CN111743785B - Nanofiber membrane with whitening and tightening effects and preparation method thereof - Google Patents

Nanofiber membrane with whitening and tightening effects and preparation method thereof Download PDF

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Publication number
CN111743785B
CN111743785B CN201910241431.XA CN201910241431A CN111743785B CN 111743785 B CN111743785 B CN 111743785B CN 201910241431 A CN201910241431 A CN 201910241431A CN 111743785 B CN111743785 B CN 111743785B
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whitening
tightening
oil
stirring
mass ratio
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CN111743785A (en
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岳娟
徐思伟
毕永贤
毕天宇
邱玉想
邵平
蒋丽刚
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Proya Cosmetics Co Ltd
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Proya Cosmetics Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0212Face masks
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/347Phenols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4906Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
    • A61K8/4913Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom having five membered rings, e.g. pyrrolidone carboxylic acid
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/55Phosphorus compounds
    • A61K8/553Phospholipids, e.g. lecithin
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • A61K8/602Glycosides, e.g. rutin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F4/00Monocomponent artificial filaments or the like of proteins; Manufacture thereof
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326Condensation or reaction polymers
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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Abstract

The invention relates to a nanofiber membrane with whitening and tightening effects and a preparation method thereof, and is characterized in that: the nanofiber membrane simultaneously contains an oil-soluble whitening and tightening active ingredient pterostilbene, dipalmitoyl hydroxyproline, prinus davidiana oil and a water-soluble whitening and tightening active ingredient fructose diphosphate trisodium, asiaticoside, hydrolyzed elastin and a gynostemma pentaphyllum leaf extract; the oil-soluble whitening and tightening active ingredients and the water-soluble whitening and tightening active ingredients are coated by hydrogenated lecithin to prepare a whitening and tightening nano composition, and then the whitening and tightening nano composition is mixed with succinoglycan, rhizobium glue and deionized water to prepare a nano fiber membrane through an electrostatic spinning process. The whitening and firming cream has the advantages of good skin-friendly property, good stability, quick absorption, convenience in use and the like, and meanwhile, the whitening and firming cream is loaded with the oil-soluble whitening and firming active substance and the water-soluble whitening and firming active substance, so that the technical defect that only one of the oil-soluble whitening and firming active substances can be loaded in the prior art is overcome, and the whitening and firming cream has better whitening and firming effects.

Description

Nanofiber membrane with whitening and tightening effects and preparation method thereof
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a nanofiber membrane with whitening and tightening effects and a preparation method thereof.
Background
People pursue various cosmetics with various categories and efficacies for the mild taste of cumin, and the facial mask is taken as a category of skin care products, and has the advantages of convenient use, comprehensive efficacy, high cost performance and the like, so that the facial mask becomes one of the most rapidly growing market segments in the cosmetic industry at present. The existing commercially available facial masks can be mainly divided into a smearing type, a tearing type and a patch type according to the using mode, the smearing type is generally limited in absorption and unobvious in effect, the tearing type is easy to damage the skin, the patch type has the effects of instantly moisturizing, brightening the skin and improving the skin texture, and meanwhile, the types of the membrane cloth and the essence are various and can meet different requirements of consumers, so that the existing commercially available facial masks become products with the largest sales volume and the fastest growth speed in facial mask products.
The traditional patch type facial mask has certain limitations, on one hand, in order to maintain the stability and shelf life of the product, a certain preservative is often added into the essence, the patch type facial mask isolates the outside air, the skin temperature is improved, pores are expanded, the permeation and absorption of the essence are enhanced, and the preservative has certain stimulation and allergy possibility; on one hand, the stability of the functional components is always problematic, the activity of the functional components is lost after the functional components are soaked in essence for a long time, and the efficacy of the product is limited; moreover, essence is easy to drip during the taking out and applying processes of the patch type facial mask, and the use is inconvenient; in addition, the conventional non-woven fabric membrane cloth has poor skin conformability and affinity.
The freeze-drying shaping technology is a technology that flowable liquid, semisolid or solid active ingredients contain or are added with a skeleton supporting agent and a binding agent, the flowable liquid, semisolid or solid active ingredients are poured into a forming mold, and then the molding is carried out through a freeze-drying process. The freeze-drying excipient technology is applied to the patch type facial mask, so that active ingredients can be protected from being damaged, a preservative is not added, the patch type facial mask is mild and safe, and the use process has an appearance feeling and a participation feeling. However, the freeze-dried facial mask still depends on the mask cloth, the fitting property, the affinity and the conductivity of active ingredients depend on the mask cloth, and in addition, the problems that the essence is easy to drip and inconvenient to use still exist. Meanwhile, the freeze-drying excipient technology needs a large amount of skeleton supporting agents, and has long freeze-drying time, limited yield and higher production cost.
The nanofiber has the characteristics of large specific surface area, good fiber continuity, high porosity, small pore diameter, light weight, easiness in processing and the like, and the characteristics promote the nanofiber and active ingredients carried by the nanofiber to be easily absorbed by a human body, improve the stability of active substances, control the release of the active ingredients and be a preferred material of an effective membrane material. The electrostatic spinning is an excellent method for industrially preparing the nanofiber material due to the advantages of wide material selection, good uniformity of prepared fibers, simple manufacturing device, low spinning cost, controllable process and the like.
The active ingredients with whitening and firming effects which can be applied to cosmetics mostly have the problems of poor stability and low solubility, and the development and the use of products are limited. In the prior art, patent publication No. CN108301068A, namely, nanofiber with a core-shell structure prepared by electrostatic spinning of gel-like oil-in-water emulsion, prepares biodegradable nanofiber by using hydrophilic colloid to entrap hydrophobic active substances, and the technical scheme disclosed in the patent is only suitable for entrapping hydrophobic active substances. The invention relates to a method for preparing a biodegradable polymer nanofiber membrane by an emulsion electrospinning method, which is disclosed in Chinese patent publication No. CN103572508B, and the biodegradable polymer 'poly (butylene succinate), polylactic acid, poly (glycolide-co-lactide), poly (epsilon-caprolactone), polylactic acid-glycolic acid copolymer and other' load incompatible liquids 'such as water, isopropanol, glycol, glycerol' and the like are adopted to prepare the nanofiber membrane, so that the nanofiber membrane is only suitable for loading hydrophilic active substances and is not suitable for hydrophobic active substances.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a nanofiber membrane with whitening and firming effects and a preparation method thereof, wherein the nanofiber membrane has the advantages of good skin-friendly property, good stability, quick absorption, convenience in use and the like, and meanwhile, an oil-soluble whitening and firming active substance and a water-soluble whitening and firming active substance are loaded, so that the technical defect that only one load can be selected in the prior art is overcome, and the whitening and firming effects are better.
In order to solve the technical problems, the invention adopts the following technical scheme: a nanofiber membrane with whitening and tightening effects is characterized in that: meanwhile, the whitening and tightening cream contains the oil-soluble whitening and tightening active ingredients of pterostilbene, dipalmitoyl hydroxyproline, prinsepia utilis royle oil and the water-soluble whitening and tightening active ingredients of fructose diphosphate trisodium, asiaticoside, hydrolyzed elastin and gynostemma pentaphylla leaf extract. The oil-soluble whitening and tightening active ingredients and the water-soluble whitening and tightening active ingredients are coated by hydrogenated lecithin to prepare a whitening and tightening nano composition, and then the whitening and tightening nano composition is mixed with succinoglycan, rhizobium glue and deionized water and prepared into a nano fiber membrane through an electrostatic spinning process.
The invention also provides a method for preparing the nanofiber membrane with whitening and tightening effects, which is characterized by comprising the following steps of:
A. according to the mass ratio of 1: 1-2: 10 weighing pterostilbene, dipalmitoyl hydroxyproline and prinsepia utilis royle oil, mixing, heating, stirring until the mixture is completely dissolved, and cooling to room temperature to obtain an oil-soluble whitening and firming active ingredient; according to the mass ratio of 1: 1-2: 3: 1-5: 5-10 weighing fructose diphosphate trisodium, asiaticoside, hydrolyzed elastin, gynostemma pentaphylla leaf extract and polyhydric alcohol, mixing, heating, stirring to completely dissolve, and cooling to room temperature to obtain water-soluble whitening and firming active ingredients;
B. according to the mass ratio of 2-5: 1: 1-2 weighing polydimethylsiloxane, hydrogenated C6-14 alkene polymers and octyl dodecanol, heating and stirring to 75-80 ℃ to obtain an oil phase for later use;
C. according to the mass ratio of 1: weighing hydrogenated lecithin and deionized water 10-30, stirring, heating to 75-85 deg.C, and collecting water phase;
D. the oil-soluble whitening and tightening active ingredient, the water-soluble whitening and tightening active ingredient, the oil phase and the water phase are mixed according to the mass ratio of 1: 1-2: 1: 1-4, heating to 75-85 ℃, uniformly stirring, and circularly homogenizing for 5-10 times under the condition of 90-120MPa by a high-pressure homogenizer to obtain the whitening and compacting nano composition;
E. according to the mass ratio of 0.5-1: 0.5-2: 100, weighing succinoglycan, rhizobium glue and deionized water, and stirring for 10-30min at the stirring speed of 1000-2000rpm to obtain a colloidal solution;
F. according to the mass ratio of 1: 2-10, weighing the whitening and tightening nano composition and the colloidal solution, and stirring at the rotating speed of 1000-1500rpm for 5-15min to prepare an electrostatic spinning solution;
G. and F, transferring the electrostatic spinning solution obtained in the step F into a nano spider electrostatic spinning instrument, carrying out electrostatic spinning under the conditions of electrostatic field voltage of 10-25kv, spinning speed of 0.1-1mL/h and receiving distance of 10-20cm, and receiving with aluminum foil to obtain the nano fiber membrane with whitening and tightening effects.
The nano spider electrostatic spinning instrument is an Elmarco NS Lab 2G nano spider electrostatic spinning instrument.
The application method of the nanofiber membrane with whitening and tightening effects comprises the following steps: cutting and cutting according to actual needs, and can be used as facial mask, eye mask, neck mask, etc., before application, the part to be applied is moistened with moisturizing spray, then the nanofiber membrane prepared by the invention is applied, the moisturizing spray can be used again to ensure that the facial mask is sufficiently moistened and completely attached to the skin, and after the application for 5-30 minutes, the nanofiber membrane is completely absorbed by the skin.
The nanofiber membrane with the whitening and tightening effects is prepared from nanofibers taking nanoliposomes as cores, wherein the diameter range of the nanofibers is 100-300nm, and the thickness range of the nanofibers is 30-100 mu m.
The pterostilbene (PTEROSIBILENE, PTER), CAS number 537-42-8, INCI brand Pterocarpus marsupium bark extract, numbered 02986 in the catalogue of names of used cosmetic raw materials (2015 edition) in China, was purchased from Sabinsa USA, and had a purity of not less than 98%. The pterostilbene is insoluble in water, has strong lipophilicity and is unstable to light and heat, and can simultaneously show excellent effects of resisting oxidation, eliminating free radicals, inhibiting melanin deposition, whitening, resisting inflammation and resisting ultraviolet rays.
The DIPALMITOYL HYDROXYPROLINE (DIPALMITOYL HYDROXYPROLINE) was purchased from Saybox, having a purity of not less than 98%, and having a serial number of 02255 in catalog of names of used cosmetic raw materials (2015 edition) in China. Dipalmitoyl hydroxyproline is hydroxyproline biological conductor, not only has good skin affinity, but also has various effects of stimulating collagen fiber contraction, effectively protecting elastin, eliminating oxygen free radicals, increasing moisture content in skin and the like.
The Prinsepia utilis Royle oil (PRINSEPIA UTILIS OIL), with the serial number of 05313 in catalog of used cosmetic raw materials (2015 edition) in China, was purchased from natural nutritional vegetable oil of Prinsepia utilis Royle of Yunnan Lijiang, wherein the content of vitamin A is not less than 0.03 mg/g. The Prinsepia utilis Royle oil is a pure natural skin care oil, is very close to human body lipid and is easy to be absorbed by skin, and the abundant vitamin A in the Prinsepia utilis Royle oil can promote the mitotic capacity of cells, improve the enzyme activity, prevent the decomposition of collagen and improve epithelial cells, thereby achieving the effects of smoothing wrinkles, reducing pigmentation, improving the barrier function of the skin and improving the moisture retention.
The TRISODIUM FRUCTOSE DIPHOSPHATE (TRISODIUM FRUCTOSE DIPHOSPHATE sodium) is numbered 02700 in catalog (2015 edition) of Chinese names of used cosmetic raw materials, purchased from Hibiscus limited science and technology development in Shanghai, and has a purity of not less than 98%. The trisodium fructodiphosphate can inhibit the generation of melanin by activating three enzymes of a human body, thereby achieving the effect of whitening.
The ASIATICOSIDE (asioticoside) with a serial number of 03173 in catalog of names of used cosmetic raw materials (2015 edition) in china was purchased from doff biotechnology limited, and has a purity of not less than 90%. Asiaticoside can improve skin elasticity and delay skin aging by promoting fibroblast growth, collagen synthesis and epithelial cell growth.
The HYDROLYZED ELASTIN (HYDROLYZED ELASTIN) has a sequence number of 06293 in the catalogue of names of used cosmetic raw materials (2015 edition) in China, and is purchased from Japanese aquatic plant and has a desmosine and heterodesmosine (amino acid specific to ELASTIN) content of not less than 0.12%. The hydrolyzed elastin can promote the generation of hyaluronic acid and cell proliferation of skin, and has effects of improving skin elasticity, and improving wrinkle or flabbiness.
The Gynostemma PENTAPHYLLUM LEAF EXTRACT (Gynostemma PENTAPHYLLUM LEAF EXTRACT) was purchased from Yiwan corporation, Japan, with number 03436 in catalog of names of used cosmetic raw materials (2015 edition) in China. The gynostemma pentaphylla leaf extract can improve the aquaporins in skin cells, improve the water absorption capacity of the cells from the inside, and promote the degradation of skin cutin and the renewal of collagen fibers, thereby improving the skin, whitening the skin, and smoothing and tightening the skin.
The polyalcohol is one or mixture of glycerol, butanediol, propylene glycol, dipropylene glycol, diglycerol, pentanediol and hexanediol.
The polydimethylsiloxane, having an INCI name DIMETHICONE, was numbered 03732 in the catalogue of used cosmetic raw materials (2015 edition) in China, and had a viscosity of 20 CST.
The HYDROGENATED C6-14 OLEFIN POLYMERS, INCI name HYDROGENATED C6-14 OLEFIN POLYMERS, number 05327 in the catalogue of used cosmetic raw materials (2015) in China.
The OCTYLDODECANOL, Octyldodecanol, INCI name in Chinese catalog of names of used cosmetic raw materials (2015 edition), serial number 07177.
The HYDROGENATED LECITHIN is named as HYDROGENATED LECITHIN in English, and has the serial number of 05378 in Chinese catalogue of names of used cosmetic raw materials (2015 edition), and the commercial product is sold by LIOID company in Germany. The preferred hydrogenated lecithin of the invention contains hydrogenated phosphatidylcholine with a mass ratio content of not less than 75%.
The SUCCINOGLYCAN, SUCCINOGLYCAN, English name, was numbered 02971 in the catalogue of names of used cosmetic raw materials (2015 edition) in China.
The Rhizobium glue is named RHIZOBIAN GUM in English, and has a serial number of 02547 in catalog of names of used cosmetic raw materials (2015 edition) in China.
To demonstrate the advantageous effects of the present invention, the following experiment was further performed.
The following is a description of the whitening and firming efficacy experiment of the present invention: 80 female volunteers between 30-50 years of age were selected on a voluntary basis and divided into 4 groups for parallel testing. The experimental group 1 directly smears a nano solution with a whitening and tightening effect composition, the experimental group 2 uses the nano solution with the whitening and tightening effect composition as a patch type facial mask essence to match with a common non-woven fabric membrane cloth, the experimental group 3 uses a freeze-dried facial mask prepared by adding a skeleton supporting agent and a binder into the nano solution with the whitening and tightening effect composition to match with the same non-woven fabric membrane cloth and by using a freeze-drying shaping technology, the experimental group 4 uses a facial mask prepared by using nano fibers with nano liposomes as cores, and the nano solutions in the 4 groups of samples are prepared by using the preparation method of the embodiment 1. Subjects were asked to use three times a week, before use and after 1 month of use for follow-up tests, totaling 2 times, with follow-up being the same time of day and no other products of the same type being used during the trial. During the follow-up period, the phenomena of skin allergy, erythema, itching and the like caused by using the test sample do not occur to the user. Before the test, the tested subject needs to sit still for 20min in a constant temperature and humidity environment (room temperature is 22 ℃ plus or minus 2 ℃, and relative humidity is 45 percent plus or minus 5 percent), and then the skin elasticity, wrinkles and whiteness change ratio before use and after 1 month of use are measured and analyzed by an MPA580 skin elasticity tester, a PRIMOS PICO skin wrinkle detector and a Menetta CM-700D spectrophotometer, and the results are respectively shown in Table 1.
Table 1 skin elasticity, wrinkle and whiteness change ratio test data before and after use
Figure DEST_PATH_IMAGE001
R2 is the ratio of the rebound quantity of the skin without negative pressure to the maximum stretching quantity with negative pressure, and can represent the elasticity of the skin, Wv is a comprehensive parameter representing the severity of wrinkles, and ITA DEG is a comprehensive parameter representing the whiteness of the skin. In table 1, Δ R2, Δ Wv, and Δ ITA ° indicate the change ratio of skin elasticity, wrinkles, and whiteness before and after the use of samples by 4 parallel experimental groups, as can be seen from the table, the elasticity and whiteness of the skin in the 4 groups of experiments are improved, the wrinkles become shallow, the experimental group 1, the experimental group 2, and the experimental group 3 are not greatly different, that is, the whitening and tightening effects of the ordinary non-woven fabric mask and the freeze-dried mask are not greatly different, while the whitening and tightening effects of the facial mask prepared by the nano-fibers with the nano-liposomes as the core in the experimental group 4 are obviously higher than those of the experimental group 1, the experimental group 2, and the experimental group 3, which are different from the traditional non-woven fabric mask, the nano-fibers are used for carrying active ingredients, so as to facilitate the diffusion and dissolution of the active ingredients, improve the percutaneous absorption capability, and thus better exert the whitening and tightening effects.
According to the invention, the water-soluble whitening and tightening active ingredients and the oil-soluble whitening and tightening active ingredients are wrapped by the nano-liposome, and then the nano-fiber membrane is prepared by using the electrostatic spinning technology, and compared with the prior art, the nano-fiber membrane has the following advantages: 1) the stability is good, the water-soluble whitening and firming active ingredients and the oil-soluble whitening and firming active ingredients are not easily oxidized after being wrapped by the liposome, the stability of the active ingredients is improved, and the technical problem that the whitening active ingredients are difficult to dissolve is solved; 2) The obtained nanofiber membrane is instantly dissolved in water, and the succinoglycan and the rhizobium glue are used as main viscosity control components of the electrostatic spinning solution, so that the nanofiber membrane is good in skin-friendly property, beneficial to absorption of active components, natural in material source and environment-friendly, and has a certain skin tightening effect; 3) the obtained nanofiber membrane has good skin fitness and affinity, no dripping phenomenon, complete absorption, no need of cleaning, convenient use, and better biocompatibility and biodegradability; 4) the obtained nanofiber membrane has good permeability and absorbability, the active ingredients are synergistic, and the effects of all-round whitening and tightening are achieved.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples, but the scope of the present invention is not limited thereto.
Example 1: a nanofiber membrane with whitening and tightening effects and a preparation method thereof are disclosed, and the preparation method comprises the following steps:
A. according to the mass ratio of 1: 2: 10 weighing pterostilbene, dipalmitoyl hydroxyproline and prinsepia utilis royle oil, mixing, heating, stirring until the mixture is completely dissolved, and cooling to room temperature to obtain an oil-soluble whitening and firming active ingredient; according to the mass ratio of 1: 2: 3: 5: 10 weighing fructose diphosphate trisodium, asiaticoside, hydrolyzed elastin, gynostemma pentaphylla leaf extract and polyhydric alcohol, mixing, heating, stirring to completely dissolve, and cooling to room temperature to obtain water-soluble whitening and firming active ingredients;
B. according to the mass ratio of 2: 1: 1 weighing polydimethylsiloxane, hydrogenated C6-14 alkene polymers and octyl dodecanol, heating and stirring to 75 ℃ to obtain an oil phase for later use;
C. according to the mass ratio of 1: 20 weighing hydrogenated lecithin and deionized water, uniformly stirring, and heating to 80 ℃ to obtain a water phase for later use;
D. the oil-soluble whitening and tightening active ingredient, the water-soluble whitening and tightening active ingredient, the oil phase and the water phase are mixed according to the mass ratio of 1: 2: 1: 2, heating to 80 ℃ after mixing, uniformly stirring, and circularly homogenizing for 10 times under the condition of 120MPa by a high-pressure homogenizer to obtain the whitening and compacting nano composition;
E. according to the mass ratio of 1: 1: 100, weighing succinoglycan, rhizobium bacterial gel and deionized water, and stirring for 30min at the stirring speed of 1500rpm to prepare a colloidal solution;
F. according to the mass ratio of 1: 5, weighing the whitening and tightening nano composition and the colloidal solution, and stirring at the rotating speed of 1500rpm for 15min to prepare an electrostatic spinning solution;
G. and F, transferring the electrostatic spinning solution obtained in the step F into a nano spider electrostatic spinning instrument, carrying out electrostatic spinning under the conditions of electrostatic field voltage of 15kv, spinning speed of 0.5mL/h and receiving distance of 20cm, and receiving with aluminum foil to obtain the nano fiber membrane with whitening and tightening effects.
The diameter of the nanofiber in the nanofiber membrane with whitening and tightening effects prepared by the method is 120nm, and the thickness of the nanofiber membrane is 50 microns. The nanofiber membrane with the whitening and tightening effects prepared by the method can be cut and cut according to actual needs, and can be used as a facial mask, an eye mask, a neck mask and the like, a part to be applied before use is wetted by moisturizing spray, then the prepared nanofiber membrane is applied, the moisturizing spray can be used again to ensure that the facial mask is fully wetted and completely attached to the skin, and the nanofiber membrane is completely absorbed by the skin after 5-30 minutes of use.
Example 2: a nanofiber membrane with whitening and tightening effects and a preparation method thereof are disclosed, and the preparation method comprises the following steps:
A. according to the mass ratio of 1: 1: 10 weighing pterostilbene, dipalmitoyl hydroxyproline and prinsepia utilis royle oil, mixing, heating, stirring until the mixture is completely dissolved, and cooling to room temperature to obtain an oil-soluble whitening and firming active ingredient; according to the mass ratio of 1: 1: 3: 1: 10 weighing fructose diphosphate trisodium, asiaticoside, hydrolyzed elastin, gynostemma pentaphylla leaf extract and polyhydric alcohol, mixing, heating, stirring to completely dissolve, and cooling to room temperature to obtain water-soluble whitening and firming active ingredients;
B. according to the mass ratio of 5: 1: 2 weighing polydimethylsiloxane, hydrogenated C6-14 alkene polymers and octyl dodecanol, heating and stirring to 80 ℃ to obtain an oil phase for later use;
C. according to the mass ratio of 1: 30 weighing hydrogenated lecithin and deionized water, uniformly stirring, and heating to 80 ℃ to obtain a water phase for later use;
D. the oil-soluble whitening and tightening active ingredient, the water-soluble whitening and tightening active ingredient, the oil phase and the water phase are mixed according to the mass ratio of 1: 1: 1: 2 heating to 80 ℃ after mixing, stirring uniformly, and then circularly homogenizing for 8 times under the condition of 100MPa by a high-pressure homogenizer to obtain the whitening and compacting nano composition.
E. According to the mass ratio of 1: 2: 100, weighing succinoglycan, rhizobium bacterial gel and deionized water, and stirring for 20min at the stirring speed of 1800rpm to obtain a colloidal solution;
F. according to the mass ratio of 1: 10, weighing the whitening and tightening nano composition and the colloidal solution, and stirring at a stirring speed of 1800rpm for 10min to prepare an electrostatic spinning solution;
G. and F, transferring the electrostatic spinning solution prepared in the step F into a nano spider electrostatic spinning instrument, performing electrostatic spinning under the conditions of electrostatic field voltage of 20kv, spinning speed of 0.2mL/h and receiving distance of 15cm, and receiving with aluminum foil to obtain the nano fiber membrane with whitening and tightening effects.
The diameter of the nanofiber in the nanofiber membrane with whitening and tightening effects prepared by the method is 135nm, and the thickness of the nanofiber membrane is 80 microns. The nanofiber membrane with the whitening and tightening effects prepared by the method can be cut and cut according to actual needs, and can be used as a facial mask, an eye mask, a neck mask and the like, a part to be applied before use is wetted by moisturizing spray, then the prepared nanofiber membrane is applied, the moisturizing spray can be used again to ensure that the facial mask is fully wetted and completely attached to the skin, and the nanofiber membrane is completely absorbed by the skin after 5-30 minutes of use.
Example 3: a nanofiber membrane with whitening and tightening effects and a preparation method thereof are disclosed, and the preparation method comprises the following steps:
A. according to the mass ratio of 1: 2: 10 weighing pterostilbene, dipalmitoyl hydroxyproline and prinsepia utilis royle oil, mixing, heating, stirring until the mixture is completely dissolved, and cooling to room temperature to obtain an oil-soluble whitening and firming active ingredient; according to the mass ratio of 1: 1: 3: 3: 6 weighing fructose diphosphate trisodium, asiaticoside, hydrolyzed elastin, gynostemma pentaphylla leaf extract and polyhydric alcohol, mixing, heating, stirring to completely dissolve, and cooling to room temperature to obtain water-soluble whitening and firming active ingredients;
B. according to the mass ratio of 4: 1: 1 weighing polydimethylsiloxane, hydrogenated C6-14 alkene polymers and octyl dodecanol, heating and stirring to 78 ℃ to obtain an oil phase for later use;
C. according to the mass ratio of 1: 15 weighing hydrogenated lecithin and deionized water, uniformly stirring, and heating to 78 ℃ to obtain a water phase for later use;
D. the oil-soluble whitening and tightening active ingredient, the water-soluble whitening and tightening active ingredient, the oil phase and the water phase are mixed according to the mass ratio of 1: 1: 1: 3, heating to 78 ℃ after mixing, uniformly stirring, and circularly homogenizing for 6 times under the condition of 100MPa by a high-pressure homogenizer to obtain the whitening and compacting nano composition.
E. According to the mass ratio of 1: 1: 100, weighing succinoglycan, rhizobium bacterial gel and deionized water, and stirring for 30min at the stirring speed of 1300rpm to obtain a colloidal solution;
F. according to the mass ratio of 1: 6, weighing the whitening and compacting nano composition and the colloidal solution, and stirring for 10min at a stirring speed of 1300rpm to prepare an electrostatic spinning solution;
G. and F, transferring the electrostatic spinning solution obtained in the step F to a nano spider electrostatic spinning instrument, carrying out electrostatic spinning under the conditions of electrostatic field voltage of 15kv, spinning speed of 0.6mL/h and receiving distance of 15cm, and receiving with aluminum foil to obtain the nano fiber membrane with whitening and compacting effects.
The nanofiber membrane with the whitening and tightening effects prepared by the method has the diameter of 150nm and the thickness of 60 microns. The nanofiber membrane with the whitening and tightening effects prepared by the method can be cut and cut according to actual needs, and can be used as a facial mask, an eye mask, a neck mask and the like, a part to be applied before use is wetted by moisturizing spray, then the prepared nanofiber membrane is applied, the moisturizing spray can be used again to ensure that the facial mask is fully wetted and completely attached to the skin, and the nanofiber membrane is completely absorbed by the skin after 5-30 minutes of use.
Example 4: a nanofiber membrane with whitening and tightening effects and a preparation method thereof are disclosed, and the preparation method comprises the following steps:
A. according to the mass ratio of 1: 1: 10 weighing pterostilbene, dipalmitoyl hydroxyproline and prinsepia utilis royle oil, mixing, heating, stirring until the mixture is completely dissolved, and cooling to room temperature to obtain an oil-soluble whitening and firming active ingredient; according to the mass ratio of 1: 2: 3: 2: 8, weighing fructose diphosphate trisodium, asiaticoside, hydrolyzed elastin, gynostemma pentaphylla leaf extract and polyhydric alcohol, mixing, heating, stirring to completely dissolve, and cooling to room temperature to obtain water-soluble whitening and firming active ingredients;
B. according to the mass ratio of 3: 1: 1 weighing polydimethylsiloxane, hydrogenated C6-14 alkene polymers and octyl dodecanol, heating and stirring to 80 ℃ to obtain an oil phase for later use;
C. according to the mass ratio of 1: 20 weighing hydrogenated lecithin and deionized water, uniformly stirring, and heating to 80 ℃ to obtain a water phase for later use;
D. the oil-soluble whitening and tightening active ingredient, the water-soluble whitening and tightening active ingredient, the oil phase and the water phase are mixed according to the mass ratio of 1: 1: 1: 3, heating to 80 ℃ after mixing, uniformly stirring, and circularly homogenizing for 8 times under the condition of 120MPa by a high-pressure homogenizer to obtain the whitening and compacting nano composition.
E. According to the mass ratio of 1: 1.5: 100, weighing succinoglycan, rhizobium bacterial gel and deionized water, and stirring for 25min at the stirring speed of 1800rpm to obtain a colloidal solution;
F. according to the mass ratio of 1: 8, weighing the whitening and tightening nano composition and the colloidal solution, and stirring at a stirring speed of 1800rpm for 10min to prepare an electrostatic spinning solution;
G. and F, transferring the electrostatic spinning solution obtained in the step F to a nano spider electrostatic spinning instrument, carrying out electrostatic spinning under the conditions of electrostatic field voltage of 18kv, spinning speed of 0.3mL/h and receiving distance of 16cm, and receiving with aluminum foil to obtain the nano fiber membrane with whitening and compacting effects.
The diameter of the nanofiber in the nanofiber membrane with the whitening and tightening effects prepared by the method is 140nm, and the thickness of the nanofiber membrane is 75 microns. The nanofiber membrane with the whitening and tightening effects prepared by the method can be cut and cut according to actual needs, and can be used as a facial mask, an eye mask, a neck mask and the like, a part to be applied before use is wetted by moisturizing spray, then the prepared nanofiber membrane is applied, the moisturizing spray can be used again to ensure that the facial mask is fully wetted and completely attached to the skin, and the nanofiber membrane is completely absorbed by the skin after 5-30 minutes of use.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (1)

1. The nanofiber membrane with whitening and tightening effects is characterized by being prepared by the following method:
A. according to the mass ratio of 1: 1-2: 10 weighing pterostilbene, dipalmitoyl hydroxyproline and prinsepia utilis royle oil, mixing, heating, stirring until the mixture is completely dissolved, and cooling to room temperature to obtain an oil-soluble whitening and firming active ingredient; according to the mass ratio of 1: 1-2: 3: 1-5: 5-10 weighing fructose diphosphate trisodium, asiaticoside, hydrolyzed elastin, gynostemma pentaphylla leaf extract and polyhydric alcohol, mixing, heating, stirring to completely dissolve, and cooling to room temperature to obtain water-soluble whitening and firming active ingredients;
B. according to the mass ratio of 2-5: 1: 1-2 weighing polydimethylsiloxane, hydrogenated C6-14 alkene polymers and octyl dodecanol, heating and stirring to 75-80 ℃ to obtain an oil phase for later use;
C. according to the mass ratio of 1: weighing hydrogenated lecithin and deionized water 10-30, stirring, heating to 75-85 deg.C, and collecting water phase;
D. the oil-soluble whitening and tightening active ingredient, the water-soluble whitening and tightening active ingredient, the oil phase and the water phase are mixed according to the mass ratio of 1: 1-2: 1: 1-4, heating to 75-85 ℃, uniformly stirring, and circularly homogenizing for 5-10 times under the condition of 90-120MPa by a high-pressure homogenizer to obtain the whitening and compacting nano composition;
E. according to the mass ratio of 0.5-1: 0.5-2: 100, weighing succinoglycan, rhizobium glue and deionized water, and stirring for 10-30min at the stirring speed of 1000-2000rpm to obtain a colloidal solution;
F. according to the mass ratio of 1: 2-10, weighing the whitening and tightening nano composition and the colloidal solution, and stirring at the rotating speed of 1000-1500rpm for 5-15min to prepare an electrostatic spinning solution;
G. and F, transferring the electrostatic spinning solution obtained in the step F into a nano spider electrostatic spinning instrument, carrying out electrostatic spinning under the conditions of electrostatic field voltage of 10-25kv, spinning speed of 0.1-1mL/h and receiving distance of 10-20cm, and receiving with aluminum foil to obtain the nano fiber membrane with whitening and tightening effects.
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