A kind of whitening antibacterial facial mask and preparation method thereof that apple polyphenol/chitosan oligosaccharide is modified
Technical field
The invention belongs to daily cosmetics technical fields, and in particular to a kind of whitening that apple polyphenol/chitosan oligosaccharide is modified is anti-
Bacterium facial mask and preparation method thereof.
Background technique
Human skin and hair color are determined by many factors, wherein the main melanin that depends on closes in melanocyte
At type and cumulative amount, and the distribution form around in epithelial cells.Although melanin can protect cell DNA, keep away
Exempt from skin by ultraviolet ray burn, the growth or when being unevenly distributed but it is overrun will cause that local skin is excessively black and pigmentation, from
And the illnesss such as black spot, freckle, senile plaque are generated, and recently as life, the continuous quickening of work rhythm, and pollution
Caused by environment and ozone layer destruction so that melanin formed enzyme metabolic disorder so as to cause various black spots symptom people
Group is more and more.Whitening type functional form cosmetics become the hot spot of cosmetic field research in recent years.
At present the inhibition approach of melanocyte include it is intracellular inhibition and extracellular inhibition, wherein it is intracellular inhibition mainly by pair
Tyrosinase, DOPA isomerase, peroxidase, DHICA oxidizing ferment etc. are individually or collaboration inhibits, and realize the whitening of skin,
Extracellular inhibition is to be inhibited by natural materials extracts such as green-tea extract, moral citrus extracts to Endothelin peptide material, real
The whitening of existing skin.Chitosan is unique alkaline polysaccharide in nature, safe and non-toxic, and has biocompatibility and biology drop
The advantages that solution property, but the dissolution of chitosan largely limits its application, and chitosan oligosaccharide is also referred to as chitooligosaccharide-, be by
What degradation of chitosan obtained, not only good water solubility, is easily absorbed by the body, have antibacterial, antitumor, Adjust-blood lipid, adjust it is immune and
Different physiological roles, the application fields such as activation intestinal bifidobacteria are widened significantly, and chitosan oligosaccharide is commonly used for moisturizer in cosmetics.
A kind of plant whitening preparation disclosed in Chinese patent CN 104207985B and preparation method thereof in skin-lightening cosmetic
In application, the plant whitening preparation be by Luteolin, Cortex Mori extract, licoflavone, tanshinone, vitamin E mix
After uniformly, after emulsifier homogenization is added, chitosan aqueous solution is added, obtains solution I, solution I is slowly added into carboxylic first
In base chitosan solution, heating stirring, answers lime set and cools down under mildly acidic conditions, addition curing agent, heated water bath curing reaction,
Obtain microcapsule emulsion.Finally by after microcapsule emulsion centrifugation, pure water dispersion, spray drying obtains plant whitening
Preparation.In the plant whitening preparation of this method preparation, chitosan and carboxymethyl chitosan are used as moisturizer, main whitening
Substance is the compound of four kinds of Luteolin, Cortex Mori extract, licoflavone, tanshinone natural flavones.Chinese patent CN
A kind of electro-spinning disclosed in 107485578A exists chitosan and oligopeptides for chitosan/oligopeptides biology whitening mask method
It is slowly added into acetic acid solvent, is stirred at room temperature to chitosan after being completely dissolved under stirring, degassing forms spinning solution, quiet
Electrospun obtains chitosan nano fiber membrane, and chitosan nano fiber membrane is put into the drier containing glutaraldehyde cross-linking agent and is handed over
Connection, it is dry, obtain chitosan/oligopeptides biology whitening mask.Oligopeptides in chitosan/oligopeptides biology whitening mask of this method preparation
For heptapeptide, molecular sequences IIe-GIn-Ser-Pro-His-Phe-Phe, oligopeptides TYR enzyme can be played it is strong always
Effect, to prevent the synthesis of melanin, chitosan has the performances such as antibacterial, film forming, high-strength, by oligopeptides and the compound system of chitosan
Standby face-mask material has good whitening performance and biodegradability on the basis of meeting usability.By above-mentioned existing skill
Art it is found that chitosan perhaps chitosan oligosaccharide mostly be to use as film forming, moisturizing and sterilization material to chitosan or chitosan oligosaccharide itself
Research in terms of the whitening function having is actually rare.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of modified whitening antibacterial facial mask of apple polyphenol/chitosan oligosaccharide and its
Porous chitosan oligosaccharide/fibroin film preparation is formed porous composite balls using secondary dissolution process by preparation method, then with porous multiple
Ball is closed as carrier adsorption apple polyphenol formation concentrate, final load is on nonwoven carrier, obtaining whitening antibacterial facial mask.
In order to solve the above technical problems, the technical scheme is that:
A kind of whitening antibacterial facial mask that apple polyphenol/chitosan oligosaccharide is modified, which is characterized in that the apple polyphenol/chitosan oligosaccharide
Modified whitening antibacterial facial mask includes the microballoon concentrate of non-woven fabrics and absorption apple polyphenol, the microballoon of the absorption apple polyphenol
It include chitosan oligosaccharide, fibroin and apple polyphenol in concentrate, the chitosan oligosaccharide and fibroin are cross-linked to form chitosan oligosaccharide/silk
Albumen composite porous microspheres.
As a preferred embodiment of the above technical solution, the chitosan oligosaccharide/fibroin composite porous microspheres raw material is porous shell
Oligosaccharides/fibroin film secondary treatment obtains.
As a preferred embodiment of the above technical solution, the non-woven fabrics is silk based nonwoven, chitosan-based non-woven fabrics or silkworm
Silk/chitosan-based compound nonwoven cloth.
As a preferred embodiment of the above technical solution, the porous chitosan oligosaccharide/fibroin film secondary treatment technique is that irradiation is pre-
Processing, ultrasonic treatment and spray drying treatment.
The present invention also provides a kind of preparation method of the modified whitening antibacterial facial mask of apple polyphenol/chitosan oligosaccharide, feature exists
In:Include the following steps:
(1) polyethylene glycol will be added in chitosan oligosaccharide solution, after mixing, fibroin solutions is added, after mixing,
Still aging, after liquid nitrogen frozen, porous chitosan oligosaccharide/fibroin film is prepared in freeze-drying;
(2) the porous chitosan oligosaccharide/fibroin film of step (1) preparation is dissolved in molten after gamma-ray irradiation pre-processes
In agent, after ultrasonic treatment, spray drying obtains chitosan oligosaccharide/fibroin composite porous microspheres;
(3) chitosan oligosaccharide of step (2) preparation/fibroin composite porous microspheres are added in apple polyphenol extract, are stirred
It after mixing uniformly, sufficiently adsorbs, filtering obtains the microballoon concentrate of absorption apple polyphenol;
(4) the microballoon concentrate of the absorption apple polyphenol of step (3) preparation is impregnated in nonwoven carrier, is sufficiently adsorbed
Afterwards, it sterilizes, packaging obtains the modified whitening antibacterial facial mask of apple polyphenol/chitosan oligosaccharide.
As a preferred embodiment of the above technical solution, in the step (1), the molecular weight of chitosan oligosaccharide is 1-10KDa, deacetylation
> 90%, the concentration of chitosan oligosaccharide solution are 2.5-20mg/mL.
As a preferred embodiment of the above technical solution, in the step (1), the quality of chitosan oligosaccharide, polyethylene glycol and fibroin
Than being 1:0.1-0.25:0.3-0.6.
As a preferred embodiment of the above technical solution, in the step (1), porous chitosan oligosaccharide/fibroin film porosity is
20-30%.
As a preferred embodiment of the above technical solution, in the step (2), the pretreated amount of radiation of gamma-ray irradiation is 5-
10KGy。
As a preferred embodiment of the above technical solution, in the step (2), the frequency of ultrasonic treatment is 50-150W, and the time is
30-60min, chitosan oligosaccharide/fibroin composite porous microspheres partial size are 200-800 μm.
As a preferred embodiment of the above technical solution, in the step (3), it is more to adsorb apple in the microballoon concentrate of apple polyphenol
The content of phenol is 10-30wt%.
Compared with prior art, the invention has the advantages that:
The modified whitening antibacterial facial mask of apple polyphenol prepared by the present invention/chitosan oligosaccharide includes non-woven fabrics and absorption apple polyphenol
Microballoon concentrate, wherein including chitosan oligosaccharide, fibroin and apple polyphenol in the microballoon concentrate of absorption apple polyphenol, shell is few
Sugar and fibroin are first cross-linked to form porous chitosan oligosaccharide/fibroin film, then via radiation, microwave and spraying treatment obtain shell widow
Sugar/fibroin composite porous microspheres, first chitosan oligosaccharide can significantly improve the vigor of skin, delay its aging, keep skin
Normal " breathing " because not only chitosan oligosaccharide can with scavenging capacity oxygen radical, inhibit peroxidating, but also can be improved SOD,
The vigor of apple polyphenol additionally can be improved in the activity of the antioxidases such as CAT, prevents brown stain and muddiness, therefore by chitosan oligosaccharide
Can effectively remove with apple polyphenol as main antioxidant material causes skin aging and the active oxygen of blackening process free
Base protects the healthy vigor of skin.And compared with the prior art is that technique is simply mixed, the present invention is by chitosan oligosaccharide and silk egg
White line crosslinking film forming is that pore former makes film have certain porosity using polyethylene glycol, then molten again by irradiation and microwave
Solution technique makes porous chitosan oligosaccharide/fibroin film kind chitosan and fibroin reunite again during decomposition, passes through spoke
The degree decomposed is adjusted according to processing, chitosan oligosaccharide/fibroin composite porous microspheres is prepared, then with the chitosan oligosaccharide/silk
Albumen composite porous microspheres are that carrier sufficiently adsorbs apple polyphenol extract, during absorption, chitosan oligosaccharide and fibroin
It is swollen, wherein by apple polyphenol cladding, improves the stability of middle apple polyphenol, and pass through in the use process of facial mask
Moisture evaporation, beating and squeezing action release react on skin surface with chitosan oligosaccharide and fibroin one, synchronous to carry out beauty
White, sterilization and moisture-keeping function, will not cause skin excessively to bear, using effect is good.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1:
It (1) is 1 according to the mass ratio of chitosan oligosaccharide, polyethylene glycol and fibroin:0.1:0.3, it is 2.5mg/mL by concentration
Molecular weight be 1KDa, polyethylene glycol is added in 90% chitosan oligosaccharide solution of deacetylation >, after mixing, is added 5wt%'s
Fibroin solutions, after mixing, the still aging 12h at 15 DEG C, after liquid nitrogen frozen, hole is prepared in freeze-drying
Porous chitosan oligosaccharide/fibroin film that gap rate is 20%.
(2) porous chitosan oligosaccharide/fibroin film is dissolved in solvent, after the pretreatment of 5KGy gamma-ray irradiation in 50W
After being ultrasonically treated 30min under power, spray drying obtains chitosan oligosaccharide/fibroin composite porous microspheres that partial size is 200 μm.
(3) chitosan oligosaccharide/fibroin composite porous microspheres are added in apple polyphenol extract, after mixing evenly, sufficiently
Absorption, is filtered through micro-nano film, obtains the microballoon concentrate of absorption apple polyphenol, wherein adsorb the microballoon concentrate of apple polyphenol
The content of middle apple polyphenol is 10wt%.
It (4) is 1mg according to the microballoon concentrate of absorption apple polyphenol and the materials ratio of non-woven fabrics:1.5g will adsorb apple
The microballoon concentrate of polyphenol is impregnated in silk based nonwoven carrier, sufficiently after absorption, is sterilized, and packaging obtains apple polyphenol/shell
The modified whitening antibacterial facial mask of oligosaccharides.
Embodiment 2:
It (1) is 1 according to the mass ratio of chitosan oligosaccharide, polyethylene glycol and fibroin:0.25:0.6, it is 20mg/mL by concentration
Molecular weight be 10KDa, polyethylene glycol is added in 90% chitosan oligosaccharide solution of deacetylation >, after mixing, is added 8wt%'s
Fibroin solutions, after mixing, at 25 DEG C it is still aging for 24 hours, after liquid nitrogen frozen, freeze-drying, hole is prepared
Porous chitosan oligosaccharide/fibroin film that gap rate is 30%.
(2) porous chitosan oligosaccharide/fibroin film is dissolved in solvent after the pretreatment of 10KGy gamma-ray irradiation,
After being ultrasonically treated 60min under 150W power, it is compound porous micro- to obtain chitosan oligosaccharide/fibroin that partial size is 800 μm for spray drying
Ball.
(3) chitosan oligosaccharide/fibroin composite porous microspheres are added in apple polyphenol extract, after mixing evenly, sufficiently
Absorption, is filtered through micro-nano film, obtains the microballoon concentrate of absorption apple polyphenol, wherein adsorb the microballoon concentrate of apple polyphenol
The content of middle apple polyphenol is 30wt%.
It (4) is 1mg according to the microballoon concentrate of absorption apple polyphenol and the materials ratio of non-woven fabrics:3g is more by absorption apple
The microballoon concentrate of phenol is impregnated in chitosan-based nonwoven carrier, sufficiently after absorption, is sterilized, and packaging obtains apple polyphenol/shell
The modified whitening antibacterial facial mask of oligosaccharides.
Embodiment 3:
It (1) is 1 according to the mass ratio of chitosan oligosaccharide, polyethylene glycol and fibroin:0.15:0.4, it is 5mg/mL's by concentration
Molecular weight is 5KDa, and polyethylene glycol is added in 90% chitosan oligosaccharide solution of deacetylation >, after mixing, the silkworm of 6wt% is added
Silk protein solution, after mixing, the still aging 18h at 20 DEG C, after liquid nitrogen frozen, hole is prepared in freeze-drying
Porous chitosan oligosaccharide/fibroin film that rate is 25%.
(2) porous chitosan oligosaccharide/fibroin film is dissolved in solvent after the pretreatment of 8KGy gamma-ray irradiation,
After being ultrasonically treated 45min under 120W power, it is compound porous micro- to obtain chitosan oligosaccharide/fibroin that partial size is 600 μm for spray drying
Ball.
(3) chitosan oligosaccharide/fibroin composite porous microspheres are added in apple polyphenol extract, after mixing evenly, sufficiently
Absorption, is filtered through micro-nano film, obtains the microballoon concentrate of absorption apple polyphenol, wherein adsorb the microballoon concentrate of apple polyphenol
The content of middle apple polyphenol is 15wt%.
It (4) is 1mg according to the microballoon concentrate of absorption apple polyphenol and the materials ratio of non-woven fabrics:2.5g will adsorb apple
The microballoon concentrate of polyphenol is impregnated in silk/chitosan-based compound nonwoven cloth carrier, sufficiently after absorption, is sterilized, and packaging obtains
The modified whitening antibacterial facial mask of apple polyphenol/chitosan oligosaccharide.
Embodiment 3:
It (1) is 1 according to the mass ratio of chitosan oligosaccharide, polyethylene glycol and fibroin:0.23:0.45, it is 10mg/mL by concentration
Molecular weight be 8KDa, polyethylene glycol is added in 90% chitosan oligosaccharide solution of deacetylation >, after mixing, 6.5wt% is added
Fibroin solutions, after mixing, the still aging 16h at 18 DEG C, after liquid nitrogen frozen, freeze-drying, be prepared
Porous chitosan oligosaccharide/fibroin film that porosity is 27%.
(2) porous chitosan oligosaccharide/fibroin film is dissolved in solvent after the pretreatment of 7.5KGy gamma-ray irradiation,
After being ultrasonically treated 40min under 120W power, it is compound porous micro- to obtain chitosan oligosaccharide/fibroin that partial size is 400 μm for spray drying
Ball.
(3) chitosan oligosaccharide/fibroin composite porous microspheres are added in apple polyphenol extract, after mixing evenly, sufficiently
Absorption, is filtered through micro-nano film, obtains the microballoon concentrate of absorption apple polyphenol, wherein adsorb the microballoon concentrate of apple polyphenol
The content of middle apple polyphenol is 17wt%.
It (4) is 1mg according to the microballoon concentrate of absorption apple polyphenol and the materials ratio of non-woven fabrics:2.3g will adsorb apple
The microballoon concentrate of polyphenol is impregnated in silk based nonwoven carrier, sufficiently after absorption, is sterilized, and packaging obtains apple polyphenol/shell
The modified whitening antibacterial facial mask of oligosaccharides.
Embodiment 4:
It (1) is 1 according to the mass ratio of chitosan oligosaccharide, polyethylene glycol and fibroin:0.17:0.35, it is 16mg/mL by concentration
Molecular weight be 3KDa, polyethylene glycol is added in 90% chitosan oligosaccharide solution of deacetylation >, after mixing, 6.5wt% is added
Fibroin solutions, after mixing, the still aging 20h at 20 DEG C, after liquid nitrogen frozen, freeze-drying, be prepared
Porosity is porous chitosan oligosaccharide/fibroin film of 23%d.
(2) porous chitosan oligosaccharide/fibroin film is dissolved in solvent, after the pretreatment of 9KGy gamma-ray irradiation in 80W
After being ultrasonically treated 45min under power, spray drying obtains chitosan oligosaccharide/fibroin composite porous microspheres that partial size is 450 μm.
(3) chitosan oligosaccharide/fibroin composite porous microspheres are added in apple polyphenol extract, after mixing evenly, sufficiently
Absorption, is filtered through micro-nano film, obtains the microballoon concentrate of absorption apple polyphenol, wherein adsorb the microballoon concentrate of apple polyphenol
The content of middle apple polyphenol is 15wt%.
It (4) is 1mg according to the microballoon concentrate of absorption apple polyphenol and the materials ratio of non-woven fabrics:2g is more by absorption apple
The microballoon concentrate of phenol is impregnated in silk/chitosan-based compound nonwoven cloth carrier, sufficiently after absorption, is sterilized, and packaging obtains apple
The modified whitening antibacterial facial mask of fruit polyphenol/chitosan oligosaccharide.
Embodiment 5:
It (1) is 1 according to the mass ratio of chitosan oligosaccharide, polyethylene glycol and fibroin:0.1:0.6, it is 2.5mg/mL by concentration
Molecular weight be 10KDa, polyethylene glycol is added in 90% chitosan oligosaccharide solution of deacetylation >, after mixing, is added 5wt%'s
Fibroin solutions, after mixing, the still aging 12h at 25 DEG C, after liquid nitrogen frozen, hole is prepared in freeze-drying
Porous chitosan oligosaccharide/fibroin film that gap rate is 30%.
(2) porous chitosan oligosaccharide/fibroin film is dissolved in solvent after the pretreatment of 5KGy gamma-ray irradiation,
After being ultrasonically treated 30min under 150W power, it is compound porous micro- to obtain chitosan oligosaccharide/fibroin that partial size is 800 μm for spray drying
Ball.
(3) chitosan oligosaccharide/fibroin composite porous microspheres are added in apple polyphenol extract, after mixing evenly, sufficiently
Absorption, is filtered through micro-nano film, obtains the microballoon concentrate of absorption apple polyphenol, wherein adsorb the microballoon concentrate of apple polyphenol
The content of middle apple polyphenol is 10wt%.
It (4) is 1mg according to the microballoon concentrate of absorption apple polyphenol and the materials ratio of non-woven fabrics:3g is more by absorption apple
The microballoon concentrate of phenol is impregnated in silk based nonwoven carrier, sufficiently after absorption, is sterilized, and it is few to obtain apple polyphenol/shell for packaging
The modified whitening antibacterial facial mask of sugar.
Embodiment 6:
It (1) is 1 according to the mass ratio of chitosan oligosaccharide, polyethylene glycol and fibroin:0.25:0.3, it is 20mg/mL by concentration
Molecular weight be 1KDa, polyethylene glycol is added in 90% chitosan oligosaccharide solution of deacetylation >, after mixing, is added 8wt%'s
Fibroin solutions, after mixing, at 15 DEG C it is still aging for 24 hours, after liquid nitrogen frozen, freeze-drying, hole is prepared
Porous chitosan oligosaccharide/fibroin film that gap rate is 20%.
(2) porous chitosan oligosaccharide/fibroin film is dissolved in solvent after the pretreatment of 10KGy gamma-ray irradiation,
After being ultrasonically treated 60min under 50W power, it is compound porous micro- to obtain chitosan oligosaccharide/fibroin that partial size is 200 μm for spray drying
Ball.
(3) chitosan oligosaccharide/fibroin composite porous microspheres are added in apple polyphenol extract, after mixing evenly, sufficiently
Absorption, is filtered through micro-nano film, obtains the microballoon concentrate of absorption apple polyphenol, wherein adsorb the microballoon concentrate of apple polyphenol
The content of middle apple polyphenol is 30wt%.
It (4) is 1mg according to the microballoon concentrate of absorption apple polyphenol and the materials ratio of non-woven fabrics:1.5g will adsorb apple
The microballoon concentrate of polyphenol is impregnated in silk/chitosan-based compound nonwoven cloth carrier, sufficiently after absorption, is sterilized, and packaging obtains
The modified whitening antibacterial facial mask of apple polyphenol/chitosan oligosaccharide.
Through detecting, the stickiness of the modified whitening antibacterial facial mask of apple polyphenol/chitosan oligosaccharide of embodiment 1-6 preparation is breathed freely
The result of property, antibiotic rate, whitening effect and moistening effect is as follows:
As seen from the above table, the modified whitening antibacterial facial mask of apple polyphenol prepared by the present invention/chitosan oligosaccharide is ventilative using fitting,
With good antibacterial whitening and moisture-keeping efficacy.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.