A kind of anti-ageing composition of hyaluronic acid and its preparation method and application
Technical field
The present invention relates to hyaluronic acid and its derivative technical field, more particularly to a kind of anti-ageing composition of hyaluronic acid,
Further relate to the preparation method and applications of the anti-ageing composition of the hyaluronic acid.
Background technology
Skin aging shows as the loss of skin volume and elasticity.Skin volume loss is caused due to skin HA missings
Caused by the dermal fillers dehydration such as collagen hardening;And since the loss of skin volume causes skin to become coarse, loses bullet
There is wrinkle in property.Therefore, hyaluronic acid is young most important for the health of skin.
Hyaluronic acid (hyaluronic acid, HA) is a kind of acidic mucopolysaccharide, by n-acetylglucosamine and D- glucose
Aldehydic acid disaccharide recurring unit constitute without branched high molecular glycosaminoglycan, be present in animal tissue cell's interstitial and certain bacteriums
In pod membrane.Hyaluronic acid is widely used in the fields such as medicine, cosmetics, food, and molecular weight is generally 105- 107Da (dalton).
It is well known that HA is natural moisturizing factor, excellent performances of the high HA of molecular weight with water conservation moisturizing, film forming, lubrication.Low molecule
HA is measured because its relative molecular mass is smaller, the outer used time can preferably be absorbed by skin, promote supply and the waste row of skin-nourishing
Let out, to prevent skin aging, achieve the effect that deep moisturizing and beautifying face and moistering lotion, and may additionally facilitate epidermal cell proliferation and
Differentiation, scavenging activated oxygen repair the skin of daylight or uv damage.
Also have in the prior art many for preventing skin aging, the hyaluronic acid compositions of scavenging activated oxygen as follows:
CN 105233270A disclose a kind of pharmaceutical composition for water light treatment, are by high, medium and low, 4 kinds of molecular weight of oligomerization
The gel of hyaluronic acid and collagen, epidermal growth factor and adjuvant composition.4 kinds of molecular weight are respectively 1300~2000kDa,
500~1000kDa, 50~300kDa, 3~8kDa, their optimal contents in gel are respectively 0.1%~0.2%,
0.1%~0.2%, 0.1%~0.5%, 0.2%~0.6%.Documents composition also contains collagen, epidermal growth
The well-known activity of fighting against senium ingredient of two kinds of the factor.Improve the skin problems such as drying, microgroove, aging by face injection.
Hyaluronic acid, collagen and epidermal growth factor are delivered directly in skin (water optoinjection by documents by injecting
Depth is usually in skin corium), the improvement for skin problems such as dry skin, microgroove, agings derives from injection to a certain extent
The effect of filling, by expanding skin volume, and directly replenishing collagen and growth factor, so that skin collagen
Content dramatically increases, and is achieved the effect that the proliferation function of cell to resisting age of skin by growth factor.
The performance for making full use of hyaluronic acid itself develops a kind of simple hyaluronic acid with fine anti-ageing effect
Composition, to hyaluronic acid performance make full use of and the development of industry, all have more profound significance.
Invention content
In order to solve the problems, such as that performance performance of the above hyaluronic acid in the prior art in anti-ageing is not enough, the application
It discloses a kind of three-dimensional moisturizing, remove that free radical, cell repair, to restore the significant hyaluronic acids of anti-aging effects such as skin elasticity anti-
Decline composition.
It is a further object to provide the preparation methods of the anti-ageing composition of the hyaluronic acid.
It is also another object of the present invention to provide the applications of the anti-ageing composition of the hyaluronic acid.
What the present invention was obtained through the following steps:
A kind of anti-ageing composition of hyaluronic acid, raw material weight percentage composition are as follows:
Molecular weight is the hydrolysis hyaluronic acid or its salt 60%~62% of 3~8kDa, and molecular weight is the saturating of 300~500kDa
Bright matter acid or its salt 18%~20%, molecular weight are the hyaluronic acid or its salt 18%~20% of 1000~1200kDa.
The anti-ageing composition of the hyaluronic acid, raw material weight percentage composition are as follows:
Molecular weight be 7kDa hydrolysis hyaluronic acid or its salt 60%~62%, molecular weight be 320kDa hyaluronic acid or
Its salt 18%~20%, molecular weight are the hyaluronic acid or its salt 18%~20% of 1100kDa.
The anti-ageing composition of the hyaluronic acid, raw material weight percentage composition are as follows:
Molecular weight is the hydrolysis hyaluronic acid or its salt 62% of 7kDa, and molecular weight is the hyaluronic acid or its salt of 320kDa
18%, molecular weight is the hyaluronic acid or its salt 20% of 1100kDa.
The anti-ageing composition of the hyaluronic acid, the hydrolysis hyaluronic acid or its salt are with bacillus
The bacillus hyaluronidase that A50CGMCCNO.5744 fermented and cultureds obtain degrades to hyaluronic acid or its salt
Digestion oligomerization hyaluronic acid or its salt.
Oligomerization hyaluronic acid refers to the hyaluronic acid that molecular weight is less than 10kDa.Studies have shown that molecular weight is to hyaluronic acid
Activity has a significant impact.Oligomerization hyaluronic acid can penetrate into corium, improve the lasting moistening effect of skin, while have mild dilation
Capillary increases blood circulation, improves intermediate supersession, promotes skin-nourishing absorption, also has the function of stronger wrinkle-chasing,
Skin elasticity, delay skin aging can be increased.In addition, the hydroxyl, carboxyl in oligomerization hyaluronic acid molecules of salt and other polar groups
Group can form hydrogen bond with hydrone and combine a large amount of moisture, and Water-saving effect is apparent, therefore oligomerization hyaluronate can be used for preventing
In solarization, anti-aging, moisture-keeping cosmetics.
Digestion oligomerization hyaluronic acid hydrolyzes hyaluronic acid, for Hua Xi Fu Ruida biomedical company's independent researches and produces
HA products, the hyaluronidase obtained using microbial fermentation degrades to high molecular weight hyaluronic acid or its salt, enzyme activity
Height, mild condition, easy to operate, non-environmental-pollution;And obtained digestion oligomerization hyaluronic acid or its salt structural integrity.With it
He compares the oligomerization hyaluronic acid of producer's chemical method production, and digestion oligomerization hyaluronic acid is with percutaneous absorbability is good, purity is high, nothing
The advantages that cytotoxicity, strong oxidation resistance.In addition, experiment confirms, digestion oligomerization hyaluronic acid, which also has, to be removed free radical, repaiies
After multiple solarization the effects that cell, sun-proof and Angiogensis, it can be used in cosmetics, food and field of medicaments, had a extensive future.
But for skin aging, moisture of skin, skin nutrition are kept and improved, skin free radical is removed and improves skin
Skin elasticity is all particularly important, and only this purpose can not be fully achieved in digestion oligomerization hyaluronic acid.So this field is urgent
Need a kind of composition that can reach holding and improve moisture of skin, skin nutrition, remove skin free radical, repair damaging cells
And improve the anti-aging effectiveness of skin elasticity.
The hyaluronate or hydrolysis hyaluronate be hyaluronic acid or hydrolyze the sodium salt of hyaluronic acid, sylvite,
Magnesium salts, calcium salt or zinc salt.
The preparation method of the anti-ageing composition of the hyaluronic acid:By the hyaluronic acid of two kinds of molecular weight or its salt and hydrolysis
Hyaluronic acid or its salt are mixed according to weight ratio, stir evenly to get.
Application of the anti-ageing composition of the hyaluronic acid in preparing anti-aging product.
The anti-aging is moisturizing, removes free radical, cell repair, restores skin elasticity.
The anti-aging product be smoothing toner, Essence, gel, lotion, cream, facial mask, color make-up, perfumed soap, facial cleanser or
Shower cream.
Beneficial effects of the present invention:
1) the anti-ageing composition of hyaluronic acid contains hydrolysis hyaluronic acid or its salt and hyaluronic acid or its salt, by different molecular
Amount hyaluronic acid or its salt are combined with hydrolysis hyaluronic acid or its salt (i.e. digestion oligomerization hyaluronic acid or its salt), both have high score
Sub- HA skin protections, natural moisture preserving essential effectiveness, and easily absorbs with middle molecule HA, the characteristic of skin nutrition, separately with enzyme
Cut oligomerization hyaluronic acid Transdermal absorption, remove free radical, cell repair, the bioactivity such as anti-aging, can Transdermal absorption, and have
Three-dimensional moisturizing removes free radical, repairs damaging cells and restores the anti-aging effectiveness of skin elasticity;
2) the different skin care effects for making full use of different molecular weight section HA, by skin moisture content, skin elasticity and
The multinomial test such as wrinkle depth, finally determines there is significantly anti-ageing optimum proportioning, fully excavates the anti-of hyaluronic acid
Decline effect, and more possibilities are provided for hyaluronic acid product development.
Description of the drawings
Fig. 1 moisture of skin incrementss measurement results,
Fig. 2 skin water loss reduction amount measurement results,
Fig. 3 wrinkle mean depth test results,
Fig. 4 in the original photo using 8 weeks before 2 composition of embodiment and after use,
Fig. 5 is the 3D photos before using 2 composition of embodiment,
Fig. 6 is the 3D photos after using 2 composition of embodiment.
Specific implementation mode
With reference to specific embodiment, invention is further explained:
Embodiment 1:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 6.0kg, molecule
Measure 5.4kDa;Sodium Hyaluronate I 2.0kg, molecular weight 480kDa;Sodium Hyaluronate II 2.0kg, molecular weight 1050kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Embodiment 2:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 6.2kg, molecule
Measure 7.0kDa;Sodium Hyaluronate I 1.8kg, molecular weight 320kDa;Sodium Hyaluronate II 2.0kg, molecular weight 1100kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Embodiment 3:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 6.2kg, molecule
Measure 8.5kDa;Sodium Hyaluronate I 2.0kg, molecular weight 230kDa;Sodium Hyaluronate II 1.8kg, molecular weight 1500kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Embodiment 4:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 6.2kg, molecule
Measure 3.5kDa;Sodium Hyaluronate I 1.9kg, molecular weight 120kDa;Sodium Hyaluronate II 1.9kg, molecular weight 1010kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Embodiment 5:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 6.1kg, molecule
Measure 9.5kDa;Sodium Hyaluronate I 1.9kg, molecular weight 580kDa;Sodium Hyaluronate II 2.0kg, molecular weight 1760kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Comparative example 1:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 2.0kg, molecule
Measure 7.0kDa;Sodium Hyaluronate I 2.0kg, molecular weight 320kDa;Sodium Hyaluronate II 6.0kg, molecular weight 1100kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Comparative example 2:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 8.0kg, molecule
Measure 7.0kDa;Sodium Hyaluronate I 1.0kg, molecular weight 320kDa;Sodium Hyaluronate II 1.0kg, molecular weight 1100kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Comparative example 3:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 5.0kg, molecule
Measure 7.0kDa;Sodium Hyaluronate I 2.5kg, molecular weight 320kDa;Sodium Hyaluronate II 2.5kg, molecular weight 1100kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Comparative example 4
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 5.8kg, molecule
Measure 7.0kDa;Sodium Hyaluronate I 2.1kg, molecular weight 320kDa;Sodium Hyaluronate II 2.1kg, molecular weight 1100kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Comparative example 5:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 6.7kg, molecule
Measure 7.0kDa;Sodium Hyaluronate I 1.6kg, molecular weight 320kDa;Sodium Hyaluronate II 1.7kg, molecular weight 1100kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop
Comparative example 6:
Accurate weighing hydrolyzes Sodium Hyaluronate (digestion oligomerization Sodium Hyaluronate, trade nameHA) 6.0kg, molecule
Measure 8.5kDa;Sodium Hyaluronate I 2.0kg, molecular weight 900kDa;Sodium Hyaluronate II 2.0kg, molecular weight 2000kDa;It throws respectively
Enter double conic rotary vacuum dryer, opens machine, rotation mixing 1 hour.Product after mixing is packed into sterilized packaging material
Interior (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Comparative example 7:
Accurate weighing Sodium Hyaluronate I 5.0kg, molecular weight 240kDa;II 5.0kg of Sodium Hyaluronate, molecular weight
1150kDa;Double conic rotary vacuum dryer is put into respectively, opens machine, rotation mixing 1 hour.Product after mixing is packed into
In the packaging material of sterilizing (bottled, packed, plastic-aluminum dress etc.).The above operation is carried out in dust proof workshop.
Test example 1:The moisture-keeping efficacy of hyaluronic acid compositions
With cosmetic emulsion basic components as control group, the sample of 0.2% hyaluronic acid compositions is added as experiment
Group, skin moisture content and skin water loss amount are come the difference of moistening effect between comparative sample after being smeared by measurement.
1, lotion basic components preparation process
1 lotion basic components of table
Note:A phases are oil phase, and B phases are water phase
1) A first is added to oil phase tank, is heated to 70-75 DEG C, stirring is spare to melting completely.
2) B is added to emulsion tank, is warming up to 80-85 DEG C, is uniformly dispersed, is added in tank with 78, and heat preservation is stirred to complete
Fully dissolved.
3) A is added to B phases, homogeneous is opened after mixing 2 minutes.Then C phases are added, stir evenly.It is cooled between 40-45 DEG C
D phases are added, are uniformly mixed, 38-40 DEG C of discharging.
2, test method:
Subject age is 22-55 Sui, totally 12 people.In 4 × 4cm of right-hand man's inner forearm label2Test area, by 3mg
Sample/cm2Dosage, sample is spread evenly across in trial zone.Moisture of skin tester is used respectively
CorneometerCM825 (Courage+Khazaka companies, Germany) and skin water loss tester Tewanmeter
TM300 (Courage+Khazaka companies, Germany) is measured smear before and tested region and blank when 1h, 2h, 4h, 6h after smearing
The moisture content of skin and skin water loss amount of control zone.The test of the same volunteer is completed by the same survey crew.
Measurement site and indoor temperature and humidity are consistent when front and back measurement.
3, computational methods:
4, test result:
Human skin moisture measurement result is as depicted in figs. 1 and 2.
From Fig. 1, Fig. 2 it is found that each embodiment group skin moisture content is significantly improved than comparative example group, water loss amount situation
Also it is obviously improved.Each embodiment is compared, and Examples 1 to 2 is better than embodiment 3~5.Therefore, hyaluronic acid compositions can be short
The moisture of skin is improved in time, while skin barrier can also maintain preferable state, the effect for being retained moisturizing is good.
Test example 2:Hyaluronic acid compositions free radical scavenging ability research
Respectively it is accurate measure 0.1mM DPPH (2- methyl -2,3- dihydro -5,6- diphenyl pyrazines) ethanol solution 5.0mL and
0.5% each embodiment is set with comparative sample solution 5.0mL in tool plug test tube, mixing.It is mixed with isometric water and 95% ethyl alcohol
Conjunction solution is blank control.30 minutes are placed at room temperature for, measures solution absorbance value respectively at 523nm.Free radical scavenger
Ability is stronger, and absorbance is smaller.
The experimental result of the Scavenging ability of hyaluronic acid compositions is shown in Table 2.
The Scavenging ability of 2 hyaluronic acid compositions of table
The free radical scavenging activity of embodiment 1,2,4 is apparently higher than each comparative example, and therefore, hyaluronic acid compositions have preferable
Removing free radical ability, to playing the role of and oxidation resistant, delay skin aging to skin.
Test example 3:Influence of the hyaluronic acid compositions to skin elasticity
Embodiment sample and comparative sample are prepared according to the method in test example 1.
Skin elasticity test method:Each 10 people of sample subjects recruitment, sample are applied at Face and cheek, are gently massaged into
All absorb.Once in the morning and once at night, continue 8 weeks.It is measured with skin elasticity within 2 weeks, 4 weeks, 8 weeks before smearing and after smearing
Instrument MPA580 (Courage+Khazaka companies, Germany) measures the Flexible change situation of Face and cheek position (apple flesh).Test two
It is secondary, it averages.
Common elasticity indexes have following three kinds:
Thick elasticity:R2=Ua/Uf;
Net elasticity:R5=Ur/Ue;
Bioelastic:R7=Ur/Uf;
As a result:The measurement result of skin elasticity is shown in Table 3 after smearing 8 weeks.
Influence of 3 composition containing hyaluronic acid of the table smearing after 8 weeks to skin elasticity
From table 3 it can be seen that compared with comparative example, after being used continuously 8 weeks, sample of the embodiment of the present invention can significantly improve
The elasticity of skin restores skin elasticity.
Test example 4:Influence of the hyaluronic acid compositions to wrinkle of skin
2 sample of embodiment, 5 sample of comparative example 4 and comparative example are prepared according to the method in test example 1.
Test method:Each 10 people of sample subjects recruitment, sample are applied at canthus, once in the morning and once at night, continue 8
Week.It is wrinkled after use to subject's right eye angle with human skin rapid three dimensional imaging system (Primos) within 2 weeks, 4 weeks, 8 weeks respectively
Line depth is assessed.
Evaluation method:
A is evaluated by shooting the front and back photo of smearing
B evaluates wrinkle depth with three-dimensional quick imaging system
From figure 3, it can be seen that compared with comparative example, after being used continuously 8 weeks, the tested of 2 sample of the embodiment of the present invention is used
Person, crow's foot depth are substantially reduced.Fig. 4 is the wherein one subject canthus photo using 2 sample of embodiment, uses 8
Zhou Hou, its wrinkle improves situation naked eyes as it can be seen that from 3D photos (Fig. 5,6) it can be seen that wrinkle gully obviously subtracts from original photo
It is few.
Therefore, in summary Efficacy experiments data it can be shown that hyaluronic acid compositions of the present invention take full advantage of difference
The different skin care effects of molecular weight section HA are more by the scavenging effect to free radical, and to moisture of skin, elasticity and wrinkle etc.
The improvement of aspect, to show significant anti-aging effects.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not limited by embodiment
System, other any changes made without departing from the spirit and principles of the present invention, modification, combination, replacement, simplification should be
Equivalence replacement mode, is included within the scope of the present invention.