defensin 2,
Promote mucocutaneous secretion functional component, and then suppress the inflammatory stimulus effect of inflammation and anti-endotoxin, strengthen cutaneous immunisation
The effect of power, makes skin beauty health.The recombined human hyaluronidase used simultaneously in the hyaluronic acid technique of production activation
Itself it is safe and efficient penetrating agent, it can digest the hyaluronic acid in skin, the viscosity of cytoplasm is reduced, so that temporarily
Skin barrier is opened, makes the direct rapid osmotic of nutriment to dermal layer of the skin and accelerates to spread and absorb, with efficiently oozing
Saturating absorbability, can quickly repair skin.Hyaluronic acid after activation enters after the skin corium of human body skin, makes skin and other
The hyaluronic acid synthetic quantity increase of tissue, so that the water retention property increase of skin, improves skin growth condition, be dermal collagen
The synthesis of albumen and elastomer provides superior external environment condition, it is recovered original smooth and elasticity, repairs skin sparing
Barrier, helps skin preservation moisture and nutrition, and then play effect of moisturizing reparation.
Composition containing hyaluronic acid after polyglutamic acid and activation is using it moisturizing, anti-inflammatory be antibacterial and excellent skin
Infiltrative a variety of cooperative effects can rationally prevent and solve skin problem, make the more beautiful health of skin.The synergistic combination
The health and beauty care product of for oral administration or external application, including but not limited to mouth can be made further by adding related matrix or auxiliary material in thing
Take liquid, pulvis, tablet, capsule, facial mask, lotion, emulsion, frost, cream, gel.
The content of the invention
The technical problem to be solved in the present invention be overcome the deficiencies in the prior art there is provided it is a kind of both had more preferable moisturizing,
The cooperative compositions containing polyglutamic acid and hyaluronic acid of antibacterial and excellent percutaneous permeability and the preparation method of various formulations.
In order to solve the above technical problems, the present invention is provided：
A kind of cooperative compositions containing polyglutamic acid and hyaluronic acid, it is characterised in that：The composition includes following weight
Measure the composition of part：5-30 parts of hyaluronic acid, 1-10 parts of polyglutamic acid, 1-20 parts of compound；It is saturating that the compound includes recombined human
The sour enzyme (PH20) of bright matter, sodium chloride, calcium chloride, magnesium sulfate.
The compound includes recombined human hyaluronidase (PH20), sodium chloride, calcium chloride, magnesium sulfate, each Ingredients Weight
Than for 1~2:130~160:1.5~2.5:0.5~1.0.
The compound includes recombined human hyaluronidase (PH20), sodium chloride, calcium chloride, magnesium sulfate, each Ingredients Weight
Than for 1:100:2:1.
Hyaluronic acid, polyglutamic acid, compound weight ratio are 10:5：11.
Hyaluronic acid has anti-inflammatory bacteriostatic activity and moisturizing repair after activation by the invention；Polyglutamic acid：Tool
There are superpower moisture-retaining capacity, adsorptivity, biodegradability；Enzyme of the compound comprising enzymolysis hyaluronic acid and enzymolysis environment institute
The ion needed, while the recombined human hyaluronidase used in the hyaluronic acid technique of production activation is safe and efficient in itself
Penetrating agent, it can digest the hyaluronic acid in skin, reduce the viscosity of cytoplasm, so as to temporarily open skin barrier, make
The direct rapid osmotic of nutriment is to dermal layer of the skin and accelerates to spread and absorbs, can be fast with efficient osmotic absorption
Speed repairs skin；Therefore this composition has more preferable moisturizing, anti-inflammatory antibacterial and excellent percutaneous permeability, a variety of collaboration work(
Effect can rationally prevent and solve skin problem, make the more beautiful health of skin.
Embodiment
In order to illustrate that effect and component ratio of hyaluronic acid toothpaste of the invention are properly lifted following examples and done further
Explanation.
(1) synergistic combination composition formula (part by weight)
Originally cooperative compositions composition and weight ratio containing polyglutamic acid and hyaluronic acid are：5-30 parts of hyaluronic acid, poly- paddy
1-10 parts of propylhomoserin, compound, 1-20 parts；Compound includes recombined human hyaluronidase (PH20), sodium chloride, calcium chloride, sulfuric acid
Magnesium.Various dosage form products are can be prepared by said composition addition auxiliary material.In the composition plus deionized water be made contain polyglutamic acid
With the cooperative compositions solution of hyaluronic acid.
(2) effect of each composition
Hyaluronic acid after activation：With anti-inflammatory bacteriostatic activity and moisturizing repair；
Polyglutamic acid：With superpower moisture-retaining capacity, adsorptivity, biodegradability；
Compound：Compound is made up of recombined human hyaluronidase (PH20), sodium chloride, calcium chloride, magnesium sulfate, each composition
Match as 1~2:130~160:1.5~2.5:0.5~1.0, optimum weight ratio is 1:100:2:1, while in production activation
The recombined human hyaluronidase used in hyaluronic acid technique is safe and efficient penetrating agent in itself, and it can be digested in skin
Hyaluronic acid, reduces the viscosity of cytoplasm, so as to temporarily open skin barrier, makes the direct rapid osmotic of nutriment to skin
Skin corium is simultaneously accelerated to spread and absorbed, and with efficient osmotic absorption, can quickly repair skin；
It is prepared by composition solution：Take hyaluronic acid and compound in the range of weight ratio be dissolved at 35-40 DEG C 50g go from
In sub- water, 1000-3000r/min stirring digestion 3-4h adjust pH5.0-5.6, add polyglutamic acid, plus deionized water is to 100 mixed
Close uniform, save backup.
Matrix auxiliary material：For the production of the formulations such as oral liquid, pulvis, tablet, capsule, facial mask, lotion, emulsion, frost, cream, gel
Product figuration and other effects.
(3) Efficacy experiments
First, bacteriostatic experiment
Take Clinical isolation Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans a little, connect respectively
Kind in broth bouillon, in cultivating 18h at 37 DEG C.(calf serum that 20% is added in Pseudomonas aeruginosa broth bouillon) takes
Each bacterial strain nutrient broth culture of 18h cultures, being made into bacteria suspension is used to test.Sterilizing test tubes 11, the 1st are taken respectively
Branch adds nutrient broth fluid nutrient medium 9ml, and 2-10 branch adds 5ml, and the 11st addition 10ml, separately sampled product contain polyglutamic
Acid and the cooperative compositions solution 1ml of hyaluronic acid add the 1st test tube, it is well mixed after take 5ml to add the 2nd, it is dilute successively
Release to the 10th, the 11st is not added with sample as control.Often pipe is cultivated at a temperature of adding escherichia coli suspension 0.1ml, 37 DEG C
24h, takes out observation bacterial growth situation.Staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans grow with above-mentioned Germicidal efficacy
Situation.As test tube becomes cloudy, that is, bacterial growth is represented, sample is without bacteriostasis；If test tube is limpid represent bacterial growth by
Suppress.As shown in table 2, cooperative compositions solution of the present invention is to Clinical isolation Escherichia coli, golden yellow grape for experimental result
Coccus, Pseudomonas aeruginosa, Candida albicans have stronger bacteriostasis.
The bacteriostatic experiment each sample composition of table 1 is constituted
| Hyaluronic acid | Polyglutamic acid | Compound | Deionized water | |
| Sample one | 1.0% | 0.5% | 1.1% | To 100 |
| Sample two | 1.0% | — | 1.1% | To 100 |
| Sample three | 1.0% | 0.5% | — | To 100 |
| Sample four | — | 0.5% | — | To 100 |
Last limpid test tube numbering in each sample of table 2 correspondence bacteriostatic test
| Escherichia coli | Staphylococcus aureus | Pseudomonas aeruginosa | Candida albicans | |
| Sample one | 6 | 5 | 5 | 5 |
| Sample two | 4 | 3 | 3 | 3 |
| Sample three | - | - | - | - |
| Sample four | - | - | - | - |
By above-mentioned limpid broth tubes and control group transferred species broth agar plates after diluting according to a certain percentage, observation
24h, the Cmin of no bacterial growth is bacteriocidal concentration, is designated as C, and unit is mg/mL, as a result as shown in table 3, illustrates this hair
Bright cooperative compositions solution has to Clinical isolation Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans
Stronger bactericidal action；Simultaneously by contrast it can be seen that the inventive composition solution has synergy at antibacterial aspect.
The sterilization conditions of 3 embodiment of table one
| C (Escherichia coli) | C (staphylococcus aureus) | C (Pseudomonas aeruginosa) | C (Candida albicans) | |
| Sample one | 0.07 | 0.14 | 0.12 | 0.18 |
| Sample two | 0.36 | 0.65 | 0.62 | 0.71 |
| Sample three | — | — | — | — |
| Sample four | — | — | — | — |
| Control group | — | — | — | — |
Note："-" indicates no bactericidal properties.
2nd, the compound prescription of cooperative compositions is studied
The biologically active human of cooperative compositions solution, i.e. anti-inflammatory bacteriostatic activity are now detected using the method for human experimentation,
Cooperative compositions solution is studied to prevent and treat disease of skin.
All experimenters of this experiment are different degrees of disease of skin patient, and experimental group 1 is answered using polyglutamic acid 0.5%+
Smeared 1 time before being slept every night with the composition solution of thing 1.1%+ hyaluronic acids 1.0%；Experimental group 2 is saturating using polyglutamic acid 0.5%+
Sour 1.0% composition solution of bright matter is smeared 1 time before sleeping every night；Experimental group 3 uses 1.0% group of compound 1.1%+ hyaluronic acids
Polymer solution is smeared 1 time before sleeping every night；Positive control is smeared 1 time before being slept every night using 1.0% hyaluronic acid solution；Negative control
Smeared 1 time before being slept every night using physiological saline；Comparing symptom after five groups of treatments 7 days improves situation.
The symptom therapeutic evaluatioies such as dermal sensation discomfort, allergy, inflammation, peculiar smell, spot：
It is effective：Symptom is significantly improved or disappeared, patient satisfaction；Effectively：Symptom has improvement or mitigated, and patient still has discomfort,
It is required that continual cure；It is invalid：Symptom is unsatisfied with without obvious mitigation, patient.
Statistical method：Statistical procedures are carried out using SPSS12.0 statistics softwares, compared between metering and enumeration data group
Relatively examined using t and x2 is examined, with p<0.05 is statistically significant difference.
As a result it is as follows：
As shown in table 4, the 8th day symptom improves situation：Experimental group 1 effective 10, total effective rate 100%；Experimental group 2 shows
Effect 0, effective 5, invalid 5, total effective rate 50%, obvious effective rate is compared P with experimental group 1<0.01；Experimental group 3 effective 6,
Effective 4, total effective rate 100%, obvious effective rate is compared P with experimental group 1<0.01；Effective 0 of positive control is effective 2, invalid
8, total effective rate 20%, obvious effective rate is compared P with experimental group 1<0.01.
The 8th day each group patient symptom of table 4 improves situation and is compared as follows：
| Group | Sample number | It is effective | Effectively | It is invalid | Total effective rate (%) |
| Experimental group 1 | 10 | 10 | 0 | 0 | 100 |
| Experimental group 2 | 10 | 0 | 5 | 5 | 50 |
| Experimental group 3 | 10 | 6 | 4 | 0 | 100 |
| Positive control | 10 | 0 | 2 | 8 | 20 |
| Negative control | 10 | 0 | 0 | 10 | 0 |
Conclusion：
Experimental group 1 (polyglutamic acid 0.5%+ compound 1.1%+ hyaluronic acids 1.0%) is substantially than the (polyglutamic of experimental group 2
Sour 0.5%+ hyaluronic acids 1.0%), experimental group 3 (compound 1.1%+ hyaluronic acids 1.0%), positive control it is effective.This hair
Bright human experimentation shows the composition solution of (1) polyglutamic acid, compound and hyaluronic acid three composition to prevention and treatment
Disease of skin is evident in efficacy；(2) polyglutamic acid to the hyaluronic acid after activation prevention and treatment disease of skin curative effect in terms of
There is obvious synergy.
3rd, the optimum proportioning of cooperative compositions compound prescription is studied
Method：Manufacture 0.1%, 0.5%, 1.0% polyglutamic acid and 0.5%, 1.1%, 2.0% compound and
0.5%th, the cooperative compositions solution other compositions of 1.0%, 2.5% hyaluronic acid compound prescription are deionized water, Suo Youcheng
Divide percentage by weight summation 100%.All experimenters of this experiment are different degrees of disease of skin patient, test the poly- paddy of 1-30
The cooperative compositions solution of propylhomoserin, compound and hyaluronic acid various concentrations smears 1 progress Three factors-levels before sleeping every night
Orthogonal experiment；Positive control 28-30 is respectively adopted before 0.5%, 1.0%, 2.5% hyaluronic acid solution is slept every night and smears 1
It is secondary, the situation after observation treatment；31 be that 1 prevention and treatment skin disease is smeared before negative control is slept every night using physiological saline
Disease, the situation after observation treatment；Every group of 5 patients, comparison therapy symptom improvement situation after 7 days.
The orthogonal experiment factor meter of table 5：
The symptom the standard of curative effect evaluation such as dermal sensation discomfort, allergy, inflammation, peculiar smell, spot are ibid.
Statistical method：Statistical procedures are carried out using SPSS12.0 statistics softwares, compared between metering and enumeration data group
Relatively examined using t and x2 is examined, with p<0.05 is statistically significant difference.
The 8th day each group patient symptom of table 6 improves situation and is compared as follows：
Conclusion：
Through human body using test, as a result show using 0.1%, 0.5%, 1.0% polyglutamic acid and 0.5%, 1.1%,
The cooperative compositions solution of 2.0% compound and 0.5%, 1.0%, 2.5% hyaluronic acid per distribution ratio is to disease of skin
There is prevention and treatment effect, but do not limit to this scope.
4th, percutaneous absorbability is tested
The mouse skin cuticula handled well is fixed on Franz diffusion cells upwards according to Transdermal Absorption experiment, connect
30% ethanol-physiological saline is added in receives pond, is placed in the intelligent penetrating absorption instrument of water bath with thermostatic control, design temperature (37.0 ±
0.5) DEG C, rotating speed 200rmin-1.1h is balanced, sample is added after draining the bubble in reception tank.On diffusion cell supply area
Be uniformly coated with sample 1g, every group parallel 3 times, respectively 0,0.1,0.3,0.5,1.0,2.0,4.0,6.0,8.0,10.0,12.0
When draw reception liquid 1mL, and fill into the reception liquid of equality of temperature same volume.The reception liquid of absorption adds test tube after filtering, then accurately
Add 2mLCTAB test solutions, from add when timing, gently vibrate rock enough long-times, during which trying one's best avoids reaction solution from producing
Raw foam, is stood to close to 10min, then pours into reaction solution in 1cm cuvettes, and wavelength is determined during 10min in 400nm
Absorbance (A400), the transdermal absorption factor of hyaluronic acid is obtained according to the standard curve of hyaluronic acid at that wavelength.
The each sample composition of table 7 composition situation is as follows
| Hyaluronic acid | Polyglutamic acid | Compound | Deionized water | |
| Sample one | 1.0% | 0.5% | 1.1% | To 100 |
| Sample two | 1.0% | 0.5% | — | To 100 |
| Sample three | 1.0% | — | 1.1% | To 100 |
| Control group | 1.0% | — | — | To 100 |
Note："-" represents to be not added with.
Conclusion：Using hyaluronic acid transdermal absorption factor as ordinate, the time (t) is abscissa, draws the transdermal suction of hyaluronic acid
Yield-time graph, the absorptivity for as a result showing hyaluronic acid in 12h is the ＞ control groups of one ＞ samples of sample, three ＞ samples two,
Show that hyaluronic acid compositions are remarkably improved the transdermal absorption factor of hyaluronic acid；As a result show 0.5h inner skins to hyaluronic acid
Absorption it is most fast, cooperative compositions is most obvious to the effect of the transdermal absorption factor of hyaluronic acid in 0.5h.
4th, moisture retention is tested
(man 5, female 15 by the men and women 20 without disease of skin that experimental selection can be influenceed by result of the test completely
Name) tested for object, to test the moistening effect of cooperative compositions.Specific method is as follows：Each experimental subjects is in sample
Before, first with behind water cleaning experiment position, then adapt to external environment condition 30 minutes.The environmental condition of experiment is：Keep indoor temperature 22-
24 DEG C, indoor humidity 45-50%, and tested in same place.Each 10ul of sample is smeared with 2*2cm2 in inboard arm, and
Dry 1 minute.Then respectively coat 20ul ultra-pure water again at the position of smearing, with 1 point be interval (0 with after towel moisture
Minute, 1 minute, 2 minutes, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes), use
The each skin surface moisture for smearing position of 825 couples of Corneometer CM is measured moistening effect.Measurement result such as table 8
Shown, unit is Corneometer value (Cv).
The each sample composition of table 8 composition situation is as follows
| Hyaluronic acid | Polyglutamic acid | Compound | Deionized water | |
| Sample one | 1.0% | 0.5% | 1.1% | To 100 |
| Sample two | 1.0% | 0.5% | — | To 100 |
| Sample three | 1.0% | — | 1.1% | To 100 |
| Sample four | — | 0.5% | 1.1% | To 100 |
| Control group one | 1.0% | — | — | To 100 |
| Control group two | — | 0.5% | — | To 100 |
| Control group three | — | — | 1.1% | To 100 |
The each sample moistening effect measurement result of table 9
| 0 point | 2 | 4 | 6 | 8 | 10 | |
| Sample one | 190.5 | 92.6 | 78.3 | 72.5 | 68.2 | 67.5 |
| Sample two | 170.6 | 79.8 | 69.3 | 55.5 | 53.9 | 53.1 |
| Sample three | 175.8 | 84.5 | 72.3 | 58.9 | 56.7 | 55.4 |
| Sample four | 167.3 | 79.8 | 66.9 | 57.4 | 52.3 | 52.0 |
| Control group one | 160.9 | 72.9 | 62.5 | 53.4 | 51.2 | 49.5 |
| Control group two | 164.8 | 75.4 | 62.7 | 54.9 | 51.8 | 48.9 |
| Control group three | 144.4 | 60.6 | 51.5 | 43.9 | 42.1 | 40.5 |
Cooperative compositions of the present invention, which is can be seen that, from upper table measurement result contrasts single polyglutamic acid, hyaluronic acid guarantor
Wet effect is more longlasting, illustrates that the polyglutamic acid in said composition and the hyaluronic acid after activation have brilliance on moistening effect
Synergy.5th, acute oral toxicity is tested
According to test basis《Disinfection technology standard》(defend method prison hair in the 3.4 of (third edition) first fascicle experimental technique specification
[1999] No. 448).By animal (regular grade NIH mouse 20, male and female half and half, 18~22g of body weight) water supply fasting 12 hours,
Distilled water is solvent, and tested material (uses weight ratio for 1:0.5：1.1 hyaluronic acid, polyglutamic acid, compound deionization are water-soluble
Liquid) dosage is set as 5500mg/kg, tested material is once filled to animal with gavage syringe needle by 0.2ml/20g body weight.After administration immediately
The poisoning manifestations, death toll and death time of animal are observed and recorded, observe secondary daily, two weeks observation periods.According to acute poison
Property grade scale carry out toxicity grading.Experimental result：In observation period, test mice does not occur manifest symptom, no dead generation.
The tested material of table 10 is to NIH chmice acute Oral toxicity result of the tests
| Sex | Dosage (mg/kg) | Number of animals (only) | Death toll (only) | The death rate (%) |
| It is female | 5500 | 10 | 0 | 0 |
| It is male | 5500 | 10 | 0 | 0 |
Conclusion：Cooperative compositions of the present invention is to the acute through LD50 ＞ 5000mg/kg, the true nontoxic level in border of NIH mouse.
6th, vaginal mucosa stimulation test
Press《Disinfection technology standard》(third edition) first fascicle《Experimental technique specification》The 3.5th in (Ministry of Public Health, 2012.4)
Carry out.Healthy White Rabbit 12 is chosen, is divided into experimental group 8, excipient group 2 and blank control group 2.Experimental group：It will apply
There is cooperative compositions test specimen of the present invention (to use weight ratio for 1:0.5：1.1 hyaluronic acid, polyglutamic acid, compound are gone
Deionized water solution) the roundlet sliver of 2.0cm length insert experimental animal intravaginal, every kind of each 2 of sample；Excipient group：With same
The sliver of sample size is soaked with sterile saline, inserts animal intravaginal；Blank group：Do not process.Sliver is removed after 4 hours,
Animal is put to death after 24 hours, topical vaginal tissue is taken out, observation whether there is the phenomenons such as hyperemia, oedema.
The sample vaginal mucosa stimulation test of table 11 is as follows：
| Symptom of erythema | Edematous condition | Stimulate the reaction is integrated | |
| Experimental group | — | — | 0 |
| Excipient group | — | — | 0 |
| Blank group | — | — | 0 |
Note："-" indicates no erythema or edematous condition；" 0 " represents no vaginal irritation reaction.
As a result show, in the observation period, test group, excipient group, blank control group animal topical vaginal tissue are to occur
Erythema or edematous condition, stimulate the reaction integral mean value are 0.According to《Disinfection technology standard》(third edition) first fascicle《Test skill
Art specification》Relevant criterion judges in (Ministry of Public Health, 2012.4), and the present invention is nonirritant to healthy White Rabbit vaginal mucosa.
(4) embodiment
1) embodiment one：Cooperative compositions solution containing polyglutamic acid and hyaluronic acid
First, it is formulated (part by weight)
2nd, preparation method (technical scheme)
A, above-mentioned formula rate hyaluronic acid and compound is taken to be dissolved in 37 DEG C in 50g deionized water, 1000r/min is stirred
Digestion 3h is mixed, pH5.5 is adjusted；
B, addition polyglutamic acid fully dissolve；
C plus deionized water are saved backup to 100 well mixed.
2) embodiment two：Cooperative compositions facial mask containing polyglutamic acid and hyaluronic acid
First, it is formulated (part by weight)
2nd, preparation method (technical scheme)
A, take the hyaluronic acid and compound of ratio in above-mentioned formula to be dissolved in 37 DEG C in 50g deionized water, 1500r/
Min stirring digestion 3h, adjust pH5.5, add polyglutamic acid and fully dissolve；
B, the addition after abundant dissolving at 35 DEG C by hydroxyethyl cellulose；
C, glycerine, butanediol, D-sorbite, soluble olive oil, polyethylene glycol 400 sequentially added into above-mentioned solution, mixed
Close uniform, fully dissolving；
D, by aloe extract, hamamelis extract, EDTA-2Na Phenoxyethanols, Sensiva SC50, essence add on
Solution is stated, is well mixed, fully dissolves；
E, tune pH are standby to 5.5.
3) embodiment three：Cooperative compositions effervescent tablet containing polyglutamic acid and hyaluronic acid
First, it is formulated (part by weight)
2nd, preparation method (technical scheme)
A, by the citric acid of ratio in above-mentioned formula under the conditions of 100 DEG C dry 2 hours, sodium acid carbonate is in 100 DEG C of conditions
Lower drying 2 hours, crushed 100 mesh sieves respectively, was well mixed, and sealing is cooled to 40 DEG C；
B, hyaluronic acid and compound is taken to be dissolved in 37 DEG C in 50g deionized water, 2000r/min stirring digestion 3h are adjusted
PH5.5, adds polyglutamic acid and fully dissolves, be spray dried to dry powder, adds a and is well mixed；
C, sodium chloride, sorbierite, peppermint, amino acid foaming agent, sodium benzoate, essence are added into above-mentioned material mix equal
Even, grinding, sealing is put in 60 DEG C of oven drying 30min；
D, the above-mentioned material of Macrogol 4000 addition that will spray ethanol solution, are well mixed, cross 140 mesh sieves, be put into pressure
Piece machine carries out tabletting, produces effervescent tablet.
4) example IV：Synergistic combination composition soft capsule containing polyglutamic acid and hyaluronic acid
First, soft capsule shell formula (part by weight)
Wherein, capsule heart formula (part by weight)
2nd, preparation method (technical scheme)
A, capsule shells preparation：The glycerine of aforementioned proportion, D-sorbite, mannitol, maltose are added into part successively
20min is stirred in water, it is slow to add gelatin and remaining water, do not stop stirring 25 minutes；Institute is added in upper gelatine solution
The pigment needed, artificial stirring 10min is uniform up to color, then stirring at low speed 40min, it is to avoid stir into bubble；By above-mentioned glue
Vacuum outgas three days at 60 DEG C, it is standby after detection is stable；
B, the capsule heart preparation：Hyaluronic acid and compound ratio in above-mentioned formula is taken to be dissolved in 50g deionized water at 37 DEG C
In, 2000r/min stirring digestion 3h adjust pH5.5, add polyglutamic acid and fully dissolve, be spray dried to dry powder, add sweet
Oil, PEG400 are well mixed and are crushed to 100 mesh, standby；
C, with soft capsule pellet processing machine pill is carried out to above-mentioned capsule shells and the capsule heart, it is standby.
5) embodiment five：Cooperative compositions private portion maintenance gel containing polyglutamic acid and hyaluronic acid
First, it is formulated (part by weight)
2nd, preparation method (technical scheme)
A, take the hyaluronic acid of percentage by weight 3.0% and 1.5% compound under the conditions of 37 DEG C, be dissolved in 50g deionization
In water, 1000r/min stirring digestion 3h adjust pH5.5, add 0.8% polyglutamic acid and fully dissolve；
B, glycerine, sodium chloride, preservative are sequentially added in above-mentioned mixed liquor, handled at 25 DEG C with 1000rmp rotating speeds
5min, is completely dissolved solution, is well mixed；
C, sequentially add carboxymethyl cellulose in above-mentioned mixed liquor, carbomer is handled at 40 DEG C with 800rmp rotating speeds
100min, is completely dissolved thickener, is well mixed；
D, a small amount of potassium hydroxide of addition, pH is to 4.8 for regulation, and gel is made.
6) embodiment six：Cooperative compositions emollient cream containing polyglutamic acid and hyaluronic acid
First, it is formulated (part by weight)
2nd, preparation method (technical scheme)
A, the carboxymethyl cellulose of above-mentioned formula rate, carbomer be added to the water successively, turned at 40 DEG C with 2000rmp
Speed processing 100min, is completely dissolved thickener, is well mixed；
B, by Trivent OCG, tristerin, B22 emulsifying agents, dimethyl silicone polymer, saualane, hydrogenation castor
Sesame oil heats consolute at 75 DEG C, it is fully melted, and is well mixed；
C, step a is slowly added to step b, and fully homogeneous, it is well mixed, 45 DEG C are cooled to；
D, hyaluronic acid and compound is taken to be dissolved in 37 DEG C in 50g deionized water, 1000r/min stirring digestion 3h are adjusted
PH5.5, adds polyglutamic acid and fully dissolves, and adds step c and is well mixed,
E, sequentially add glycerine, aloe extract, lecithin, ceramide, homogenization is well mixed it；
F, addition essence, preservative, pH is to 5.5 for regulation, standby.
Above-mentioned facial mask, effervescent tablet, soft capsule, private shield gel, emollient cream be all in configuration process first configure 50g go from
In sub- water, the Efficacy experiments data of this solution as above, behind different dosage forms product be all overall follow-up to add excipient, product
Effect is determined by hyaluronic acid, polyglutamic acid and compound.And it is also with liquid that the product of these formulations, which finally embodies effect,
What form was present.
Above-mentioned simply presently preferred embodiments of the present invention, not makees any formal limitation to the present invention.Although of the invention
It is disclosed above with preferred embodiment, but it is not limited to the present invention.Any those skilled in the art, are not taking off
In the case of from technical solution of the present invention scope, all technical solution of the present invention is made perhaps using the technology contents of the disclosure above
More possible variation and modification, or it is revised as the equivalent embodiment of equivalent variations.Therefore, it is every without departing from technical solution of the present invention
Content, according to the technology of the present invention essence to any simple modifications, equivalents, and modifications made for any of the above embodiments, all should fall
In the range of technical solution of the present invention protection.
Claims (10)
1. a kind of cooperative compositions containing polyglutamic acid and hyaluronic acid, it is characterised in that：The composition includes following weight
The composition of part：
5-30 parts of hyaluronic acid
1-10 parts of polyglutamic acid
1-20 parts of compound；
The compound includes recombined human hyaluronidase（PH20）, sodium chloride, calcium chloride, magnesium sulfate.
2. a kind of cooperative compositions containing polyglutamic acid and hyaluronic acid according to claim 1, it is characterised in that described
Compound includes recombined human hyaluronidase（PH20）, sodium chloride, calcium chloride, magnesium sulfate, each weight ratio of constituents be 1~2:130
~160:1.5~2.5:0.5~1.0, each composition optimum weight ratio is 1:100:2:1.
3. a kind of cooperative compositions containing polyglutamic acid and hyaluronic acid according to claim 1, it is characterised in that transparent
Matter acid, polyglutamic acid, compound optimum weight ratio are 10:5：11.
4. according to a kind of any described cooperative compositions solution containing polyglutamic acid and hyaluronic acid of claim 1-4, it is special
Levy and be：Composition and each component percentage by weight of the composition including following parts by weight are：
Hyaluronic acid 0.5-3.0%
Polyglutamic acid 0.1-1.0%
Compound 0.1-2.0%
Plus deionized water is to 100.
5. prepare the cooperative compositions solution methods described in claim 5, it is characterised in that comprise the following steps：Take correspondence weight
The hyaluronic acid and compound of percentage are dissolved in 50g deionized water at 35-40 DEG C, 1000-3000r/min stirring digestion 3-
4h, adjusts pH5.0-5.6, adds polyglutamic acid, plus deionized water is saved backup to 100 well mixed.
6. according to a kind of any described facial masks containing polyglutamic acid and hyaluronic acid cooperative compositions of claim 1-4, it is special
Levy and be：The facial mask includes following composition and each component percentage by weight is：
Hyaluronic acid 1.0%
Polyglutamic acid 0.8%
The % of compound 1.1
Glycerine 4.0%
Butanediol 3.0%
D-sorbite 1.0%
Soluble olive oil 1.0%
Polyethylene glycol 400 1.0%
Hydroxyethyl cellulose 0.3%
Aloe extract 0.05%
Hamamelis extract 0.05%
Phenoxyethanol 0.1%
Sensiva SC50 0.1%
EDTA-2Na 0.05%
Essence 0.1%
Plus deionized water is to 100.
7. a kind of effervescent tablet containing polyglutamic acid and hyaluronic acid cooperative compositions according to claim 1-4 is any, its
It is characterised by：The effervescent tablet includes following composition and each component percentage by weight is：
Hyaluronic acid 2.0%
Polyglutamic acid 1.0%
Compound 1.5%
Citric acid 20%
Sodium acid carbonate 20%
Sodium chloride 34%
Sorbierite 8.0%
Peppermint 5.0%
Macrogol 4000 2.0%
Amino acid foaming agent 5.0%
Sodium benzoate 0.5%
Ethanol 0.5%
Essence 0.5%.
8. a kind of soft capsule containing polyglutamic acid and hyaluronic acid cooperative compositions according to claim 1-4 is any, its
It is characterised by：The soft capsule includes following composition and each component percentage by weight is：
The capsule heart is formulated（Part by weight）
Hyaluronic acid 1.5%
Polyglutamic acid 1.0%
Compound 1.0%
Glycerine 5.0%
PEG400 28%
Excess water is mended to 100.
9. conserved according to a kind of any described private portions containing polyglutamic acid and hyaluronic acid cooperative compositions of claim 1-4 solidifying
Glue, it is characterised in that：Private portion's maintenance gel includes following composition and each component percentage by weight is：
Hyaluronic acid 3.0%
Polyglutamic acid 0.8%
Compound 1.5%
Carbomer 1.5%
Carboxymethyl cellulose 0.3%
Glycerine 1.5%
Sodium chloride 0.2%
Potassium hydroxide 0.1%
Preservative 0.1%
Balance deionized water is mended to 100.
10. a kind of emollient cream containing polyglutamic acid and hyaluronic acid cooperative compositions according to claim 1-4 is any, its
It is characterised by：The private emollient cream includes following composition and each component percentage by weight is：
Hyaluronic acid 1.0%
Polyglutamic acid 0.5%
Compound 0.8%
Trivent OCG 10%
Glycerine 6.0%
Tristerin 4.0%
B22 emulsifying agents 2.0%
Dimethyl silicone polymer 1.5%
Saualane 2.0%
Rilanit special 1.0%
Aloe extract 1.0%
Lecithin 1.0%
Carbomer 0.8%
Carboxymethyl cellulose 0.1%
Ceramide 0.1%
Essence 0.1%
Preservative 0.1%
Excess water is mended to 100.
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| CN107669522A (en) * | 2017-11-14 | 2018-02-09 | 北京工商大学 | A kind of method that the bionical skin care compositions suitable for youth of both sexes is prepared based on skin lipid group |
| CN107669521A (en) * | 2017-11-14 | 2018-02-09 | 北京工商大学 | A kind of method that the bionical skin care compositions suitable for the morning and evening is prepared based on skin lipid group |
| CN108403484A (en) * | 2018-06-15 | 2018-08-17 | 广州无添加主义化妆品有限公司 | A kind of fungi polysaccharide fermentation facial mask liquid, facial mask and preparation method |
| CN109674374A (en) * | 2019-01-24 | 2019-04-26 | 宁波大学 | A kind of tearable multifunctional towel and preparation method thereof |
| CN110974749A (en) * | 2019-12-27 | 2020-04-10 | 广州市科能化妆品科研有限公司 | Soothing and repairing composition, soothing and repairing solid preparation and preparation method thereof |
| CN112089643A (en) * | 2020-09-25 | 2020-12-18 | 华熙生物科技股份有限公司 | Oral care composition containing hyaluronic acid or salt thereof |
| CN112656713A (en) * | 2020-12-25 | 2021-04-16 | 华熙生物科技股份有限公司 | Cosmetic composition containing hyaluronic acid and/or derivatives thereof, and preparation method and application thereof |
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| CN107669522A (en) * | 2017-11-14 | 2018-02-09 | 北京工商大学 | A kind of method that the bionical skin care compositions suitable for youth of both sexes is prepared based on skin lipid group |
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| CN107669521B (en) * | 2017-11-14 | 2020-10-13 | 北京工商大学 | Method for preparing bionic skin care composition suitable for morning and evening based on skin lipidomics |
| CN108403484A (en) * | 2018-06-15 | 2018-08-17 | 广州无添加主义化妆品有限公司 | A kind of fungi polysaccharide fermentation facial mask liquid, facial mask and preparation method |
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| CN110974749B (en) * | 2019-12-27 | 2022-05-10 | 广州市科能化妆品科研有限公司 | Soothing and repairing composition, soothing and repairing solid preparation and preparation method thereof |
| CN112089643A (en) * | 2020-09-25 | 2020-12-18 | 华熙生物科技股份有限公司 | Oral care composition containing hyaluronic acid or salt thereof |
| CN112656713A (en) * | 2020-12-25 | 2021-04-16 | 华熙生物科技股份有限公司 | Cosmetic composition containing hyaluronic acid and/or derivatives thereof, and preparation method and application thereof |
| CN113143791A (en) * | 2021-05-17 | 2021-07-23 | 威海萨维诺健康管理有限公司 | Compound injection with whitening and anti-aging effects and preparation method thereof |
| CN114129471A (en) * | 2021-12-06 | 2022-03-04 | 华熙生物科技股份有限公司 | Suspension thickening composition and application thereof |
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Application publication date: 20170922 |