CN109431934A - A kind of wild pepper seed hair sun-screening agent and preparation method thereof - Google Patents

A kind of wild pepper seed hair sun-screening agent and preparation method thereof Download PDF

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CN109431934A
CN109431934A CN201811435670.0A CN201811435670A CN109431934A CN 109431934 A CN109431934 A CN 109431934A CN 201811435670 A CN201811435670 A CN 201811435670A CN 109431934 A CN109431934 A CN 109431934A
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pepper seed
wild pepper
hair
sun
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CN109431934B (en
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王增兰
张圣强
周建华
王海韵
聂东婧
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Yami Technology Guangzhou Co ltd
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Shandong Normal University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics 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]
    • A61K8/9794Liliopsida [monocotyledons]
    • 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
    • A61K8/645Proteins of vegetable origin; 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
    • A61K8/96Cosmetics 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
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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  • Health & Medical Sciences (AREA)
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Abstract

The present invention relates to a kind of wild pepper seed hair sun-screening agents, belong to cosmetic technical field.The sun-screening agent is made of the raw material of following parts by weight: vitamin C and/or vitamin E add up to (0.8-1.2) part, wild pepper seed kind hull melanin (2-4) part, wild pepper seed albumen peptide solution (25-31) part, wild pepper seed kernel extracting solution (53-67) part, garlic juice (100-112) part of deodorization, Bletilla glucomannan (115-145) part, Pu'er cooked tea leaching liquor (425-475) part.The present invention distinguishes effective component extracting from wild pepper seed, auxiliary hair dyeing function strong, sun-proof with inoxidizability;Also have the effects that nourish hair, sterilization.The present invention is devised with sterilization, moist and anti-sunlight function odorless garlic juice;With the Pu'er cooked tea leaching liquor for absorbing isolation ultraviolet effect and fixation, hair care effect;Bletilla glucomannan with colour fixation and nourishes effect makes the hair sun-screening agent have good sun-proof, auxiliary hair dyeing, nourish and repair the multi-efficiencies such as hair.

Description

A kind of wild pepper seed hair sun-screening agent and preparation method thereof
Technical field
The invention belongs to cosmetic technical field more particularly to a kind of hair colors for after hair dyeing especially under light illumination It is easy to decompose the wild pepper seed hair sun-screening agent and preparation method thereof for fading and developing.
Background technique
Hair dyeing product is required in many people's daily lifes, but the chemical reaction in hair dye can all change hair The structure on surface and inside, causes the hair cuticle of hair to tilt, has de- sticking phenomenon, when hair surface becomes coarse, cause light Scattering, makes hair tarnish;The protein-loss of hair, crystallinity decline, cause water holding capacity to reduce, under tensile strength Drop, the variation of the physical properties such as elasticity and toughness decline;Simultaneously because impaired hair loses the protection structure of outer layer, it is internal Also occur Voiding, thus be difficult for pigment to be effectively retained in hair.If just the hair after hair dyeing is for a long time by purple Outside line irradiation, not only allows the hair after hair dyeing more fragile, is also unfavorable for maintaining color development.
Research is found: protein is easy to happen photochemical degradation in hair, and ultraviolet light can also accelerate amino acid oxygen The oxidation of carbon between change and polypeptide chain, because ultraviolet light can be generated by light degradation amino acid and with photosensitivity material effect A large amount of active oxygen radical, so as to cause the change of hair fiber.Free radical can using the steam in water or atmosphere as medium, Series reaction occurs, these free radicals there are significantly damages to hair protein, especially keratin, and melanocyte is caused to drop Solution makes hair that color change occur.In addition the damage ratio ultraviolet light caused by lipid layer of the visible light in daylight is big, hair Lipid layer, which is illuminated by the light, to be also easy to produce lipid peroxide and is damaged, and is had to the integrality, hydrophobicity, the hardness of hair shaft that maintain hair Significant negative effect.
Currently, although there are many sunscreen product in the market, mostly based on antitan agent.Physical sunscreen skin products are More greasy thick and heavy using reflective principle, to be coated onto certain thickness can just play a role, and such as be used in that hair is sun-proof to be made Hair seems that greasy rare, hair style is difficult to keep, and influences beauty and brings sense of discomfort to user;And in bacterium, ultraviolet light etc. Under the action of, so that grease deterioration, hair follicle is blocked, scalp health system is destroyed, and then causes dandruff, head to be itched, the diseases such as alopecia Shape;Chemical sunscreen skin products are the ultraviolet lights absorbed in sunlight using chemical reaction, and chemical sunscreen additive is more, makes for a long time It is larger with being injured to hair and scalp;And the melanocyte inside hair can react with part chemical sunscreen additive, cause to contaminate The color fading of hair.
To sum up, the hair color especially easy sun-proof production of hair faded under light illumination after solving hair dyeing that there is presently no a kind of Product, therefore, it is necessary to study a kind of new hair sunscreen products, and at least solve, part is mentioned above to deposit in the prior art The problem of.
Summary of the invention
For above-mentioned problems of the prior art, the present invention is intended to provide a kind of wild pepper seed hair sun-screening agent and its system Preparation Method.The present invention distinguishes effective component extracting from wild pepper seed, auxiliary hair dyeing function strong, sun-proof with inoxidizability, simultaneously Also have the effects that nourish hair, sterilization.Have sterilization, moist and anti-sunlight function deodorization big in addition, the present invention has also been devised Garlic juice;With the Pu'er cooked tea leaching liquor for absorbing isolation ultraviolet effect and fixation, hair care effect;And there is colour fixation With the ingredients such as the Bletilla glucomannan of nourishes effect, hair sun-screening agent of the invention is made to have good sun-proof and auxiliary hair dyeing effect, and With nourishing and repair the multi-efficiencies such as hair.
The first purpose of this invention is to provide a kind of wild pepper seed hair sun-screening agent.
Second object of the present invention is to provide a kind of preparation method of wild pepper seed hair sun-screening agent.
Third object of the present invention is to provide a kind of wild pepper seed hair dyeing sunscreen spray.
Fourth object of the present invention is to provide the application of above-mentioned wild pepper seed hair sun-screening agent.
For achieving the above object, specifically, the invention discloses following technical proposals:
Firstly, the present invention discloses a kind of wild pepper seed hair sun-screening agent, the sun-screening agent by following raw material in parts by weight Than manufactured: vitamin C and/or vitamin E add up to 0.8-1.2 parts, 2-4 parts of wild pepper seed kind hull melanin, wild pepper seed protein peptides 25-31 parts of solution, 53-67 parts of wild pepper seed kernel extracting solution, deodorization 115-145 parts of 100-112 parts of garlic juice, Bletilla glucomannan, general 425-475 parts of Pu'er tea ripe tea leaching liquor.
Preferably, the sun-screening agent following raw material by ratio of weight and the number of copies made of: vitamin C and/or vitamin E close Meter 1 part, 3 parts of wild pepper seed kind hull melanin, 28 parts of wild pepper seed albumen peptide solution, 60 parts of wild pepper seed kernel extracting solution, deodorization it is big 106 parts of garlic juice, 130 parts of Bletilla glucomannan, 450 parts of Pu'er cooked tea leaching liquor.
Further, in above-mentioned wild pepper seed hair sun-screening agent, the mass ratio of the vitamin C and vitamin E is 5:8.
Further, in above-mentioned wild pepper seed hair sun-screening agent, by the pH of wild pepper seed hair sun-screening agent control 6.0-6.5 it Between, the characteristic of wild pepper seed protein peptides can be preferably kept in this way, and main component is antibacterial peptide, each group in wild pepper seed enzymolysis protein peptide At pH acidity on the weak side after combining between ingredient, and epidermis hair scale sector-meeting is closed up when hair chance weak acid, and hair good texture has light Pool, hair dyeing effect is good, can also moisten scalp skin and hair well.
Above-mentioned wild pepper seed hair sun-screening agent of the invention has the effect of sun-proof and auxiliary hair dyeing, and can moisten moisturizing head Hair, repairs the multi-efficiencies such as impaired hair, this is because: the wild pepper seed melanin that (1) present invention is extracted from wild pepper seed kind skin , dye black function strong with inoxidizability can play the main function of sun-proof auxiliary hair dyeing;Wild pepper seed kernel extracting solution contains A large amount of alpha-linolenic acids and other nutriments can play the role of nourishing hair;Wild pepper seed albumen peptide solution has sterilization etc. Function;(2) garlic juice of deodorization have the function of sterilization, moisten and it is sun-proof;And Pu'er cooked tea leaching liquor has absorption isolation purple Outside line and fixation, hair care effect;(3) Bletilla glucomannan has colour fixation and nourishes effect;(4) VE can effectively prevent Fructus Zanthoxyli oil It is oxidized, improves the anti-oxidant efficiency of Fructus Zanthoxyli oil;Vitamin C has unsaturated fat anti-oxidant, in protection natural oil The effect of density, alleviation trichoxerosis between acid, enhancing hair horn cell.
Secondly, the present invention discloses a kind of preparation method of wild pepper seed hair sun-screening agent, include the following steps:
Wild pepper seed is isolated to the shell of the wild pepper seed of the wild pepper seed kind Renhe black of white, it is spare.
(1) preparation of wild pepper seed kind hull melanin:
S1, by the shell of black wild pepper seed, coarse crushing is removed with dehydrated alcohol extraction and is deoiled, dries shell after separation, fine crushing, Sieving, obtains the wild pepper seed shell powder of brown;
S2, wild pepper seed shell powder is placed in NaOH solution and extracts melanin, pH is then adjusted to 2.5-3 progress acid and is sunk, Obtain the unformed powder of dark-brown, as wild pepper seed pigment crude product;
S3, solution is made in wild pepper seed pigment crude product, is mixed with the enzyme solution containing alkali protease and carries out the de- egg of enzymatic isolation method It is white;PH is adjusted to 2.5-3 and carries out the heavy wild pepper seed kind hull melanin to get black of acid.
In step S1, extraction is to extract 1h at 80 DEG C under the constant temperature.
In step S1, the liquid ratio of the wild pepper seed shell and dehydrated alcohol are as follows: 1g:5mL.
In step S1, the sieving was 180~200 meshes.
In step S2, the concentration of the NaOH solution is 1.1-1.3moL/L, preferably 1.2moL/L.
In step S2, the liquid ratio of the wild pepper seed shell powder and NaOH solution are as follows: 1g:24.6mL.
In step S2, the reaction condition for extracting melanin are as follows: extract 2h at 70 DEG C, extract 2 times altogether, extracting solution closes And it uses;Preferably, pH 2.5 carry out acid are adjusted to sink.
In step S3, the concentration of alkali protease (vigor 10000U/g) solution is 10g/L, and using preceding at 4 DEG C Preservation.
In step S3, the wild pepper seed pigment crude product solution concentration is 1mg/mL;The investment of the alkaline protease solution Amount is the 6% of wild pepper seed pigment crude product solution volume;
In step S3, the Deproteinated reaction condition of enzymatic isolation method is to digest 0.5-2h at 50 DEG C, pH=9;Finally by pH It is heavy to be adjusted to 2.5 carry out acid.
(2) preparation of wild pepper seed kernel extracting solution
By the wild pepper seed kernel of white, coarse crushing is extracted at a constant temperature with dehydrated alcohol, is separated, the white after must deoiling Wild pepper seed kind Renhe leaching liquor;Ethyl alcohol is distilled off to get flaxen wild pepper seed kernel extracting solution in leaching liquor.
Further, in step (2), extraction is to extract 2h at 80 DEG C under the constant temperature.
Further, in step (2), the liquid ratio of the wild pepper seed kind Renhe dehydrated alcohol of the white is 1g:10mL.
(3) preparation of wild pepper seed albumen peptide solution
Alkali extraction-acid precipitation is used to the wild pepper seed kernel of the white after deoiling first, the wild pepper seed egg of white is prepared It is white;Then wild pepper seed albumen is preheated after mixing with deionized water, is adjusted to the pH of mixed liquor after reaching predetermined temperature 2.5-3 is added the extraction that pepsin carries out wild pepper seed protein peptides, carries out destroy the enzyme treatment after extraction, be finally centrifuged, Supernatant pH is adjusted to meta-alkalescence to get transparent more sticky wild pepper seed albumen peptide solution.
Further, in step (3), the concentration of substrate of the wild pepper seed albumen in deionized water is 4.9%.
Further, in step (3), the pH of mixed liquor is adjusted to 2.5 after being 32 DEG C by the predetermined temperature.
Further, in step (3), the pepsin (Rate activity 1:3000-1:3500) and wild pepper seed protein solution Mass ratio be 0.9:100, the extraction time be 3h.
Further, in step (3), the destroy the enzyme treatment, which refers to, keeps the temperature 15min in 90 DEG C of water bath with thermostatic control, is cooled to room Temperature.
Further, in step (3), the centrifugation, which refers to, is centrifuged 10min under the revolving speed of 8000r/min.
(4) preparation of the garlic juice of deodorization
By blanching 5-10s after garlic peeling, expect that water quality ratio is that 1:1 mashes garlic juice;Then by garlic juice and edible oil It is sufficiently mixed, is placed in be stored under greenhouse (25-30 DEG C) and soaks 48h;Waving with penetrating odor in edible oil extract garlic juice Object is sent out, is centrifuged after standing, the intermediate garlic juice in absinthe-green clear liquid to get deodorization is extracted.
Preferably, in step (4), selection is fresh, not damaged, nothing goes rotten, do not germinate and full and glossiness intact big Garlic is as raw material.
Further, in step (4), the edible oil includes soybean oil, peanut oil, rapeseed oil etc..
Further, in step (4), the volume ratio of the garlic juice and edible oil are as follows: 100:1-15.
(5) preparation of Bletilla glucomannan
Bletilla striata powder is impregnated with deionized water, is then filtered, by filtrate concentration gelled to get the gelatinous bletilla striata Glue.
Further, in step (5), the additional amount of the deionized water is 15-20 times of bletilla striata silty amount.
Further, in step (5), the soaking time is 1-2h, and soaking temperature is 90-95 DEG C.
Further, in step (5), 1/4-1/5 times of original volume is concentrated the filtrate to get gelatinous Bletilla glucomannan.
(6) preparation of Pu'er cooked tea leaching liquor
It is filtered after Pu'er cooked tea stem tea is soaked in water, takes filtrate;It is big by being extracted in Pu'er cooked tea residue, step (4) It is soaked in water after bletilla striata slag mixing after extracting Bletilla glucomannan in garlic slag and step (5) after garlic juice, filtrate is taken after filtering;It will twice Resulting filtrate merges to get auburn Pu'er cooked tea leaching liquor.Second extraction is carried out to the waste residue carried out after once extracting, Remaining effective component in waste residue can be extracted, it is more effective and economical.
Further, in step (6), the liquid ratio of the Pu'er cooked tea Ye Yushui is 3-5g:100mL.
Preferably, it is impregnated using 80 DEG C of hot water, helps to improve immersion efficiency.
Further, in step (6), the total amount of three kinds of residues and the liquid ratio of water are 5-7g:50mL.
Further, in step (6), 40-60 DEG C of warm water of the immersion in the second step.
(7) preparation of wild pepper seed hair sun-screening agent
(a) wild pepper seed kind hull melanin is added to while stirring in wild pepper seed albumen peptide solution, is stirred until homogeneous, obtained mixed Close liquid A;(b) Pu'er cooked tea leaching liquor is added after mixing Bletilla glucomannan and the extracting solution of wild pepper seed kernel, is heated to 80 DEG C, keeps 10min is stirred evenly, and obtains mixed liquid B;(d) mixed liquid B is added in mixed liquor A while stirring while hot, is stirred until homogeneous, Under the conditions of ultraviolet irradiation, it is cooled to room temperature, obtains mixed liquor C;(e) under the conditions of ultraviolet irradiation, by VC and/or VE mixing fine powders It is added in mixed liquor C, stirs evenly while stirring, add the garlic juice of deodorization, be stirred until homogeneous, and pH is adjusted to 6.0- 6.5, finally using magnetic force/concussion stirring, the time is wild pepper seed hair sun-screening agent of the 30min to get deep rattan color.
Again, the present invention discloses a kind of wild pepper seed hair sunscreen spray: by wild pepper seed hair sun-screening agent prepared by the present invention It is filling in spray bottle to get.
The application method of the wild pepper seed hair sunscreen spray are as follows: gently shaken up using preceding, need when use to be slightly away from Hair is uniformly sprayed at drying hair middle section until the hair tip, is then softly massaged with hand and make hair in order.The wild pepper seed hair is anti- Shine it is spraying mainly for may or hair that through a long time is exposed under sunlight is sprayed, can play in this way it is sun-proof and The effect of auxiliary hair dyeing, if being accidentally sprayed onto clothes, on hand etc., by usual laundry clothes, wash one's hands in the way of can remove, It is convenient and efficient, if necessary to clear up the sunscreen spray on hair, can be realized by way of conventional hair washing, it will not After using not easy-clear due to extended stationary periods on hair, in fact, this sunscreen spray of the invention is natural component group At use is safe and healthy.
Finally, the invention discloses the wild pepper seed hair sun-screening agents in application sun-proof, in auxiliary hair dyeing product.
It should be understood that specific effect of raw material selected by wild pepper seed hair sun-screening agent of the present invention is as follows:
(1) wild pepper seed, wild pepper seed are rich in vegetable fat, study and identify 12 kinds of fatty acid, and normalized with peak area Method measures each component relative amount, and component is mainly palmitinic acid (20.14), oleic acid (29.72), linoleic acid (29.65) and α- Linolenic acid (17.11), it is necessary to which Fatty Acids Linoleic acid and alpha-linolenic acid account for 46.76%;Protein matter content is high in wild pepper seed (41.17%), contain 17 kinds of amino acid, Glutamic Acid, arginine, leucine content is compared with horn of plenty;Chinese prickly ash seed volatile oil has More than 30 kinds, what wherein content was most is 4- terpinol, 1, 8-Cineole, menthol, piperitenone, the chemistry such as clove tree oxide Ingredient.
1. wild pepper seed kind hull melanin, the melanin belong to phenolic substances, heat-resisting good at 0~80 DEG C.Wild pepper seed is black Pigment is a kind of with compared with the active natural pigment of high anti-oxidation, and antioxidant activity in vitro is in pigment extract mass concentration It is positively correlated, when research finds that mass concentration is 1.0mg/mL, the total reducing power of wild pepper seed melanin and total antioxidant capacity light absorption value Respectively 0.782 (± 0.065) and 0.18 (± 0.003), to lipid peroxidation inhibiting rate up to 65.68% (± 1.13%), with Vc is close;When mass concentration is respectively 0.66mg/mL and 0.76mg/mL, wild pepper seed melanin is to DPPH and OH clearance rate Up to 50%, but the above index is below VC;Wild pepper seed melanin is to O when mass concentration is 0.1mg/mL- 2Clearance rate reaches 65.43%, it is much higher than VC.Research finds that wild pepper seed kind hull melanin is oxidized with the extension of light application time, but its color change It is unobvious.
2. wild pepper seed kernel extracting solution, mainly contains wild pepper seed seed kernel oil, main component is palmitoleic acid, oleic acid and Asia oil Acid and a- linolenic acid, these four components account for 95% or more;Ingredient alpha-linolenic acid is synthesis eicosapentaenoic acid (EPA) He Ershi bis- The precursor substance of carbon acid (DHA) has the function of beauty and skin care, promotes hair growth, improves hair quality;In linoleic acid system With certain inoxidizability;Also contain active material general flavone, polyphenol.Wild pepper seed kernel extracting solution has preferable total reduction Power, research find the IC of DPPH and ABTS free radical scavenging activity50Respectively 0.066mg/mL, 0.43mg/mL.To large intestine bar Bacterium, staphylococcus aureus and bacillus subtilis have bacteriostasis.
3. wild pepper seed albumen peptide solution, wild pepper seed antibacterial peptide is to Escherichia coli, salmonella, bacillus subtilis and golden yellow Color staphylococcus all has inhibiting effect, and research finds that the bacteriostatic activity of antibacterial peptide enhances with the raising of concentration;Antibacterial peptide exists PH value >=6 all have good dissolubility (nitrogen soluble index NSI=80%) in 30~50 DEG C;The emulsifying capacity of antibacterial peptide with The increase of peptide concentration and reduce, stability increases with the increase of concentration;The hydrophilic lipophilic balance (HLB value) of antibacterial peptide Greater than 16.7, hydrophily is stronger.Antibacterial peptide has good foam stability (>=82%) in 10min, pH value >=6;Antibacterial Peptide has good heat, acid, alkali, metal ion and organic solvent stability.
(2) garlic juice, garlic juice include allicin and sulfide, have bactericidal effect, are good natural bacteriostatic agents, can have The multiple functions such as effect control dandruff generation, antipruritic, hair-growing and hair care, hair care.Garlic juice also contain there are many amino acid, vitamin, The nutritional ingredients such as minerals, microelement and volatile oil and oxidation-resistant active ingredient have nourishing effect to scalp cells, improve hair Hair washes shield sun-proof result.The trace elements of selenium being rich in garlic juice, selenium play antioxygen in the form of glutathione peroxidase Change effect is played the role of protecting cell membrane, moreover it is possible to reinforce the antioxidation of vE.Civil have that control scalp using garlic juice white Tinea, bald to old age, young alopecia and post disease alopecia disease also have certain curative effect.
(3) Bletilla glucomannan, using the dry bletilla striata powder obtained of natural plants bletilla striata stem tuber, the Bletilla glucomannan directly boiled has spy Different viscosity property, can be used as assistant for emulsifying agent has good using effect.The main chemical compositions of the bletilla striata are bibenzyl, dihydro phenanthrene Class joins luxuriant and rich with fragrance class and its derivative;Also contain a small amount of volatile oil, lymphatic temperament, bletilla mannan and starch, glucose etc..It is white Splendid achnatherum glue has the function of sore, functions of detumescence, relieving inflammation, myogenic, convergence, protection skin, delay skin aging etc., to treating and prevent skin Pernio and chap, promote blood circulation, improve skin-nourishing situation etc. have obvious curative effects.In civil plant dyeing formulation its It is commonly used for fixation of having hair dyed.
(4) Pu'er cooked tea, due to the effect of just solarization processed and pile fermentation microorganism, fatty acid in tealeaves, carrotene oxidation Degradation increases certain aldehyde materials and linalool oxide;The effect of various enzymes, decomposes portion of cellulose;Polyphenols contains Amount decline, soluble sugar reduce (as microbial energy).As the related effect of pile fermentation, Amino Acids in Tea is by microbial action For nitrogen source utilization, while reducing, some pairs of beneficial amino acid of human body obviously increase partial amino-acid again, such as lysine, The amino acid of methionine, phenylalanine, leucine, isoleucine, valine etc., such as sulfur-bearing can be by disulfide bond in hair fibre It is cross-linked into reticular structure in dimension, plays an important role to the mechanical stability and chemoresistance of hair fiber.In addition civil Also it is commonly used for fixation of having hair dyed in plant dyeing formulation.
(5) VC is a kind of water-soluble strong antioxidant, can protect other antioxidants, such as vitamin E, unsaturation Fatty acid prevents injury of the free radical to human body.
(6) VE is a kind of natural phenolic antioxidant, has the characteristics that antioxidant effect is good, safe and non-toxic.Studies have shown that with Ultraviolet radiation and by 100 DEG C of heat treatment 3h, is not added the iodine number change rate △ I/I of the Fructus Zanthoxyli oil of VE0Than adding VE difference big 3.72% and 1.92%;The Fructus Zanthoxyli oil iodine number change rate △ I/I of VE is not added in air oxidation 3h0Value is bigger by 4.72% than adding VE.Cause This adds a small amount of VE in Fructus Zanthoxyli oil, Fructus Zanthoxyli oil can be effectively prevent to be oxidized, and improves the anti-oxidant efficiency of Fructus Zanthoxyli oil.
Compared with prior art, the beneficial effect that the present invention obtains is:
(1) Chinese prickly ash generallys use its shell and uses as condiment, and wild pepper seed is taken as waste to abandon all the time, this hair It is bright farthest to utilize wild pepper seed, wild pepper seed kind hull melanin is extracted using wild pepper seed kind skin, it is anti-oxidant as natural sun-prevention Ingredient and hair hair dye ingredient;Using wild pepper seed kernel extracting solution as the natural nourishing hair care ingredient of product, wild pepper seed albumen Peptide solution is as natural antibacterial ingredient and emulsifier.The trace elements of selenium being rich in garlic juice, selenium is with glutathione peroxidase Form play antioxidation, the antioxidation of vitamin E can be reinforced.Vitamin E has very strong antioxidation, can subtract The generation of few oxygen radical, improves the anti-oxidant efficiency of Fructus Zanthoxyli oil.Vitamin C and vitamin E use in conjunction have and eliminate carefully The synergistic effect such as lipofuscin, freckle removing and whitening, delay skin aging in born of the same parents, it is significant in efficacy to treatment pigmented spots.
(2) hair sun-screening agent of the present invention be natural component composition, wherein wild pepper seed kind hull melanin can not only have hair dyed but also It can be used as natural sun-screening agents, can reduce ultraviolet light irradiation to the damage of hair and prevent damaged hair from further damaging;Chinese prickly ash Antibacterial peptide all has suppression to Escherichia coli, salmonella, bacillus subtilis and staphylococcus aureus in seed albumen peptide solution Production is used;Garlic juice includes allicin and sulfide, has significant inhibition to make the growth of staphylococcus aureus and Escherichia coli With.Chinese prickly ash is usually used in treatment head moss civil, has good therapeutic effect to treatment psoriasis;Garlic juice is usually used in having treatment head civil The effect of skin tinea alba, the two combine and have preferable effect to each tinea class (such as: favus of the scalp, ringworm of the body, tinea of feet and hands) germ.
(3) Bletilla glucomannan has treatment and prevents skin pernio and chap, promote blood circulation, improving the function such as skin-nourishing situation Effect, is used for the significant effect of scalp care and hair nursing etc.;Wild pepper seed kind hull melanin is water-insoluble materials, In order to reinforce its emulsification degree, it usually needs HLB (hydrophilic lipophilic balance) high emulsifier.Resist in wild pepper seed albumen peptide solution The HLB of bacterium peptide is greater than 16.7, can improve the emulsification degree of wild pepper seed kind hull melanin well;Bletilla glucomannan is natural hydrophilic height Molecule can effectively emulsify wild pepper seed seed kernel oil, assign the present invention apparent consistency and heavy feeling well.
(4) garlic juice includes allicin and sulfide, with certain penetrating odor, and contains abundant tea in Pu'er cooked tea The substances such as polyphenol can cover the penetrating odor of garlic juice to a certain extent, while have the works such as antibacterial, hair dyeing fixation again With.In addition all exist between tea polyphenols and vitamin C, vitamin E and a degree of cooperate with antioxidation.
(5) invention formula is natural component, to hair and scalp skin without any pessimal stimulation, after being especially suitable for hair dyeing Crowd use, mainly for may or through a long time be exposed to the hair under sunlight use, hair dyeing, sun-proof effect can be strengthened Fruit, it is especially obvious to colour fixation after hair dyeing, the flexible gloss of hair can be made.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As background technique is introduced, currently, being with antitan agent mostly although there are many sunscreen product in the market It is main, it is seldom specifically for the sunscreen product of hair.And hair is different from the structure of skin, substance having sun-screening function application method is different, Ask the effect reached different, antitan agent product is not appropriate for being used directly for hair.Therefore, the present invention proposes a kind of wild pepper seed Hair sun-screening agent and preparation method thereof, the present invention is described further With reference to embodiment.
In the following example, wild pepper seed is isolated to the shell of the wild pepper seed of the wild pepper seed kind Renhe black of white, it is spare.
Embodiment 1
1, a kind of preparation method of wild pepper seed hair sun-screening agent, includes the following steps:
(1) preparation of wild pepper seed kind hull melanin
S1, by the shell of black wild pepper seed, coarse crushing is removed with dehydrated alcohol extraction and is deoiled, dries shell after separation, fine crushing, 180 meshes are crossed, the wild pepper seed shell powder of brown is obtained;
S2, wild pepper seed shell powder is placed in NaOH solution and extracts melanin, pH is then adjusted to 2.5-3 progress acid and is sunk, Obtain the unformed powder of dark-brown, as wild pepper seed pigment crude product;
S3, solution is made in wild pepper seed pigment crude product, is mixed with the enzyme solution containing alkali protease and carries out the de- egg of enzymatic isolation method It is white;PH is adjusted to 2.5-3 and carries out the heavy wild pepper seed kind hull melanin to get black of acid.
In step S1, extraction is to extract 1h at 80 DEG C under the constant temperature.
In step S1, the liquid ratio of the wild pepper seed shell and dehydrated alcohol is 1g:5mL.
In step S2, the concentration of the NaOH solution is 1.1moL/L.
In step S2, the liquid ratio of the wild pepper seed shell powder and NaOH solution are as follows: 1g:24.6mL.
In step S2, the reaction condition for extracting melanin are as follows: extract 2h at 70 DEG C, extract 2 times altogether, extracting solution closes And it uses;Preferably, pH 3 carry out acid are adjusted to sink.
In step S3, the concentration of alkali protease (vigor 10000U/g) solution is 10g/L, and using preceding at 4 DEG C Preservation.
In step S3, the wild pepper seed pigment crude product solution concentration is 1mg/mL;The investment of the alkaline protease solution Amount is the 6% of wild pepper seed pigment crude product solution volume;
In step S3, the Deproteinated reaction condition of enzymatic isolation method is to digest 1h at 50 DEG C, pH=9;Finally pH is adjusted It is heavy that acid is carried out to 3.
(2) preparation of wild pepper seed kernel extracting solution
By the wild pepper seed kernel of white, coarse crushing is extracted at a constant temperature with dehydrated alcohol, is separated, the white after must deoiling Wild pepper seed kind Renhe leaching liquor;Ethyl alcohol is distilled off to get flaxen wild pepper seed kernel extracting solution in leaching liquor.
In step (2), extraction is to extract 2h at 80 DEG C under the constant temperature.
In step (2), the liquid ratio of the wild pepper seed kind Renhe dehydrated alcohol of the white are as follows: 1g:10mL.
(3) preparation of wild pepper seed albumen peptide solution
Alkali extraction-acid precipitation is used to the wild pepper seed kernel of the white after deoiling first, the wild pepper seed egg of white is prepared It is white;Then wild pepper seed albumen is preheated after mixing with deionized water, is adjusted to the pH of mixed liquor after reaching predetermined temperature 2.5, the extraction that pepsin carries out wild pepper seed protein peptides is added, carries out destroy the enzyme treatment after extraction, is finally centrifuged, it will Supernatant pH is adjusted to meta-alkalescence to get transparent more sticky wild pepper seed albumen peptide solution.
In step (3), the concentration of substrate of the wild pepper seed albumen in deionized water is 4.9%.
In step (3), the pH of mixed liquor is adjusted to 2.5 after being 32 DEG C by the predetermined temperature.
In step (3), the mass ratio of the pepsin (Rate activity 1:3000) and wild pepper seed protein solution is 0.9: 100, the extraction time is 3h.
In step (3), the destroy the enzyme treatment, which refers to, keeps the temperature 15min in 90 DEG C of water bath with thermostatic control, is cooled to room temperature.
In step (3), the centrifugation, which refers to, is centrifuged 10min under the revolving speed of 8000r/min.
(4) preparation of the garlic juice of deodorization
By blanching 5s after garlic peeling, expect that water quality ratio is that 1:1 mashes garlic juice;Then garlic juice and edible oil is abundant Mixing, is placed in be stored under greenhouse (30 DEG C) and soaks 48h;Volatile matter with penetrating odor in edible oil extract garlic juice, it is quiet Centrifugation is postponed, the intermediate garlic juice in absinthe-green clear liquid to get deodorization is extracted.
In step (4), selection is fresh, not damaged, nothing goes rotten, do not germinate and full and glossiness intact garlic is as former Material.
In step (4), the edible oil is soybean oil.
In step (4), the volume ratio of the garlic juice and edible oil is 100:5.
(5) preparation of Bletilla glucomannan
Bletilla striata powder is impregnated with deionized water, is then filtered, by filtrate concentration gelled to get the gelatinous bletilla striata Glue.
In step (5), the additional amount of the deionized water is 15 times of bletilla striata silty amount.
In step (5), the soaking time is 1h, and soaking temperature is 95 DEG C.
In step (5), 1/4 times of original volume is concentrated the filtrate to get gelatinous Bletilla glucomannan.
(6) preparation of Pu'er cooked tea leaching liquor
It is filtered after Pu'er cooked tea stem tea is impregnated with 80 DEG C of water, takes filtrate;Pu'er cooked tea residue, step are mentioned in (4) It is soaked in water after bletilla striata slag mixing after extracting Bletilla glucomannan in garlic slag and step (5) after taking garlic juice, filtrate is taken after filtering;It will Resulting filtrate merges to get auburn Pu'er cooked tea leaching liquor twice.The waste residue carried out after once extracting is carried out secondary It extracts, remaining effective component in waste residue can be extracted, it is more effective and economical.
In step (6), the liquid ratio of the Pu'er cooked tea Ye Yushui is 3g:100mL.
It is impregnated using 80 DEG C of hot water, helps to improve immersion efficiency.
In step (6), the residue (bletilla striata after garlic slag, extraction Bletilla glucomannan after Pu'er cooked tea residue, extraction garlic juice Residue) and water liquid ratio are as follows: 5g:50mL.
The warm water impregnated with 40 DEG C in step (6), in the second step.
(7) preparation of wild pepper seed hair sun-screening agent
(a) wild pepper seed kind hull melanin is added to while stirring in wild pepper seed albumen peptide solution, is stirred until homogeneous, obtained mixed Close liquid A;(b) Pu'er cooked tea leaching liquor is added after mixing Bletilla glucomannan and the extracting solution of wild pepper seed kernel, is heated to 80 DEG C, keeps 10min is stirred evenly, and obtains mixed liquid B;(d) mixed liquid B is added in mixed liquor A while stirring while hot, is stirred until homogeneous, Under the conditions of ultraviolet irradiation, it is cooled to room temperature, obtains mixed liquor C;(e) under the conditions of ultraviolet irradiation, by VC and VE (vitamin C and E) mixing fine powders are added to while stirring in mixed liquor C, are stirred evenly, and are added the garlic juice of deodorization, are stirred until homogeneous, and will PH is adjusted to 6.5, and finally using magnetic force/concussion stirring, the time is wild pepper seed hair sun-screening agent of the 30min to get deep rattan color.
2, a kind of wild pepper seed hair sun-screening agent prepared according to the method for the present embodiment, the sun-screening agent are pressed by following raw material Made of weight fraction ratio: vitamin C and/or vitamin E add up to 1 part, 3 parts of wild pepper seed kind hull melanin, wild pepper seed protein peptides 28 parts of solution, 60 parts of wild pepper seed kernel extracting solution, deodorization 130 parts of 106 parts of garlic juice, Bletilla glucomannan, Pu'er cooked tea leaching liquor 450 Part.The mass ratio of the vitamin C and vitamin E is 5:8, and the pH of the wild pepper seed hair sun-screening agent is between 6.0-6.5.
3, a kind of wild pepper seed hair sunscreen spray: under the conditions of ultraviolet irradiation, wild pepper seed prepared by the present embodiment method Hair sun-screening agent it is filling in volume 30mL vacuum spraying Aluminum Bottle to get.
Embodiment 2
1, a kind of preparation method of wild pepper seed hair sun-screening agent, includes the following steps:
(1) preparation of wild pepper seed kind hull melanin
S1, by the shell of black wild pepper seed, coarse crushing is removed with dehydrated alcohol extraction and is deoiled, dries shell after separation, fine crushing, 190 meshes are crossed, the wild pepper seed shell powder of brown is obtained;
In step S1, extraction is to extract 1h at 80 DEG C under the constant temperature.
In step S1, the liquid ratio of the wild pepper seed shell and dehydrated alcohol are as follows: 1g:5mL.
S2, wild pepper seed shell powder is placed in NaOH solution and extracts melanin, pH is then adjusted to 2.5-3 progress acid and is sunk, Obtain the unformed powder of dark-brown, as wild pepper seed pigment crude product;
S3, solution is made in wild pepper seed pigment crude product, is mixed with the enzyme solution containing alkali protease and carries out the de- egg of enzymatic isolation method It is white;PH is adjusted to 2.5-3 and carries out the heavy wild pepper seed kind hull melanin to get black of acid.
In step S2, the concentration of the NaOH solution is 1.2moL/L.
In step S2, the liquid ratio of the wild pepper seed shell powder and NaOH solution are as follows: 1g:24.6mL.
In step S2, the reaction condition for extracting melanin are as follows: extract 2h at 70 DEG C, extract 2 times altogether, extracting solution closes And it uses;Preferably, pH 2.5 carry out acid are adjusted to sink.
In step S3, the concentration of alkali protease (vigor 10000U/g) solution is 10g/L, and using preceding at 4 DEG C Preservation.
In step S3, the wild pepper seed pigment crude product solution concentration is 1mg/mL;The investment of the alkaline protease solution Amount is the 6% of wild pepper seed pigment crude product solution volume;
In step S3, the Deproteinated reaction condition of enzymatic isolation method is to digest 1.5h at 50 DEG C, pH=9;Finally by pH tune Section carries out acid to 2.5 and sinks.
(2) preparation of wild pepper seed kernel extracting solution
By the wild pepper seed kernel of white, coarse crushing is extracted at a constant temperature with dehydrated alcohol, is separated, the white after must deoiling Wild pepper seed kind Renhe leaching liquor;Ethyl alcohol is distilled off to get flaxen wild pepper seed kernel extracting solution in leaching liquor.
In step (2), extraction is to extract 2h at 80 DEG C under the constant temperature.
In step (2), the liquid ratio of the wild pepper seed kind Renhe dehydrated alcohol of the white is 1g:10mL.
(3) preparation of wild pepper seed albumen peptide solution
Alkali extraction-acid precipitation is used to the wild pepper seed kernel of the white after deoiling first, the wild pepper seed egg of white is prepared It is white;Then wild pepper seed albumen is preheated after mixing with deionized water, reaches and the pH of mixed liquor is adjusted to 3 after predetermined temperature, The extraction that pepsin carries out wild pepper seed protein peptides is added, carries out destroy the enzyme treatment after extraction, is finally centrifuged, by supernatant Liquid pH is adjusted to meta-alkalescence to get transparent more sticky wild pepper seed albumen peptide solution.
In step (3), the concentration of substrate of the wild pepper seed albumen in deionized water is 4.9%.
In step (3), the pH of mixed liquor is adjusted to 3 after being 32 DEG C by the predetermined temperature.
In step (3), the mass ratio of the pepsin (Rate activity 1:3500) and wild pepper seed protein solution is 0.9: 100, the extraction time is 3h.
In step (3), the destroy the enzyme treatment, which refers to, keeps the temperature 15min in 90 DEG C of water bath with thermostatic control, is cooled to room temperature.
In step (3), the centrifugation, which refers to, is centrifuged 10min under the revolving speed of 8000r/min.
(4) preparation of the garlic juice of deodorization
By blanching 8s after garlic peeling, expect that water quality ratio is that 1:1 mashes garlic juice;Then garlic juice and edible oil is abundant Mixing, is placed in be stored under greenhouse (27 DEG C) and soaks 48h;Volatile matter with penetrating odor in edible oil extract garlic juice, it is quiet Centrifugation is postponed, the intermediate garlic juice in absinthe-green clear liquid to get deodorization is extracted.
In step (4), selection is fresh, not damaged, nothing goes rotten, do not germinate and full and glossiness intact garlic is as former Material.
In step (4), the edible oil is rapeseed oil.
In step (4), the volume ratio of the garlic juice and edible oil are as follows: 100:1~15.
(5) preparation of Bletilla glucomannan
Bletilla striata powder is impregnated with deionized water, is then filtered, by filtrate concentration gelled to get the gelatinous bletilla striata Glue.
In step (5), the additional amount of the deionized water is 18 times of bletilla striata silty amount.
In step (5), the soaking time is 1.5h, and soaking temperature is 93 DEG C.
In step (5), 1/4 times of original volume is concentrated the filtrate to get gelatinous Bletilla glucomannan.
(6) preparation of Pu'er cooked tea leaching liquor
It is filtered after Pu'er cooked tea stem tea is impregnated with 80 DEG C of water, takes filtrate;Pu'er cooked tea residue, step are mentioned in (4) It is soaked in water after bletilla striata slag mixing after extracting Bletilla glucomannan in garlic slag and step (5) after taking garlic juice, filtrate is taken after filtering;It will Resulting filtrate merges to get auburn Pu'er cooked tea leaching liquor twice.The waste residue carried out after once extracting is carried out secondary It extracts, remaining effective component in waste residue can be extracted, it is more effective and economical.
In step (6), the liquid ratio of the Pu'er cooked tea Ye Yushui is 4g:100mL.
In step (6), the residue (bletilla striata after garlic slag, extraction Bletilla glucomannan after Pu'er cooked tea residue, extraction garlic juice Residue) and water liquid ratio are as follows: 6g:50mL.
The warm water impregnated with 50 DEG C in step (6), in the second step.
(7) preparation of wild pepper seed hair sun-screening agent
(a) wild pepper seed kind hull melanin is added to while stirring in wild pepper seed albumen peptide solution, is stirred until homogeneous, obtained mixed Close liquid A;(b) Pu'er cooked tea leaching liquor is added after mixing Bletilla glucomannan and the extracting solution of wild pepper seed kernel, is heated to 80 DEG C, keeps 10min is stirred evenly, and obtains mixed liquid B;(d) mixed liquid B is added in mixed liquor A while stirring while hot, is stirred until homogeneous, Under the conditions of ultraviolet irradiation, it is cooled to room temperature, obtains mixed liquor C;(e) under the conditions of ultraviolet irradiation, by VC (vitamin C) fine powder side Stirring side is added in mixed liquor C, is stirred evenly, is added the garlic juice of deodorization, be stirred until homogeneous, and pH is adjusted to 6.3, most Afterwards using magnetic force/concussion stirring, the time is wild pepper seed hair sun-screening agent of the 30min to get deep rattan color.
2, a kind of wild pepper seed hair sun-screening agent prepared according to the present embodiment method, the sun-screening agent are pressed by following raw material Made of weight fraction ratio: 1.2 parts of vitamin C, 4 parts of wild pepper seed kind hull melanin, 31 parts of wild pepper seed albumen peptide solution, Chinese prickly ash 67 parts of seed kernel extracting solution, deodorization 475 parts of 145 parts of 112 parts of garlic juice, Bletilla glucomannan, Pu'er cooked tea leaching liquor.The wild pepper seed Between the pH control 6.0-6.5 of hair sun-screening agent.
3, a kind of wild pepper seed hair sunscreen spray: under the conditions of ultraviolet irradiation, wild pepper seed prepared by the present embodiment method Hair sun-screening agent it is filling in volume 30mL vacuum spraying Aluminum Bottle to get.
Embodiment 3
A kind of preparation method of wild pepper seed hair sun-screening agent, includes the following steps:
(1) preparation of wild pepper seed kind hull melanin
S1, by the shell of black wild pepper seed, coarse crushing is removed with dehydrated alcohol extraction and is deoiled, dries shell after separation, fine crushing, 200 meshes are crossed, the wild pepper seed shell powder of brown is obtained;
In step S1, extraction is to extract 1h at 80 DEG C under the constant temperature;
In step S1, the liquid ratio of the wild pepper seed shell and dehydrated alcohol are as follows: 1g:5mL.
S2, wild pepper seed shell powder is placed in NaOH solution and extracts melanin, pH is then adjusted to 2.5-3 progress acid and is sunk, Obtain the unformed powder of dark-brown, as wild pepper seed pigment crude product;
S3, solution is made in wild pepper seed pigment crude product, is mixed with the enzyme solution containing alkali protease and carries out the de- egg of enzymatic isolation method It is white;PH is adjusted to 2.5-3 and carries out the heavy wild pepper seed kind hull melanin to get black of acid.
In step S2, the concentration of the NaOH solution is 1.3moL/L.
In step S2, the liquid ratio of the wild pepper seed shell powder and NaOH solution are as follows: 1g:24.6mL.
In step S2, the reaction condition for extracting melanin are as follows: extract 2h at 70 DEG C, extract 2 times altogether, extracting solution closes And it uses;Preferably, pH 2.5 carry out acid are adjusted to sink.
In step S3, the concentration of alkali protease (vigor 10000U/g) solution is 10g/L, and using preceding at 4 DEG C Preservation.
In step S3, the wild pepper seed pigment crude product solution concentration is 1mg/mL;The investment of the alkaline protease solution Amount is the 6% of wild pepper seed pigment crude product solution volume;
In step S3, the Deproteinated reaction condition of enzymatic isolation method is to digest 2h at 50 DEG C, pH=9;Finally pH is adjusted It is heavy that acid is carried out to 2.5.
(2) preparation of wild pepper seed kernel extracting solution
By the wild pepper seed kernel of white, coarse crushing is extracted at a constant temperature with dehydrated alcohol, is separated, the white after must deoiling Wild pepper seed kind Renhe leaching liquor;Ethyl alcohol is distilled off to get flaxen wild pepper seed kernel extracting solution in leaching liquor.
In step (2), extraction is to extract 2h at 80 DEG C under the constant temperature.
In step (2), the liquid ratio of the wild pepper seed kind Renhe dehydrated alcohol of the white are as follows: 1g:10mL.
(3) preparation of wild pepper seed albumen peptide solution
Alkali extraction-acid precipitation is used to the wild pepper seed kernel of the white after deoiling first, the wild pepper seed egg of white is prepared It is white;Then wild pepper seed albumen is preheated after mixing with deionized water, is adjusted to the pH of mixed liquor after reaching predetermined temperature 2.5, the extraction that pepsin carries out wild pepper seed protein peptides is added, carries out destroy the enzyme treatment after extraction, is finally centrifuged, it will Supernatant pH is adjusted to meta-alkalescence to get transparent more sticky wild pepper seed albumen peptide solution.
In step (3), the concentration of substrate of the wild pepper seed albumen in deionized water is 4.9%.
In step (3), the pH of mixed liquor is adjusted to 2.5 after being 32 DEG C by the predetermined temperature.
In step (3), the mass ratio of the pepsin (Rate activity 1:3000) and wild pepper seed protein solution is 0.9: 100, the extraction time is 3h.
In step (3), the destroy the enzyme treatment, which refers to, keeps the temperature 15min in 90 DEG C of water bath with thermostatic control, is cooled to room temperature.
In step (3), the centrifugation, which refers to, is centrifuged 10min under the revolving speed of 8000r/min.
(4) preparation of the garlic juice of deodorization
By blanching 10s after garlic peeling, expect that water quality ratio is that 1:1 mashes garlic juice;Then garlic juice and edible oil are filled Divide mixing, is placed in be stored under greenhouse (25 DEG C) and soaks 48h;Volatile matter with penetrating odor in edible oil extract garlic juice, It is centrifuged after standing, extracts the intermediate garlic juice in absinthe-green clear liquid to get deodorization.
In step (4), selection is fresh, not damaged, nothing goes rotten, do not germinate and full and glossiness intact garlic is as former Material.
In step (4), the edible oil is peanut oil.
In step (4), the volume ratio of the garlic juice and edible oil is 100:15.
(5) preparation of Bletilla glucomannan
Bletilla striata powder is impregnated with deionized water, is then filtered, by filtrate concentration gelled to get the gelatinous bletilla striata Glue.
In step (5), the additional amount of the deionized water is 20 times of bletilla striata silty amount.
In step (5), the soaking time is 2h, and soaking temperature is 90 DEG C.
In step (5), 1/5 times of original volume is concentrated the filtrate to get gelatinous Bletilla glucomannan.
(6) preparation of Pu'er cooked tea leaching liquor
It is filtered after Pu'er cooked tea stem tea is impregnated with 80 DEG C of water, takes filtrate;Pu'er cooked tea residue, step are mentioned in (4) It is soaked in water after bletilla striata slag mixing after extracting Bletilla glucomannan in garlic slag and step (5) after taking garlic juice, filtrate is taken after filtering;It will Resulting filtrate merges to get auburn Pu'er cooked tea leaching liquor twice.The waste residue carried out after once extracting is carried out secondary It extracts, remaining effective component in waste residue can be extracted, it is more effective and economical.
In step (6), the liquid ratio of the Pu'er cooked tea Ye Yushui is 5g:100mL.
In step (6), the residue (bletilla striata after garlic slag, extraction Bletilla glucomannan after Pu'er cooked tea residue, extraction garlic juice Residue) and water liquid ratio be 7g:50mL.
The warm water impregnated with 60 DEG C in step (6), in the second step.
(7) preparation of wild pepper seed hair sun-screening agent
(a) wild pepper seed kind hull melanin is added to while stirring in wild pepper seed albumen peptide solution, is stirred until homogeneous, mixed Liquid A;(b) Pu'er cooked tea leaching liquor is added after mixing Bletilla glucomannan and the extracting solution of wild pepper seed kernel, is heated to 80 DEG C, keeps 10min is stirred evenly, and obtains mixed liquid B;(d) mixed liquid B is added in mixed liquor A while stirring while hot, is stirred until homogeneous, Under the conditions of ultraviolet irradiation, it is cooled to room temperature, mixed liquor C;(e) under the conditions of ultraviolet irradiation, VE (vitamin E) fine powder side is stirred It mixes side to be added in mixed liquor C, stir evenly, add the garlic juice of deodorization, be stirred until homogeneous, and pH is adjusted to 6.0, finally Using magnetic force/concussion stirring, the time is wild pepper seed hair sun-screening agent of the 30min to get deep rattan color.
2, a kind of wild pepper seed hair sun-screening agent prepared according to the present embodiment method, the sun-screening agent are pressed by following raw material Made of weight fraction ratio: vitamin E is 0.8 part total, 2 parts of wild pepper seed kind hull melanin, 25 parts of wild pepper seed albumen peptide solution, spends 53 parts of green pepper seed kernel extracting solution, deodorization 425 parts of 115 parts of 100 parts of garlic juice, Bletilla glucomannan, Pu'er cooked tea leaching liquor.The Chinese prickly ash Between the pH control 6.0-6.5 of seed hair sun-screening agent.
3, a kind of wild pepper seed hair sunscreen spray: under the conditions of ultraviolet irradiation, wild pepper seed prepared by the present embodiment method Hair sun-screening agent it is filling in volume 30mL vacuum spraying Aluminum Bottle to get.
The effect performance test of wild pepper seed hair sunscreen products embodiment 1
Before carrying out effect performance test, wild pepper seed is had hair dyed, and sunscreen products first test by the acute dermal toxicity through mouse It is tested with the skin phototoxicity of rabbit, without finding any undesirable reaction.It can be considered that wild pepper seed hair dyeing is sun-proof Agent product uses safe.
Experiment volunteer: choosing the more crowd of white hair and needs to contaminate 30 people of sepia hair, and men and women is unlimited, is randomly assigned reality Test each 15 people of group, contrast groups.According to requirement of experiment using the hair of same brand pure natural hair dye dye sepia, and it is every as required It is primary (have one's hair wash and take care of hair using the shampoo of same brand) every hair washing in 3 days.
Experimental method: volunteer is tested as requested daily outdoors at least 2 hours under sunlight.Experimental group is from after having hair dyed the Start within 3 days to spray wild pepper seed hair dyeing sunscreen products of the invention, control group then sprays aliquots of deionized water.It is right in experimentation It requires to take pictures to the first pass water after hair washing after 3 times having one's hair wash.
Experimental result counts after 30 days:
Hair color is still 12 people of sepia person, 1 people of brown person, 2 people of light brown person in experimental group;It has hair dyed in control group face Color is 4 people of sepia person, and 5 people of brown person, 6 people of light brown person (wherein has 1 people more white hair occur, need at hair dyeing again Reason);
Meanwhile have in experimental group 8 people's readme hair hair qualitys be improved significantly, hair more moisten, without 1 discomfort it is anti- It answers;And the reflection is had no in control group, and have after 2 people (man, each people of Ms) readme hair dyeing and have that hair is dry and astringent, itching of the scalp Problem.
In addition the color of the first pass water after having one's hair wash three times before observation, color of the control group than the water after experimental group hair washing Deep, the color of the water after especially having hair dyed for the first time, after second of hair washing has the difference of conspicuousness.
Effect performance the experimental results showed that, wild pepper seed hair dyeing sunscreen products of the invention have it is sun-proof, auxiliary hair dyeing, grow Support and repair the multi-efficiencies such as hair.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for those skilled in the art For member, various changes and changes are possible in this application.Within the spirit and principles of this application, it is made it is any modification, Equivalent replacement, improvement etc., should be included within the scope of protection of this application.

Claims (10)

1. a kind of wild pepper seed hair sun-screening agent, it is characterised in that: the sun-screening agent is made by ratio of weight and the number of copies of following raw material : vitamin C and/or vitamin E add up to (0.8-1.2) part, wild pepper seed kind hull melanin (2-4) part, wild pepper seed protein peptides molten Liquid (25-31) part, wild pepper seed kernel extracting solution (53-67) part, garlic juice (100-112) part of deodorization, Bletilla glucomannan (115-145) Part, Pu'er cooked tea leaching liquor (425-475) part.
2. wild pepper seed hair sun-screening agent as described in claim 1, it is characterised in that: preferably the sun-screening agent is by following raw material Made of by ratio of weight and the number of copies: vitamin C and/or vitamin E add up to 1 part, 3 parts of wild pepper seed kind hull melanin, wild pepper seed albumen 28 parts of peptide solution, 60 parts of wild pepper seed kernel extracting solution, deodorization 130 parts of 106 parts of garlic juice, Bletilla glucomannan, Pu'er cooked tea leaching liquor 450 parts.
3. wild pepper seed hair sun-screening agent as claimed in claim 1 or 2, it is characterised in that: the vitamin C and vitamin E Mass ratio is 5:8;Between the pH control 6.0-6.5 of the wild pepper seed hair sun-screening agent.
4. the preparation method of the described in any item wild pepper seed hair sun-screening agents of claim 1-3, it is characterised in that: including walking as follows It is rapid:
(1) wild pepper seed the preparation of wild pepper seed kind hull melanin: is isolated to the Chinese prickly ash of the wild pepper seed kind Renhe black of white first The shell of seed;
S1, by the shell of black wild pepper seed, coarse crushing is removed with dehydrated alcohol extraction and is deoiled, dries shell after separation, fine crushing, sieving, Obtain the wild pepper seed shell powder of brown;
S2, wild pepper seed shell powder is placed in NaOH solution and extracts melanin, pH is then adjusted to 2.5-3 progress acid and is sunk, depth is obtained The unformed powder of brown, as wild pepper seed pigment crude product;
S3, solution is made in wild pepper seed pigment crude product, is mixed with the enzyme solution containing alkali protease and carries out the de- albumen of enzymatic isolation method;It will PH is adjusted to 3 or less the heavy wild pepper seed kind hull melanins to get black of progress acid;
(2) preparation of wild pepper seed kernel extracting solution: by the wild pepper seed kernel of white, coarse crushing is soaked at a constant temperature with dehydrated alcohol It mentions, separates, the wild pepper seed kind Renhe leaching liquor of the white after must deoiling;Ethyl alcohol is distilled off to get flaxen in leaching liquor Wild pepper seed kernel extracting solution;
(3) alkali extraction-acid precipitation, system the preparation of wild pepper seed albumen peptide solution: are used to the wild pepper seed kernel of the white after deoiling first The standby wild pepper seed albumen for obtaining white;Then wild pepper seed albumen is preheated after mixing with deionized water, after reaching predetermined temperature The pH of mixed liquor is adjusted to 2.5-3, the extraction that pepsin carries out wild pepper seed protein peptides is added, carries out enzyme deactivation after extraction Processing, is finally centrifuged, supernatant pH is adjusted to meta-alkalescence to get transparent more sticky wild pepper seed albumen peptide solution;
(4) preparation of the garlic juice of deodorization: by blanching (5~10) s after garlic peeling, expect that water quality ratio is that 1:1 mashes garlic Juice;Then garlic juice and edible oil are sufficiently mixed, are placed in be stored at (25-30) DEG C and soak 48h;Have in edible oil extract garlic juice The volatile matter of irritant smell is centrifuged after standing, extracts the intermediate garlic juice in absinthe-green clear liquid to get deodorization;
(5) preparation of Bletilla glucomannan: bletilla striata powder being impregnated with deionized water, is then filtered, by filtrate concentration gelled to get solidifying Gelatinous Bletilla glucomannan;
(6) it the preparation of Pu'er cooked tea leaching liquor: is filtered after Pu'er cooked tea stem tea is soaked in water, takes filtrate;By Pu'er cooked tea Water logging is used after bletilla striata slag mixing after extracting Bletilla glucomannan in garlic slag and step (5) after extracting garlic juice in residue, step (4) Bubble, takes filtrate after filtering;Resulting filtrate it will merge twice to get auburn Pu'er cooked tea leaching liquor;
(7) wild pepper seed kind hull melanin (a) preparation of wild pepper seed hair sun-screening agent: is added to wild pepper seed protein peptides while stirring It in solution, is stirred until homogeneous, obtains mixed liquor A;(b) Pu'er cooked tea is added after mixing Bletilla glucomannan and the extracting solution of wild pepper seed kernel Leaching liquor, heating, stirs evenly, obtains mixed liquid B;(d) mixed liquid B is added in mixed liquor A while stirring while hot, stirring is extremely Uniformly, cooling, obtain mixed liquor C;(e) VC and/or VE mixing fine powders are added to while stirring in mixed liquor C, are stirred evenly, then The garlic juice of deodorization is added, is stirred until homogeneous, and pH is adjusted to 6.0-6.5, finally using magnetic force/concussion stirring, the time is 30min to get deep rattan color wild pepper seed hair sun-screening agent.
5. the preparation method of wild pepper seed hair sun-screening agent as claimed in claim 4, it is characterised in that: in step S1, the perseverance The lower extraction of temperature is to extract 1h at 80 DEG C;
Alternatively, in step S1, the liquid ratio of the wild pepper seed shell and dehydrated alcohol are as follows: 1g:5mL;
Alternatively, the sieving was (180~200) mesh in step S1;
Alternatively, the concentration of the NaOH solution is (1.1-1.3) moL/L, preferably 1.2moL/L in step S2;
Alternatively, the liquid ratio of the smashed black wild pepper seed and NaOH solution is 1g:24.6mL in step S2;
Alternatively, in step S2, the reaction condition for extracting melanin are as follows: extract 2h at 70 DEG C, extract 2 times altogether, extracting solution Merge and uses;Preferably, pH 2.5 carry out acid are adjusted to sink;
Alternatively, the concentration of the alkaline protease solution is 10g/L, vigor 10000U/g, and using preceding 4 in step S3 DEG C preservation;
Alternatively, the wild pepper seed pigment crude product solution concentration is 1mg/mL in step S3;The investment of the alkaline protease solution Amount is the 6% of wild pepper seed pigment crude product solution volume;
Alternatively, the Deproteinated reaction condition of enzymatic isolation method is to digest 1-2h at 50 DEG C, pH=9 in step S3;Finally by pH It is heavy to be adjusted to 2.5 carry out acid.
6. the preparation method of wild pepper seed hair sun-screening agent as claimed in claim 4, it is characterised in that: in step (2), the perseverance The lower extraction of temperature is to extract 2h at 80 DEG C;
Alternatively, in step (2), the liquid ratio of the wild pepper seed kind Renhe dehydrated alcohol of the white are as follows: 1g:10mL;
Alternatively, the concentration of substrate of the wild pepper seed albumen in deionized water is 4.9% in step (3);
Alternatively, in step (3), the pH of mixed liquor is adjusted to 2.0 after being 32 DEG C by the predetermined temperature;
Alternatively, the mass ratio of the pepsin and wild pepper seed protein solution is 0.9:100, the extraction time in step (3) For 3h, the Rate activity of the pepsin is 1:(3000-3500);
Alternatively, the destroy the enzyme treatment, which refers to, keeps the temperature 15min in 90 DEG C of water bath with thermostatic control in step (3), it is cooled to room temperature;
Alternatively, the centrifugation, which refers to, is centrifuged 10min under the revolving speed of 8000r/min in step (3).
7. the preparation method of wild pepper seed hair sun-screening agent as claimed in claim 4, it is characterised in that: in step (4), choose new It is fresh, not damaged, without going rotten, do not germinate and full and glossiness intact garlic is as raw material;
Alternatively, the edible oil includes soybean oil, peanut oil, rapeseed oil in step (4);
Alternatively, in step (4), the volume ratio of the garlic juice and edible oil are as follows: 100:(1-15);
Alternatively, the additional amount of the deionized water is (15-20) times of bletilla striata silty amount in step (5);
Alternatively, the soaking time is (1-2) h in step (5), soaking temperature is (90-95) DEG C;
Alternatively, concentrating the filtrate to (1/4-1/5) of original volume again to get gel Bletilla glucomannan in step (5).
8. the preparation method of wild pepper seed hair sun-screening agent as claimed in claim 4, it is characterised in that: described general in step (6) The liquid ratio of the ripe tealeaves of Pu'er tea and water is (3-5) g:100mL;
Preferably, it in step (6), is impregnated using 80 DEG C of hot water, helps to improve immersion efficiency;
Alternatively, the residue is (white after the garlic slag, extraction Bletilla glucomannan after Pu'er cooked tea residue, extraction garlic juice in step (6) Splendid achnatherum slag) and water liquid ratio are as follows: (5~7) g:50mL;
Alternatively, in step (6), the warm water of the immersion use (40-60) DEG C in the second step;
Alternatively, described last using magnetic force/concussion stirring, the time is 30min in step (7).
9. a kind of wild pepper seed hair sunscreen spray: by the described in any item wild pepper seed hair sun-screening agents of claim 1-3 and/or power Benefit require the wild pepper seed hair sun-screening agent of 4-8 described in any item methods preparation to be placed in vacuum spraying Aluminum Bottle to get.
10. wild pepper seed hair sun-screening agent as described in any one of claims 1-3 and/or claim 4-9 are described in any item The wild pepper seed hair sun-screening agent of method preparation is in application sun-proof, in auxiliary hair dyeing product.
CN201811435670.0A 2018-11-28 2018-11-28 Pricklyash seed hair sun-screening agent and preparation method thereof Active CN109431934B (en)

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