CN105581964A

CN105581964A - Product for rejuvenating and beautifying and preparation method thereof

Info

Publication number: CN105581964A
Application number: CN201610077801.7A
Authority: CN
Inventors: 姚蓉
Original assignee: Individual
Current assignee: Individual
Priority date: 2016-02-04
Filing date: 2016-02-04
Publication date: 2016-05-18

Abstract

The invention relates to a product for rejuvenating and beautifying and a preparation method thereof. The preparation method comprises the following steps: adding bletilla striata polysaccharide into distilled water which is 4-25 times of the weight of the bletilla striata polysaccharide and has a temperature of 50-70 DEG C; adding collagen hydrolysate having a molecular weight of lower than 3000, uniformly stirring, and insulating for 10-60 minutes; adding dihydromyricetin, pearl powder and bletilla striata gel, and immediately deoxidizing by adopting ultrasonic wave treatment to accelerate dissolution; drying in vacuum to reduce the moisture content to be lower than 30 percent after 3-30 minutes of ultrasonic wave treatment; and storing by adopting vacuum package for later use. According to the method, the solubility of dihydromyricetin can be remarkably improved by sufficiently utilizing the collagen hydrolysate and bletilla striata saccharides, and the stability of the dihydromyricetin can be facilitated since the pH value of the dihydromyricetin solution is partially acidic.

Description

A kind of skin-active cosmetics and preparation method thereof

Technical field

The present invention relates to a kind of skin-active cosmetics and preparation method thereof, be specifically related to a kind of skin-active cosmetics that add bletillaApplication in beautifying face, preserving moisture, belongs to the technical field that natural drug is applied.

Background technology

Dibydro myricetrin is one of ampelopsis grossdentata main active ingredient of claiming again vine tea, is traditional medication among the people, once by extensivelyBe used for the treatment of the infectious diseases such as skin disease, furuncle and osteomyelitis, acute lymphoblastic inflammation, can suppress multiple harmful germ. Dihydro poplarThe time of occurrence of syphilis energy delaying skin chloasma and senile plaque expelling, in 25 DEG C of water, solubility is 4%, in hot water, solubility is larger;Be soluble in methyl alcohol, ethanol and acetone, the atomic ethyl acetate that is dissolved in; Be insoluble in chloroform, benzinum. Lin Shuying etc. are steady to DMYQualitative and influence factor is investigated, and confirms that dihydromyricetin cellulose solution is easily oxidized, and less stable, is being no more than100 DEG C, the heat time is no more than 30min and acidity and neutrallty condition and can keeps its steady chemical structure, and transition state goldBelong to ion A l³⁺，Fe³⁺，Cu²⁺Deng the oxidation of dibydro myricetrin is played to inducing catalysis effect.

Collagen forms triple helix structure by 3 α polypeptide chains, and its molecular structure is very stable, and relative molecular weight is at 30KDaAbove. Collagen belongs to large molecule rank protein, enters after human body and needs to transform process by complicated protein, could quiltAbsorption of human body and utilization, absorption rate only rests on 2.5%. Hydrolyzed Collagen is exactly the processing of collagen through scienceAfter method, make, the collagen polypeptide that relative molecular weight is less, widely used molecular weight, can be completely molten below 3000DaXie Yushui, its utilization rate that is absorbed by the body is higher, and can promote the absorption of other protein in food.

Hydrolyzed Collagen contains several amino acids, wherein maximum with glycine, be secondly alanine, glutamic acid, arginine,Hydroxyproline etc., total amino acid content accounts for the more than 90% of Hydrolyzed Collagen, wherein the content of strong proline up to11.8--12.6%. These amino acid are important source material of the synthetic self collagen albumen of the mankind. The mankind only have the each of absorption q.sSeed amino acid, could synthesize self required range protein, maintains form and the structure of skin and histoorgan, repairs each damageInjured tissue.

Bletilla polysaccharide in bletilla pseudobulb is main pharmacodynamics position, and its main component is the water-soluble polysaccharides such as Glucomannan. BletillaThe physicochemical property of glue and Arabic gum, tragacanth are similar, but stickiness is special. Bletilla haemostatic effect is definitely reliable, with contained largeAmount bletilla glue is relevant. Bletilla glue film forming has stronger adhesion, spreads on blutpunkte or the face of animal, can be at once with surface of a wound fusionBe difficult to peel off, and be only that the one side that contacts wound dissolves, so just can stop blooding rapidly and protect from infection. Experiment showed, whiteAnd extract has the clotting time of shortening, suppresses the effect of human body to cellulose dissolution, can form rapidly artificial thrombus, to woundHemostasis or visceral hemorrhage clinical treatment all have good therapeutic effect, safe and without any side effects.

Bletilla glue is widely used in the digestive tract ulcers such as stomach, esophagus, duodenum at present, the respiratory mucosa ulcer such as nasal cavity, oral cavity,The mucosal ulcer of the gynecological disease such as uterus, vagina, and the clinical treatment such as skin injury, sore, burn and scald, total effective rate existsMore than 90%, the healing of some case type is efficient up to 100%, and curative effect be subject to age size, course of disease length,The impact of the factor such as individual difference and different occupation is less.

Bletilla glue belongs to the natural polymer of molecular weight, but no antigen, without pyrogenicity, better with animal body tissueGround is compatible, and can be by the absorption of degrading lentamente. Medicine worker utilizes the premium properties of bletilla glue to repair damaged tissue, makes certainA little surgical disease treatments need not be performed the operation and also can be solved. For example, Zhu Zhian etc. makes bletilla glue and the decalcification bone through specially treatedThe biological skull material of plyability, for repairing skull defeci, at compatibility, plasticity, free constancy, and sterilization sclerosisProperty aspect all obtains very promising result. To the phlegm pipe case after some perforated ulcer, anastomosis, use oral bletilla glue or whiteAnd treated powder, all there is good filling repair.

Partial interventional therapy technology (chemotherapy) is widely used in malignant tumour and faces. In diseased region blood vessel, give high concentration medicineEmbolism chemical therapeutic, can make malignant tumour obviously downright bad, and the survival of patients phase extends, and survival rate improves. But the conventional suppository of chemotherapy is as brightGlue, sponge, autologous sludged blood, stainless steel coil etc., all exist many deficiencies, causes the long-term curative effect of chemotherapy not satisfied.Bletilla is gluing makes a concerted effort by force, and meeting water can slowly expand, and degraded absorbs slowly,, hemostasis hemorrhage for internal organs as TAE agent andThe clinical treatment of malignant tumour all can reach complete effect of embolization in different tube diameters blood vessel, and can with various antineoplasticsMix, do not cause again systemic medication bad reaction, curative effect is obviously better than gelatin, sponge embolism, is medium-term and long-term chemotherapy is managedThe natural embolism materials of thinking.

Studies have shown that, excessive free radical in animal body, can cause cellular damage and death, accelerates skin senescence and wrinkle and producesRaw. Rui Haiyun etc. study discovery, and bletilla neutral polysaccharide has the ability of obvious removing free radical, and it removes active in vitamin E. Bletilla glue can be used as the trophism cosmetic material of delaying skin aging accordingly.

Bletilla gumminess excellent, equals to Arabic gum, tragacanth gum, can be used as the thickener, outstanding of food, cosmetic fieldFloat agent, NMF and assistant for emulsifying agent, also can be used as the host material of good excipient, powder, film, gel. BletillaGlue, bletilla alkaloid, and other active components of bletilla, at inhibition tumor cell hyperplasia, delay skin aging, and thickening,Suspension, moisturizing, help the aspect such as emulsification and excipient to there are extensive market prospects. Especially the Rhizoma Bletillae of different molecular weight,Aspect hemostasia and promoting granulation new drug development, there are very wide market prospects.

Summary of the invention

Bletilla gel can form thin film at skin surface, and water-retaining property is stronger, has skin moisture-keeping effect, and bletilla polysaccharide again canPrevent microbial growth. Dibydro myricetrin solubility in normal-temperature water is little, and itself does not have stickiness. By dibydro myricetrin and glueFormer protolysate is fixed in bletilla polysaccharide relatively, farthest makes skin surface absorb these active ingredient to the greatest extent, again can simultaneouslyMake skin moisturizing, promote widely the metabolism of skin, reach the effect of skin-active. To be present in bletilla many for dibydro myricetrin in additionIn sugar, can reduce the touch opportunity of dibydro myricetrin and oxygen, prevent that as much as possible dibydro myricetrin is not oxidized.

Therefore, first object of the present invention is to provide a kind of skin-active cosmetics and preparation method thereof: get bletilla polysaccharide 15～85Part adds 50-70 DEG C of distilled water of 4～25 times of weight, then adds the collagen hydrolysate (small peptide of molecular weight below 3000Material) 5～30 parts, after stirring, be incubated 10～60min, then add 3～15 parts of dibydro myricetrins, pearl powder 10～1510～25 parts of part and bletilla gels, adopt ultrasonic wave to process deoxidation accelerate dissolution at once, and ultrasonic wave is processed after 3～30min, trueEmpty being dried is reduced to below 30% its water content, adopts vacuum packaging to save backup.

In one embodiment, skin-active cosmetics and preparation method thereof are made up of with following weight portion each raw material composition: get20～80 parts of bletilla polysaccharides add 50-70 DEG C of distilled water of 4～25 times of weight, then add the collagen of molecular weight below 30005～25 parts of hydrolysates (small peptide material), are incubated 10～60min after stirring, then add 3～10 parts of dibydro myricetrins,10～25 parts of 10～15 parts of pearl powders and bletilla gels, adopt ultrasonic wave to process deoxidation accelerate dissolution at once, ultrasonic wave processing 3～After 30min, vacuum drying is reduced to below 30% its water content, adopts vacuum packaging to save backup.

In a specific embodiments, wherein each material composition forms with following weight portion: get 30～60 parts of bletilla polysaccharides and addEnter 50-70 DEG C of distilled water of 4～25 times of weight, then add the collagen hydrolysate (small peptide material) of molecular weight below 300010～20 parts, after stirring, be incubated 10～60min, then add 4～8 parts of dibydro myricetrins, 10～15 parts of pearl powders and whiteAnd 10～25 parts of gels, adopt at once ultrasonic wave to process deoxidation accelerate dissolution, ultrasonic wave is processed after 3～30min, vacuum dryingIts water content is reduced to below 30%, adopts vacuum packaging to save backup.

In another embodiment, wherein each material composition forms with following weight portion: get 40 parts of bletilla polysaccharides and add60 DEG C of distilled water of 15 times of weight, then add 15 parts of the collagen hydrolysate (small peptide material) of molecular weight below 3000,After stirring, be incubated 30min, then add 20 parts of 6 parts of dibydro myricetrins, 10 parts of pearl powders and bletilla gels, adopt at once superSonicated deoxidation accelerate dissolution, ultrasonic wave is processed after 25min, and vacuum drying is reduced to below 30% its water content, adoptsVacuum packaging saves backup.

Described dibydro myricetrin and collagen hydrolysate, directly buy from market, requires dihydromyricetin cellulose content >=98.8%,Collagen hydrolysate content >=98.5%.

Second object of the present invention is to provide a kind of preparation method of bletilla polysaccharide, and by it for skin-active cosmetics, stepComprise:

(1) pulverize dry bletilla, add after petroleum ether and stirring 10～30min, leave standstill layering in 1～3 hour removal and contain stoneThe upper solution of oil ether, repeats once, obtains precipitation I.

(2) in precipitation I, add a certain amount of water to wash, collect water lotion, be heated with stirring to 70～85 DEG C, protectAfter temperature 20～80min, the centrifugal 10～20min of 6000rpm～9000rpm, obtains supernatant, goes precipitation.

(3) supernatant is evaporated to certain volume at 50～65 DEG C, then adds 95% ethanol to final concentration to reach 75%Above, alcohol precipitation 10-20h, filters, and obtains filter residue and is bletilla polysaccharide.

In one embodiment, benzinum described in step (1) is the benzinum that adopts 60～90 DEG C of boiling range specifications, its volumeL is 2～6:1 with bletilla weight kg ratio.

In one embodiment, described in step (2), adding the volume L of the water yield and bletilla weight kg ratio is 2～4:1.

In one embodiment, certain volume described in step (3) refers to the 1/20-1/50 of original volume.

In one embodiment, described in step (3) filter: membrane aperture be 0.22 μ m ceramic membrane filter once.

The 3rd object of the present invention is to provide a kind of preparation method of bletilla gel, and by it for bletilla moisturizing gel products,Step comprises:

(a) get the water that 20～50 parts of refining bletilla polysaccharides add 4～10 times of weight, add 5～10 parts, acrylic acid to stir mixedClose after 10～30min, obtain mixture;

(b) in mixture, add 10% ammonium persulfate and TEMED again, after rapid mixing, under room temperature, place 1～3 hour,After adding a certain amount of water to stir, 5000～10000rpm is centrifugal again, removes supernatant, repeats once, obtains precipitation VI;

(c) precipitation VI is placed on to room temperature in vacuum drier and carries out being slowly dried to obtain dry thing, be bletilla gel.

In one embodiment, the volume μ L of 10% ammonium persulfate described in step (b) and the volume mL ratio of mixture are20～50:100; The volume μ L of TEMED (tetramethylethylenediamine) is 10～50:100 with the volume mL ratio of mixture;It is described that to add the amount mL of water and the volume mL ratio of mixture be 20～50:10.

The compound method of 10% ammonium persulfate is for taking 10g ammonium persulfate, and water is settled to 100ml after dissolving.

Hemostasis, skin that above-mentioned skin-active cosmetics or bletilla polysaccharide or bletilla gel can be directly used in various patient's wounds are moreClose etc. in material, also can be directly used in the application of the aspect such as water-keeping material in cosmetics, also can be for suppressing various pathogens etc.In medical material.

Technique effect

1, make full use of collagen hydrolysate and bletilla polysaccharide and can obviously promote the solubility of dibydro myricetrin, but protect again simultaneouslyDemonstrate,prove the pH value slant acidity of its solution, be also beneficial to the stability of dibydro myricetrin.

Though 2, material therefor of the present invention all has skin-active effect, collaborative rear effect is more remarkable mutually, makes full use of again whiteAnd the water imbibition of polysaccharide is stronger, in playing skin moisture-keeping effect, make again the touch opportunity of dibydro myricetrin and oxygen reduce.

3, bletilla polysaccharide extracting method of the present invention, can effectively improve the recovery rate of bletilla polysaccharide, effectively prevents bletilla polysaccharideHydrolysis.

4, the present invention utilizes the local fixation of bletilla polysaccharide, reinforced collagen hydrolysate and dihydro under adequate water conditionThe repair of myricetin to skin, promotes the effect of skin-active beauty treatment.

Detailed description of the invention

Below, the present invention will be further detailed with embodiment, but it is not limited to any or the class of these embodimentLike example.

Embodiment 1: the preparation method of bletilla polysaccharide

Pulverize dry bletilla 100kg, directly add after the petroleum ether and stirring 20min of 200L, leave standstill layering in 1 hour removal and containThere is the upper solution of benzinum, repeat once, obtain precipitation I; In precipitation I, add 400L water, be heated with stirring to 70-85 DEG C,After insulation 60～70min, the centrifugal 15～20min of 7000rpm, obtains supernatant, goes precipitation. By supernatant at 50-65 DEG CBe evaporated to 1/30 of original volume, then add 95% ethanol to final concentration to reach more than 75%, alcohol precipitation 15 avoids everyday-20H, the ceramic membrane filter that carries out 0.22 μ m once obtains filter residue and is bletilla polysaccharide product. Measure through anthrone-sulphate method, produceIn product, soluble sugar content is more than 99.5%.

Embodiment 2: the preparation method of bletilla gel

Take 35 grams of refining bletilla polysaccharides, add the water of 150 grams, add 8 grams of acrylic acid to be uniformly mixed after 10～30min,Obtain mixture 150mL left and right. In mixture, add 10% ammonium persulfate 50 μ L and TEMED40 μ L again, mixed fastClose under rear room temperature and place 2 hours, then add the rear 8000rpm of water stirring of 250mL centrifugal, remove supernatant, then to precipitationIn add 250mL water stir after 8000rpm centrifugal, go supernatant must precipitate VI. Precipitation VI is placed on to vacuum drierMiddle room temperature carries out being slowly dried to obtain dry thing, is 45 grams of bletilla gels.

Embodiment 3: beauty treatment is except the preparation of spot product

Get 60 DEG C of distilled water that 50 grams of bletilla polysaccharides add 400 grams, then add the collagen hydrolysate of molecular weight below 3000(small peptide material) 15 grams, is incubated 30min after stirring, then adds 6 grams of dibydro myricetrins, 15 grams of pearl powders and bletilla20 grams of gels, adopt ultrasonic wave to process deoxidation accelerate dissolution at once, and ultrasonic wave is processed after 20min, and vacuum drying makes its water contentBe reduced to below 30%, obtain 96 grams of skin-active cosmetics, and adopt vacuum packaging to save backup, get 1 gram of sample warpThe content that HPLC method detects dibydro myricetrin is 5.55%.

Control Example 1

35 DEG C of distilled water getting 400mL add the bletilla polysaccharide of 50 grams, after bletilla polysaccharide dissolves completely, then add 6 grams15 grams of dibydro myricetrin and pearl powders cannot dissolve completely under ul-trasonic irradiation, need be heated to 80 DEG C of dissolving final vacuums dryMake its water content be reduced to 30%, 75 grams of the products that obtains, and adopt vacuum packaging to save backup, get 1 gram of sample warpThe content that HPLC method detects dibydro myricetrin is 5.11%.

Embodiment 4: beauty treatment is except the preparation of spot product

Get 70 DEG C of distilled water that 70 grams of bletilla polysaccharides add 500 grams, then add the collagen hydrolysate of molecular weight below 3000(small peptide material) 25 grams, is incubated 40min after stirring, then adds 8 grams of dibydro myricetrins, 15 grams of pearl powders and bletilla20 grams of gels, adopt ultrasonic wave to process deoxidation accelerate dissolution at once, and ultrasonic wave is processed after 15min, and vacuum drying makes its water contentBe reduced to below 20%, obtain beauty treatment except 123 grams of spot products, and adopt vacuum packaging to save backup, get 1 gram of sample warpThe content that HPLC method detects dibydro myricetrin is 8.02%.

Embodiment 5: the content of dibydro myricetrin in various products

Various sample 50g are placed after a period of time under 37 DEG C of conditions, get 1 gram of sample and detect dibydro myricetrin through HPLC methodContent is in table 1. In the obtained product of control Example 1, dihydromyricetin cellulose content decrease speed is the fastest, reaches 24.46%, and thisThough in bright products obtained therefrom, dihydromyricetin cellulose content has decline, lower, be 5.74%～6.49%.

The content of table 1 dibydro myricetrin

Embodiment 6: the result for the treatment of that uses this product

Usage and consumption: when use, first clean after face, directly its product is attached to face affected part, two days once.

Clinic trial observations: test of cure 30 examples altogether, wherein male 16 examples, female's 14 examples, freckle patient's 21 examples,Butterfly macules patient 9 examples, at minimum 15 years old of age, maximum 65 years old, the course of disease was the shortest 2 years, the longest 30 years. Diagnostic criteria:Be all diagnostic criteria at hospital dermatology department, surgery through doctor's clinical diagnosis result according to patient before test, face freckle, butterfly macules.Methods for the treatment of: patient first cleans face, directly its product is attached to face affected part, and two days are once, 3 months the shortest courses for the treatment of,Long 5 months courses for the treatment of. Criterion of therapeutical effect: after external application medicament of the present invention, facial spot all disappears for curing; Spot reduces, and subtractsLittle is effectively, without obviously changing into invalid (poor).

Interpretation of result: altogether test 30 examples, wherein butterfly macules patient 9 examples, freckle patient's 21 examples, the male sex's 16 examples, women 14Example, through external application product of the present invention, 3 months the shortest courses for the treatment of, 5 months the longest courses for the treatment of, total effective rate 96%, cure rate 86%,Invalid 4%.

Claims

1. skin-active cosmetics and preparation method thereof: get 15～85 parts of bletilla polysaccharides and add 4～25 times of weight50-70 DEG C of distilled water, then add 5～30 parts of the collagen hydrolysate of molecular weight below 3000, after stirring, be incubated 10～60min, then add 10～15 parts of 3～15 parts of dibydro myricetrins and pearl powders, adopt at once ultrasonic wave to process deoxidation accelerate dissolution,Ultrasonic wave is processed after 3～30min, and vacuum drying is reduced to below 30% its water content, adopts vacuum packaging to save backup.

2. skin-active cosmetics of claim 1 and preparation method thereof are made up of with following weight portion each raw material composition: get bletilla20～80 parts of polysaccharide add 50-70 DEG C of distilled water of 4～25 times of weight, then add the collagen hydrolysate of molecular weight below 30005～25 parts of things, are incubated 10～60min after stirring, then add 10～15 parts of 3～10 parts of dibydro myricetrins and pearl powders,Adopt at once ultrasonic wave to process deoxidation accelerate dissolution, ultrasonic wave is processed after 3～30min, and vacuum drying is reduced to its water contentBelow 30%, adopt vacuum packaging to save backup.

3. skin-active cosmetics of claim 1 and preparation method thereof, wherein each material composition forms with following weight portion: get whiteAnd 30～60 parts of polysaccharide add 50-70 DEG C of distilled water of 4～25 times of weight, then add the collagen water of molecular weight below 3000Separate 10～20 parts of things, after stirring, be incubated 10～60min, then add 10～15 parts of 4～8 parts of dibydro myricetrins and pearl powders,Adopt at once ultrasonic wave to process deoxidation accelerate dissolution, ultrasonic wave is processed after 3～30min, and vacuum drying is reduced to its water contentBelow 30%, adopt vacuum packaging to save backup.

4. skin-active cosmetics of claim 1 and preparation method thereof, wherein each material composition forms with following weight portion: get whiteAnd 40 parts of polysaccharide add 60 DEG C of distilled water of 15 times of weight, then add 15 parts of the collagen hydrolysate of molecular weight below 3000,After stirring, be incubated 30min, then add 10 parts of 6 parts of dibydro myricetrins and pearl powders, adopt at once ultrasonic wave to process deoxidation and addInstant solution, ultrasonic wave is processed after 25min, and vacuum drying is reduced to below 30% its water content, adopts vacuum packaging to preserve standbyWith.

5. the preparation method of a kind of bletilla polysaccharide of claim 1-4, and by it for skin-active cosmetics, step comprises:

(3) supernatant is evaporated at 50～65 DEG C to the 1/20-1/50 of original volume, then adds 95% ethanol to wholeConcentration reaches more than 75%, and alcohol precipitation 10-20h, filters, and obtains filter residue and is bletilla polysaccharide.

6. the method for claim 4, benzinum described in step (1) is the benzinum that adopts 60～90 DEG C of boiling range specifications, its bodyLong-pending L is 2～6:1 with bletilla weight kg ratio.

7. the method for claim 4, described in step (2), adding the volume L of the water yield and bletilla weight kg ratio is 2～4:1.

8. the preparation method of the bletilla gel of claim 1～3, its concrete steps comprise:

9. the method for claim 8, the volume μ L of 10% ammonium persulfate described in step (b) with the volume mL ratio of mixture is20～50:100; The volume μ L of TEMED (tetramethylethylenediamine) is 10～50:100 with the volume mL ratio of mixture;It is described that to add the amount mL of water and the volume mL ratio of mixture be 20～50:10.

10. claim 1～9 obtains skin-active cosmetics or bletilla polysaccharide or bletilla gel and can be directly used in various patientsIn the material such as hemostasis, skin healing of wound, also can be directly used in the application of the aspect such as water-keeping material in cosmetics, also can useIn suppressing the medical materials such as various pathogens.