CN109431934B - Pricklyash seed hair sun-screening agent and preparation method thereof - Google Patents

Pricklyash seed hair sun-screening agent and preparation method thereof Download PDF

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CN109431934B
CN109431934B CN201811435670.0A CN201811435670A CN109431934B CN 109431934 B CN109431934 B CN 109431934B CN 201811435670 A CN201811435670 A CN 201811435670A CN 109431934 B CN109431934 B CN 109431934B
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pepper seed
preparing
solution
hair
sunscreen
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CN109431934A (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

Abstract

The invention relates to a pepper seed hair sun-screening agent, and belongs to the technical field of cosmetics. The sun-screening agent is prepared from the following raw materials in parts by weight: 0.8-1.2 parts of total vitamin C and/or vitamin E, 2-4 parts of pepper seed coat melanin, 25-31 parts of pepper seed protein peptide solution, 53-67 parts of pepper seed kernel extract, 100-containing garlic juice (112) parts of deodorized garlic juice, 115-containing bletilla gum (145) parts of cooked Pu' er tea extract (425-containing tea 475). The invention extracts the effective components from the pepper seeds respectively, has strong oxidation resistance, sun protection and auxiliary hair dyeing functions; it also has effects in nourishing hair and killing bacteria. The invention designs the deodorizing garlic juice with the functions of sterilization, moistening and sun protection; Pu-Er ripe tea leaching liquor with effects of absorbing and isolating ultraviolet rays, fixing color and caring hair; the bletilla striata gum with color fixing effect and nourishing effect enables the hair sun-screening agent to have multiple effects of well sun-screening, auxiliary hair dyeing, hair nourishing, hair restoration and the like.

Description

Pricklyash seed hair sun-screening agent and preparation method thereof
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a pricklyash seed hair sunscreen agent developed aiming at the problem that hair after hair dyeing is easy to decompose and fade, particularly under illumination, and a preparation method thereof.
Background
The hair dyeing product is necessary for many people in daily life, but chemical reactions in the hair dyeing process can change the surface and internal structures of the hair, so that the hair is warped, the hair is detackified, and when the hair surface is rough, light scattering is caused, so that the hair loses luster; the loss of protein and the reduction of crystallinity of the hair lead to the reduction of water retention capacity, the reduction of tensile strength, the reduction of elasticity and toughness and other physical property changes; meanwhile, damaged hair loses the protective structure of the outer layer, and hollowing also occurs inside the damaged hair, so that the pigment is difficult to effectively retain in the hair. If the hair just dyed is irradiated by ultraviolet rays for a long time, the hair dyed is not only more fragile, but also is not favorable for maintaining hair color.
The research finds that: proteins in hair are susceptible to photochemical degradation, and ultraviolet rays also accelerate oxidation of amino acids and carbon between polypeptide chains, because ultraviolet rays can generate a large amount of active oxygen radicals by photo-degrading amino acids and reacting with photosensitive substances, thereby causing alteration of hair fibers. Free radicals, mediated by water or atmospheric moisture, undergo a series of reactions that cause significant damage to hair proteins, especially keratin, and lead to degradation of melanin, causing the hair to change color. In addition, the visible light in sunlight causes more damage to the lipid layer than ultraviolet light, and the lipid layer of hair is easily damaged by lipid peroxide generated by illumination, so that the integrity, the hydrophobicity and the hardness of hair shafts of the hair are obviously and negatively influenced.
At present, although a lot of sunscreen products are available on the market, most of the sunscreen products are mainly used for skin. The physical sun-proof skin product is based on the principle of light reflection, is more greasy and heavy, and can only play a role after being coated to a certain thickness, for example, when the physical sun-proof skin product is used for sun-proof hair, the hair looks greasy and thin, the hairstyle is difficult to maintain, the appearance is influenced, and discomfort is brought to a user; under the action of bacteria, ultraviolet rays and the like, grease is deteriorated to block hair follicles, and a scalp health system is damaged, so that symptoms such as dandruff, scalp itching, alopecia and the like are caused; the chemical sunscreen skin product absorbs ultraviolet rays in sunlight by utilizing chemical reaction, and has more chemical sunscreen additives, so that the chemical sunscreen skin product has great harm to hair and scalp after long-term use; and melanin in the hair reacts with part of the chemical sunscreen additive, resulting in fading of the dyed color.
In view of the above, there is no hair sunscreen product that solves the problem of fading of hair color, especially after hair is dyed, and therefore, there is a need to develop a new hair sunscreen product that is at least partially free from the above-mentioned problems of the prior art.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a pricklyash seed hair sunscreen agent and a preparation method thereof. The invention extracts the effective components from the prickly ash seeds respectively, has strong oxidation resistance, sun protection and auxiliary hair dyeing functions, and also has the functions of nourishing hair, sterilizing and the like. In addition, the invention also designs the deodorizing garlic juice with the functions of sterilization, moistening and sun protection; Pu-Er ripe tea leaching liquor with effects of absorbing and isolating ultraviolet rays, fixing color and caring hair; and bletilla striata gum and other components with color fixing effect and nourishing effect, so that the hair sunscreen agent has good sunscreen and auxiliary hair dyeing effects, and has multiple effects of nourishing and repairing hair and the like.
The first purpose of the invention is to provide a pepper seed hair sunscreen.
The second purpose of the invention is to provide a preparation method of the pepper seed hair sunscreen agent.
The third purpose of the invention is to provide a pricklyash seed hair dyeing sunscreen spray.
The fourth purpose of the invention is to provide the application of the pepper seed hair sunscreen agent.
In order to achieve the above purpose, the invention specifically discloses the following technical scheme:
firstly, the invention discloses a pepper seed hair sun-screening agent which is prepared from the following raw materials in parts by weight: 0.8-1.2 parts of vitamin C and/or vitamin E in total, 2-4 parts of pepper seed coat melanin, 25-31 parts of pepper seed protein peptide solution, 53-67 parts of pepper seed kernel extracting solution, 100 parts of deodorized garlic juice, 145 parts of bletilla striata gelatin and 475 parts of Pu-Er ripe tea extracting solution 425 and 475 parts.
Preferably, the sun-screening agent is prepared from the following raw materials in parts by weight: 1 part of vitamin C and/or vitamin E in total, 3 parts of pepper seed coat melanin, 28 parts of pepper seed protein peptide solution, 60 parts of pepper seed kernel extracting solution, 106 parts of deodorized garlic juice, 130 parts of bletilla striata gum and 450 parts of Pu-erh ripe tea extracting solution.
Furthermore, in the pepper seed hair sunscreen agent, the mass ratio of the vitamin C to the vitamin E is 5: 8.
Furthermore, in the pepper seed hair sunscreen agent, the pH value of the pepper seed hair sunscreen agent is controlled to be 6.0-6.5, so that the characteristics of pepper seed protein peptide can be well maintained, the main component of the pepper seed enzymatic hydrolysis protein peptide is antibacterial peptide, the pH value of the combined components is weak and acidic, and epidermal scales can be folded when the hair meets weak acid, so that the hair has good texture, luster and good hair dyeing effect, and scalp skin and hair can be well moistened.
The pepper seed hair sun-screening agent has the effects of sun-screening and auxiliary hair dyeing, and can moisten and moisturize hair, repair damaged hair and the like, because: (1) the prickly ash seed melanin extracted from the prickly ash seed coat has strong oxidation resistance and black dyeing function, and can play the main roles of sun protection and auxiliary hair dyeing; the pepper seed kernel extracting solution contains a large amount of alpha-linolenic acid and other nutrient substances and has the function of nourishing hair; the pepper seed protein peptide solution has the functions of sterilization and the like; (2) the deodorized garlic juice has the functions of sterilization, moistening and sun protection; the Pu-Er ripe tea leaching liquor has the functions of absorbing and isolating ultraviolet rays, fixing color and protecting hair; (3) the bletilla striata gum has color fixing effect and nourishing effect; (4) VE can effectively prevent the prickly ash seed oil from being oxidized and improve the oxidation resistance efficiency of the prickly ash seed oil; vitamin C has effects of resisting oxidation, protecting unsaturated fatty acid in natural oil, increasing density of hair cuticle cells, and relieving hair dryness.
Secondly, the invention discloses a preparation method of a pepper seed hair sun-screening agent, which comprises the following steps:
separating white semen Zanthoxyli kernel and black semen Zanthoxyli shell from semen Zanthoxyli, and keeping.
(1) Preparing the seed coat melanin of prickly ash seeds:
s1, coarsely crushing the black pepper seed shells, leaching with absolute ethyl alcohol to remove oil, drying the shells after separation, finely crushing and sieving to obtain brown pepper seed shell powder;
s2, placing the pepper seed shell powder in NaOH solution to extract melanin, adjusting the pH value to 2.5-3, and performing acid precipitation to obtain dark brown amorphous powder, namely a crude product of pepper seed pigment;
s3, preparing the crude product of the prickly ash seed pigment into solution, mixing the solution with enzyme solution containing alkaline protease to carry out deproteinization by an enzymolysis method; adjusting pH to 2.5-3, and performing acid precipitation to obtain black semen Zanthoxyli seed coat melanin.
In step S1, the leaching at constant temperature is leaching at 80 ℃ for 1 h.
In the step S1, the material-liquid ratio of the pepper seed shells and the absolute ethyl alcohol is as follows: 1g:5 mL.
In the step S1, the sieving is performed by sieving with a 180-200 mesh sieve.
In step S2, the concentration of the NaOH solution is 1.1-1.3moL/L, preferably 1.2 moL/L.
In step S2, the ratio of the pepper seed shell powder to the NaOH solution is: 1g, 24.6 mL.
In step S2, the reaction conditions for extracting melanin are as follows: extracting at 70 deg.C for 2 hr for 2 times, and mixing extractive solutions; preferably, the pH is adjusted to 2.5 for acid precipitation.
In step S3, the alkaline protease (activity 10000U/g) solution has a concentration of 10g/L and is preserved at 4 ℃ before use.
In step S3, the concentration of the crude pricklyash seed pigment solution is 1 mg/mL; the input amount of the alkaline protease solution is 6 percent of the volume of the crude pepper seed pigment solution;
in step S3, the deproteinization reaction by the enzymolysis method is carried out at 50 ℃ and pH 9 for 0.5-2 h; finally, the pH value is adjusted to 2.5 for acid precipitation.
(2) Preparation of pricklyash seed extract
Coarsely pulverizing white semen Zanthoxyli, extracting with anhydrous ethanol at constant temperature, and separating to obtain deoiled white semen Zanthoxyli and extractive solution; distilling the leaching solution to remove ethanol to obtain light yellow semen Zanthoxyli extract.
Further, in the step (2), the leaching at constant temperature is leaching at 80 ℃ for 2 h.
Further, in the step (2), the ratio of the white pepper seed kernel to the absolute ethyl alcohol is 1g:10 mL.
(3) Preparation of pricklyash seed protein peptide solution
Firstly, preparing white pepper seed protein from deoiled white pepper seed kernels by an alkali-soluble acid precipitation method; and then mixing the pepper seed protein with deionized water, preheating, adjusting the pH of the mixed solution to 2.5-3 after reaching a preset temperature, adding pepsin to extract the pepper seed protein peptide, performing enzyme deactivation treatment after extraction, finally centrifuging, and adjusting the pH of the supernatant to be alkaline, thereby obtaining the transparent and viscous pepper seed protein peptide solution.
Further, in the step (3), the substrate concentration of the pepper seed protein in the deionized water is 4.9%.
Further, in the step (3), after the predetermined temperature is 32 ℃, the pH of the mixed solution is adjusted to 2.5.
Further, in the step (3), the mass ratio of the pepsin (specific activity 1:3000-1:3500) to the pepper seed protein solution is 0.9:100, and the extraction time is 3 hours.
Further, in the step (3), the enzyme deactivation treatment refers to heat preservation in a constant-temperature water bath at 90 ℃ for 15min, and cooling to room temperature.
Further, in the step (3), the centrifugation refers to centrifugation at 8000r/min for 10 min.
(4) Preparation method of deodorized Bulbus Allii solution
Peeling garlic, blanching for 5-10s, and mashing into pasty garlic juice with a material-water mass ratio of 1: 1; then mixing the garlic juice and the edible oil thoroughly, and soaking in a greenhouse (25-30 deg.C) for 48 h; extracting volatile matter with pungent odor from Bulbus Allii solution with edible oil, standing, centrifuging, and extracting middle light green clear liquid to obtain deodorized Bulbus Allii solution.
Preferably, in the step (4), fresh, undamaged, moldy and rotten, unmalted, full and glossy intact garlic is selected as the raw material.
Further, in the step (4), the edible oil comprises soybean oil, peanut oil, rapeseed oil and the like.
Further, in the step (4), the volume ratio of the garlic juice to the edible oil is as follows: 100:1-15.
(5) Preparation of bletilla striata gum
Soaking rhizoma bletilla powder in deionized water, filtering, and concentrating the filtrate to obtain gel-like bletilla gum.
Further, in the step (5), the addition amount of the deionized water is 15-20 times of the mass of the bletilla striata powder.
Further, in the step (5), the soaking time is 1-2h, and the soaking temperature is 90-95 ℃.
Further, in the step (5), the filtrate is concentrated to 1/4-1/5 times of the original volume, and the gelatinous bletilla hyacinthine gum is obtained.
(6) Preparation of Pu-Er ripe tea extract
Soaking Pu-Er ripe tea dry tea in water, filtering, and collecting filtrate; mixing the residue of cooked Pu-Er tea, the garlic residue obtained by extracting garlic juice in step (4) and the bletilla striata residue obtained by extracting bletilla striata gum in step (5), soaking in water, filtering, and collecting filtrate; mixing the filtrates to obtain dark brown Pu-Er ripe tea leaching solution. The waste residue after primary extraction is subjected to secondary extraction, so that the residual effective components in the waste residue can be extracted, and the method is more effective and economical.
Further, in the step (6), the ratio of the Pu-Er ripe tea leaves to the water is 3-5g:100 mL.
Preferably, the soaking is carried out by using hot water at 80 ℃, which helps to improve the soaking efficiency.
Further, in the step (6), the ratio of the total amount of the three residues to the feed liquid of water is 5-7g:50 mL.
Further, in the step (6), warm water with the temperature of 40-60 ℃ is used for soaking in the second step.
(7) Preparation of pricklyash seed hair sunscreen agent
(a) Adding the seed coat melanin of the prickly ash seed into the protein peptide solution of the prickly ash seed while stirring, and stirring uniformly to obtain a mixed solution A; (b) mixing extractive solutions of bletilla hyacinthine gum and semen Zanthoxyli kernel, adding cooked Pu-erh tea extract, heating to 80 deg.C, maintaining for 10min, and stirring to obtain mixed solution B; (d) adding the mixed solution B into the mixed solution A while stirring while the mixed solution B is hot, stirring uniformly, and cooling to room temperature under the condition of ultraviolet irradiation to obtain a mixed solution C; (e) under the condition of ultraviolet irradiation, adding VC and/or VE mixed fine powder into the mixed solution C while stirring, uniformly stirring, adding deodorized garlic juice, uniformly stirring, adjusting the pH to 6.0-6.5, and finally stirring by magnetic force/oscillation for 30min to obtain the dark rattan pepper seed hair sunscreen agent.
The invention further discloses a pepper seed hair sunscreen spray which comprises the following components in parts by weight: filling the pepper seed hair sun-screening agent prepared by the invention into a spray bottle to obtain the pepper seed hair sun-screening agent.
The application method of the prickly ash seed hair sunscreen spray comprises the following steps: the product is applied by shaking gently before application, spraying onto the middle part of dry hair to the tip of hair, and massaging with hand. The pepper seed hair sunscreen spray is mainly sprayed on hairs which are likely to be exposed to the sun or are exposed to the sun for a long time, so that the effects of sunscreen and auxiliary hair dyeing can be achieved, if the pepper seed hair sunscreen spray is sprayed on clothes, hands and the like carelessly, the hair sunscreen spray can be cleaned in a common clothes and hand washing mode, the cleaning is convenient and quick, if the sunscreen spray on the hairs is required to be cleaned, the cleaning can be achieved through a conventional hair washing mode, the hair sunscreen spray cannot stay on the hairs for a long time due to the fact that the sunscreen spray is not easy to clean after being used, and the use is safe and healthy.
Finally, the invention discloses application of the pepper seed hair sunscreen agent in sunscreen and auxiliary hair dyeing products.
It should be noted that: the pepper seed hair sunscreen agent has the following specific effects of the selected raw materials:
(1) pepper seeds which are rich in vegetable oil are researched and identified as 12 kinds of fatty acids, and the relative content of each component is determined by using a peak area normalization method, wherein the components mainly comprise palmitic acid (20.14), oleic acid (29.72), linoleic acid (29.65) and alpha-linolenic acid (17.11), and the essential fatty acid linoleic acid and the alpha-linolenic acid account for 46.76%; the kernel protein content of the pepper seeds is high (41.17%), and the pepper seeds contain 17 amino acids, wherein the contents of glutamic acid, arginine and leucine are rich; the pricklyash seed volatile oil contains more than 30 kinds, wherein the maximum content is 4-terpineol, 1, 8-cineole, menthol, menthenone, clove oxide and other chemical components.
The pepper seed coat melanin belongs to phenolic substances and has good heat resistance at 0-80 ℃. The pepper seed melanin is a natural pigment with high antioxidant activity, the in vitro antioxidant capacity of the natural pigment is in positive correlation with the mass concentration of a pigment extracting solution, researches show that when the mass concentration is 1.0mg/mL, the total reducing power and the total antioxidant capacity light absorption value of the pepper seed melanin are respectively 0.782 (+ -0.065) and 0.18 (+ -0.003), the lipid peroxidation inhibition rate reaches 65.68% (+ -1.13%), and the natural pigment is close to Vc; when the mass concentration is 0.66mg/mL and 0.76mg/mL respectively, the clearance rate of the pepper seed melanin to DPPH & OH reaches 50%, but the indexes are all lower than VC; pepper seed melanin pair O at mass concentration of 0.1mg/mL-2The clearance rate reaches 65.43 percent and is far higher than VC. The research finds that the melanin of the pepper seed coat is oxidized along with the prolonging of the illumination time, but the color change is not obvious.
② the pepper seed kernel extract mainly contains pepper seed kernel oil, the main components are palmitoleic acid, oleic acid, linoleic acid and alpha-linolenic acid, the four components account for more than 95%; the component alpha-linolenic acid is a precursor substance for synthesizing eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), and has the effects of beautifying and protecting skin, promoting hair growth and improving hair quality; the linoleic acid system has certain oxidation resistance; also contains active substances total flavone and polyphenol. The extract of the pepper seed kernel has better total reducing power, and researches show that IC of DPPH and ABTS free radical clearance rate50The concentration was 0.066mg/mL and 0.43mg/mL, respectively. Has antibacterial effect on Escherichia coli, Staphylococcus aureus and Bacillus subtilis.
③ the pepper seed protein peptide solution, the pepper seed antibacterial peptide has the inhibiting effect on colibacillus, salmonella, bacillus subtilis and staphylococcus aureus, and researches show that the antibacterial activity of the antibacterial peptide is enhanced along with the increase of the concentration; the antibacterial peptide has good solubility (nitrogen solubility index NSI is 80%) at the pH value of more than or equal to 6 and at the temperature of 30-50 ℃; the emulsifying capacity of the antibacterial peptide is reduced along with the increase of the concentration of the peptide, and the stability is increased along with the increase of the concentration; the antibacterial peptide has a hydrophilic-lipophilic balance (HLB) value of more than 16.7 and strong hydrophilicity. The antibacterial peptide has good foam stability (more than or equal to 82%) when the pH value is more than or equal to 6 within 10 min; the antibacterial peptide has good heat, acid, alkali, metal ion and organic solvent stability.
(2) The garlic liquid contains allicin and sulfide, has a bactericidal effect, is a good natural bacteriostatic agent, and can effectively control dandruff generation, relieve itching, grow hair, protect hair, nourish hair and the like. The garlic liquid also contains various amino acids, vitamins, minerals, trace elements, volatile oil and other nutrient components and antioxidant active components, has nourishing effect on scalp cells, and improves the washing, protecting and sun-screening effects of hair. The garlic solution is rich in trace element selenium which plays an antioxidation role in the form of glutathione peroxidase, plays a role in protecting cell membranes and can also strengthen the antioxidation effect of vE. The garlic liquid is used for treating scalp tinea alba in folk, and has certain curative effect on senile alopecia, juvenile alopecia and alopecia after diseases.
(3) The bletilla striata gum is prepared by drying natural plant bletilla striata tubers to obtain bletilla striata powder, and the directly decocted bletilla striata gum has special viscosity characteristic and can be used as an auxiliary emulsifier to achieve a good using effect. The main chemical components of bletilla striata are bibenzyl, dihydrophenanthrene, diphenanthryl and derivatives thereof; also contains small amount of volatile oil, mucus, rhizoma bletilla mannan, starch, glucose, etc. The bletilla striata glue has the functions of healing sore, detumescence and anti-inflammation, promoting granulation, astringing, protecting skin, delaying skin aging and the like, and has obvious curative effects of treating and preventing chilblain and chap of skin, promoting blood circulation, improving skin nutrition condition and the like. The plant hair dye is often used for dyeing and fixing hair in a folk plant hair dye formula.
(4) The Pu-Er ripe tea, because of the action of primary sun-drying and pile-fermentation microorganisms, the fatty acid and carotene in the tea are oxidized and degraded, so that certain aldehyde substances and linalool oxide are increased; partial cellulose is decomposed by the action of various enzymes; the polyphenol content is reduced, and the soluble sugar is reduced (as a microbial energy source). As a combined effect of pile fermentation, tea amino acids are used as a nitrogen source by microorganisms, and a part of amino acids are reduced while a plurality of amino acids beneficial to human bodies are obviously increased, such as lysine, methionine, phenylalanine, leucine, isoleucine, valine and the like, for example, sulfur-containing amino acids can be crosslinked into a net structure in hair fibers through disulfide bonds, and play an important role in the mechanical stability and the chemical resistance of the hair fibers. In addition, the hair dye is also commonly used for dyeing and fixing the hair in folk plant hair dyeing formulas.
(5) VC is a water-soluble strong antioxidant, can protect other antioxidants such as vitamin E and unsaturated fatty acid, and can prevent free radicals from damaging human bodies.
(6) VE is a natural phenol antioxidant and has the characteristics of good antioxidant effect, safety and no toxicity. Research shows that iodine value change rate delta I/I of pepper seed oil without VE is irradiated by ultraviolet and subjected to heat treatment at 100 ℃ for 3 hours03.72 percent and 1.92 percent respectively larger than the additive VE; oxidizing in air for 3h, and changing rate delta I/I of iodine value of pepper seed oil without VE0The value was 4.72% greater than the addition of VE. Therefore, a small amount of VE is added into the prickly ash seed oil, so that the prickly ash seed oil can be effectively prevented from being oxidized, and the oxidation resistance efficiency of the prickly ash seed oil is improved.
Compared with the prior art, the invention has the beneficial effects that:
(1) the pepper is usually used as a seasoning by adopting the shell thereof, and pepper seeds are always abandoned as wastes, the invention utilizes the pepper seeds to the maximum extent, and the pepper seed coats are used for extracting the melanin of the pepper seed coats as natural sunscreen and antioxidant components and hair dyeing components; the extract of the pricklyash seed kernel is used as the natural nourishing and hair-care component of the product, and the pricklyash seed protein peptide solution is used as the natural antibacterial component and the emulsifier. The garlic liquid is rich in trace element selenium which plays an antioxidation role in the form of glutathione peroxidase and can strengthen the antioxidation role of vitamin E. The vitamin E has strong antioxidation effect, can reduce the generation of oxygen free radicals, and improves the antioxidation efficiency of the pricklyash seed oil. The combined application of vitamin C and vitamin E has the synergistic effects of eliminating lipofuscin in cells, removing freckles, whitening, delaying skin aging and the like, and has obvious curative effect on treating pigmented spots.
(2) The hair sun-screening agent disclosed by the invention is composed of natural components, wherein the pricklyash seed coat melanin can be used for dyeing hair and can also be used as a natural sun-screening agent, so that the damage of ultraviolet irradiation to the hair can be reduced, and the further damage of the damaged hair can be prevented; the antibacterial peptide in the pepper seed protein peptide solution has an inhibiting effect on escherichia coli, salmonella, bacillus subtilis and staphylococcus aureus; the garlic liquid contains allicin and sulfide, and has obvious inhibiting effect on the growth of staphylococcus aureus and escherichia coli. The Chinese prickly ash is commonly used for treating tinea capitis in folk and has better curative effect on treating psoriasis; the garlic liquid is commonly used for folk treatment of scalp tinea alba, and the combination of the garlic liquid and the scalp tinea alba has good effect on various tinea pathogens (such as tinea capitis, tinea corporis, tinea manus and tinea pedis and the like).
(3) The bletilla striata gum has the effects of treating and preventing chilblain and chapping of skin, promoting blood circulation, improving skin nutrition and the like, and has obvious effects when being used for scalp care, hair care and the like; the melanin of the seed coat of prickly ash is a water-insoluble substance, and in order to enhance the emulsification degree thereof, an emulsifier having a high HLB (hydrophilic-lipophilic balance) is generally required. The HLB of the antibacterial peptide in the pepper seed protein peptide solution is more than 16.7, so that the emulsification degree of the melanin of the seed coat of the pepper seed can be well improved; the bletilla hyacinthine gum is a natural hydrophilic polymer, can effectively emulsify the pepper seed kernel oil, and endows the pepper seed kernel oil with good apparent thickness and heavy feeling.
(4) The garlic liquid contains allicin and sulfide and has a certain pungent smell, and the cooked puerh tea contains rich substances such as tea polyphenol and the like, so that the pungent smell of the garlic liquid can be covered to a certain degree, and the garlic liquid also has the effects of antibiosis, hair dyeing and color fixation and the like. In addition, the tea polyphenol has a certain degree of synergistic antioxidation with vitamin C and vitamin E.
(5) The formula of the invention is all natural components, has no any adverse stimulation to hair and scalp skin, is especially suitable for people after hair dyeing, is mainly used for hair which is possibly or has been exposed to the sun for a long time, can strengthen hair dyeing and sun protection effects, has obvious color fixing effect after hair dyeing, and can make the hair flexible and glossy.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As described in the background art, although many sunscreen products are available on the market, most sunscreen products are mainly used for the skin, and few sunscreen products are specially used for the hair. The structure of hair and skin is different, the use method of the sunscreen substance is different, the required effect is different, and the skin sunscreen product is not suitable for being directly used for hair. Therefore, the present invention provides a pepper seed hair sunscreen and a preparation method thereof, and the present invention will be further described with reference to the following embodiments.
In the following examples, the white pepper seeds and black pepper seed shells were separated from the pepper seeds and kept ready for use.
Example 1
1. A preparation method of a pricklyash seed hair sunscreen comprises the following steps:
(1) preparation of zanthoxylum seed coat melanin
S1, coarsely crushing the black pepper seed shells, leaching with absolute ethyl alcohol to remove oil, drying the shells after separation, finely crushing the shells, and sieving the shells with a 180-mesh sieve to obtain brown pepper seed shell powder;
s2, placing the pepper seed shell powder in NaOH solution to extract melanin, adjusting the pH value to 2.5-3, and performing acid precipitation to obtain dark brown amorphous powder, namely a crude product of pepper seed pigment;
s3, preparing the crude product of the prickly ash seed pigment into solution, mixing the solution with enzyme solution containing alkaline protease to carry out deproteinization by an enzymolysis method; adjusting pH to 2.5-3, and performing acid precipitation to obtain black semen Zanthoxyli seed coat melanin.
In step S1, the leaching at constant temperature is leaching at 80 ℃ for 1 h.
In the step S1, the ratio of the pepper seed shells to the absolute ethyl alcohol is 1g to 5 mL.
In step S2, the concentration of the NaOH solution is 1.1 moL/L.
In step S2, the ratio of the pepper seed shell powder to the NaOH solution is: 1g, 24.6 mL.
In step S2, the reaction conditions for extracting melanin are as follows: extracting at 70 deg.C for 2 hr for 2 times, and mixing extractive solutions; preferably, the pH is adjusted to 3 for acid precipitation.
In step S3, the alkaline protease (activity 10000U/g) solution has a concentration of 10g/L and is preserved at 4 ℃ before use.
In step S3, the concentration of the crude pricklyash seed pigment solution is 1 mg/mL; the input amount of the alkaline protease solution is 6 percent of the volume of the crude pepper seed pigment solution;
in step S3, the reaction conditions for deproteinization by the enzymatic hydrolysis method are that enzymolysis is performed for 1h at 50 ℃ and pH 9; finally, the pH value is adjusted to 3 for acid precipitation.
(2) Preparation of pricklyash seed extract
Coarsely pulverizing white semen Zanthoxyli, extracting with anhydrous ethanol at constant temperature, and separating to obtain deoiled white semen Zanthoxyli and extractive solution; distilling the leaching solution to remove ethanol to obtain light yellow semen Zanthoxyli extract.
In the step (2), the leaching at constant temperature is carried out for 2h at 80 ℃.
In the step (2), the material liquid ratio of the white pepper seed kernels to the absolute ethyl alcohol is as follows: 1g, 10 mL.
(3) Preparation of pricklyash seed protein peptide solution
Firstly, preparing white pepper seed protein from deoiled white pepper seed kernels by an alkali-soluble acid precipitation method; and then mixing the pepper seed protein with deionized water, preheating, adjusting the pH of the mixed solution to 2.5 after reaching a preset temperature, adding pepsin to extract the pepper seed protein peptide, performing enzyme deactivation after extraction, finally centrifuging, and adjusting the pH of the supernatant to be alkaline to obtain a transparent and viscous pepper seed protein peptide solution.
In the step (3), the substrate concentration of the pepper seed protein in the deionized water is 4.9%.
In the step (3), after the preset temperature is 32 ℃, the pH value of the mixed solution is adjusted to 2.5.
In the step (3), the mass ratio of the pepsin (specific activity 1:3000) to the pepper seed protein solution is 0.9:100, and the extraction time is 3 hours.
In the step (3), the enzyme deactivation treatment refers to heat preservation in a constant-temperature water bath at 90 ℃ for 15min, and cooling to room temperature.
In the step (3), the centrifugation refers to centrifugation for 10min at the rotating speed of 8000 r/min.
(4) Preparation method of deodorized Bulbus Allii solution
Peeling garlic, blanching for 5s, and mashing into pasty garlic juice with a material-water mass ratio of 1: 1; then mixing the garlic juice and the edible oil thoroughly, and soaking in a greenhouse (30 ℃) for 48 hours; extracting volatile matter with pungent odor from Bulbus Allii solution with edible oil, standing, centrifuging, and extracting middle light green clear liquid to obtain deodorized Bulbus Allii solution.
In the step (4), fresh, undamaged, ungerminated, full and glossy perfect garlic is selected as a raw material.
In the step (4), the edible oil is soybean oil.
In the step (4), the volume ratio of the garlic juice to the edible oil is 100: 5.
(5) Preparation of bletilla striata gum
Soaking rhizoma bletilla powder in deionized water, filtering, and concentrating the filtrate to obtain gel-like bletilla gum.
In the step (5), the addition amount of the deionized water is 15 times of the mass of the bletilla striata powder.
In the step (5), the soaking time is 1h, and the soaking temperature is 95 ℃.
In the step (5), the filtrate is concentrated to 1/4 times of the original volume, and the gelatinous bletilla hyacinthine gum is obtained.
(6) Preparation of Pu-Er ripe tea extract
Soaking Pu-Er ripe tea dried tea in 80 deg.C water, filtering, and collecting filtrate; mixing the residue of cooked Pu-Er tea, the garlic residue obtained by extracting garlic juice in step (4) and the bletilla striata residue obtained by extracting bletilla striata gum in step (5), soaking in water, filtering, and collecting filtrate; mixing the filtrates to obtain dark brown Pu-Er ripe tea leaching solution. The waste residue after primary extraction is subjected to secondary extraction, so that the residual effective components in the waste residue can be extracted, and the method is more effective and economical.
In the step (6), the feed liquid ratio of the Pu-erh ripe tea leaves to the water is 3g:100 mL.
The soaking is carried out by adopting hot water with the temperature of 80 ℃, which is beneficial to improving the soaking efficiency.
In the step (6), the material liquid proportion of the residues (Pu-erh ripe tea residues, garlic residues after garlic juice extraction and bletilla striata residues after bletilla striata gum extraction) and water is as follows: 5g, 50 mL.
In the step (6), warm water of 40 ℃ is used for soaking in the second step.
(7) Preparation of pricklyash seed hair sunscreen agent
(a) Adding the seed coat melanin of the prickly ash seed into the protein peptide solution of the prickly ash seed while stirring, and stirring uniformly to obtain a mixed solution A; (b) mixing extractive solutions of bletilla hyacinthine gum and semen Zanthoxyli kernel, adding cooked Pu-erh tea extract, heating to 80 deg.C, maintaining for 10min, and stirring to obtain mixed solution B; (d) adding the mixed solution B into the mixed solution A while stirring while the mixed solution B is hot, stirring uniformly, and cooling to room temperature under the condition of ultraviolet irradiation to obtain a mixed solution C; (e) under the condition of ultraviolet irradiation, adding mixed fine powder of VC and VE (vitamin C and E) into the mixed solution C while stirring, uniformly stirring, adding deodorized garlic juice, uniformly stirring, adjusting pH to 6.5, and finally stirring by magnetic force/oscillation for 30min to obtain the dark rattan pepper seed hair sunscreen agent.
2. The pepper seed hair sunscreen agent prepared by the method of the embodiment is prepared from the following raw materials in parts by weight: 1 part of vitamin C and/or vitamin E in total, 3 parts of pepper seed coat melanin, 28 parts of pepper seed protein peptide solution, 60 parts of pepper seed kernel extracting solution, 106 parts of deodorized garlic juice, 130 parts of bletilla striata gum and 450 parts of Pu-erh ripe tea extracting solution. The mass ratio of the vitamin C to the vitamin E is 5:8, and the pH value of the pepper seed hair sunscreen agent is 6.0-6.5.
3. A pricklyash seed hair sunscreen spray: filling the pepper seed hair sunscreen agent prepared by the method in the embodiment into a vacuum spraying aluminum bottle with the volume of 30mL under the ultraviolet irradiation condition, and thus obtaining the sunscreen agent.
Example 2
1. A preparation method of a pricklyash seed hair sunscreen comprises the following steps:
(1) preparation of zanthoxylum seed coat melanin
S1, coarsely crushing the black pepper seed shells, leaching with absolute ethyl alcohol to remove oil, drying the shells after separation, finely crushing the shells, and sieving the shells with a 190-mesh sieve to obtain brown pepper seed shell powder;
in step S1, the leaching at constant temperature is leaching at 80 ℃ for 1 h.
In the step S1, the material-liquid ratio of the pepper seed shells and the absolute ethyl alcohol is as follows: 1g:5 mL.
S2, placing the pepper seed shell powder in NaOH solution to extract melanin, adjusting the pH value to 2.5-3, and performing acid precipitation to obtain dark brown amorphous powder, namely a crude product of pepper seed pigment;
s3, preparing the crude product of the prickly ash seed pigment into solution, mixing the solution with enzyme solution containing alkaline protease to carry out deproteinization by an enzymolysis method; adjusting pH to 2.5-3, and performing acid precipitation to obtain black semen Zanthoxyli seed coat melanin.
In step S2, the concentration of the NaOH solution is 1.2 moL/L.
In step S2, the ratio of the pepper seed shell powder to the NaOH solution is: 1g, 24.6 mL.
In step S2, the reaction conditions for extracting melanin are as follows: extracting at 70 deg.C for 2 hr for 2 times, and mixing extractive solutions; preferably, the pH is adjusted to 2.5 for acid precipitation.
In step S3, the alkaline protease (activity 10000U/g) solution has a concentration of 10g/L and is preserved at 4 ℃ before use.
In step S3, the concentration of the crude pricklyash seed pigment solution is 1 mg/mL; the input amount of the alkaline protease solution is 6 percent of the volume of the crude pepper seed pigment solution;
in step S3, the reaction conditions for deproteinization by the enzymatic hydrolysis method are that enzymolysis is performed for 1.5h at 50 ℃ and pH 9; finally, the pH value is adjusted to 2.5 for acid precipitation.
(2) Preparation of pricklyash seed extract
Coarsely pulverizing white semen Zanthoxyli, extracting with anhydrous ethanol at constant temperature, and separating to obtain deoiled white semen Zanthoxyli and extractive solution; distilling the leaching solution to remove ethanol to obtain light yellow semen Zanthoxyli extract.
In the step (2), the leaching at constant temperature is carried out for 2h at 80 ℃.
In the step (2), the ratio of the white pepper seed kernels to the absolute ethyl alcohol is 1g to 10 mL.
(3) Preparation of pricklyash seed protein peptide solution
Firstly, preparing white pepper seed protein from deoiled white pepper seed kernels by an alkali-soluble acid precipitation method; and then mixing the pepper seed protein with deionized water, preheating, adjusting the pH of the mixed solution to 3 after reaching a preset temperature, adding pepsin to extract the pepper seed protein peptide, performing enzyme deactivation after extraction, finally centrifuging, and adjusting the pH of the supernatant to be alkaline to obtain the transparent viscous pepper seed protein peptide solution.
In the step (3), the substrate concentration of the pepper seed protein in the deionized water is 4.9%.
In the step (3), after the preset temperature is 32 ℃, the pH value of the mixed solution is adjusted to 3.
In the step (3), the mass ratio of the pepsin (specific activity 1:3500) to the pepper seed protein solution is 0.9:100, and the extraction time is 3 hours.
In the step (3), the enzyme deactivation treatment refers to heat preservation in a constant-temperature water bath at 90 ℃ for 15min, and cooling to room temperature.
In the step (3), the centrifugation refers to centrifugation for 10min at the rotating speed of 8000 r/min.
(4) Preparation method of deodorized Bulbus Allii solution
Peeling garlic, blanching for 8s, and mashing into pasty garlic juice with a material-water mass ratio of 1: 1; then mixing the garlic juice and the edible oil thoroughly, and soaking in a greenhouse (27 ℃) for 48 hours; extracting volatile matter with pungent odor from Bulbus Allii solution with edible oil, standing, centrifuging, and extracting middle light green clear liquid to obtain deodorized Bulbus Allii solution.
In the step (4), fresh, undamaged, ungerminated, full and glossy perfect garlic is selected as a raw material.
In the step (4), the edible oil is rapeseed oil.
In the step (4), the volume ratio of the garlic juice to the edible oil is as follows: 100: 1-15.
(5) Preparation of bletilla striata gum
Soaking rhizoma bletilla powder in deionized water, filtering, and concentrating the filtrate to obtain gel-like bletilla gum.
In the step (5), the addition amount of the deionized water is 18 times of the mass of the bletilla striata powder.
In the step (5), the soaking time is 1.5h, and the soaking temperature is 93 ℃.
In the step (5), the filtrate is concentrated to 1/4 times of the original volume, and the gelatinous bletilla hyacinthine gum is obtained.
(6) Preparation of Pu-Er ripe tea extract
Soaking Pu-Er ripe tea dried tea in 80 deg.C water, filtering, and collecting filtrate; mixing the residue of cooked Pu-Er tea, the garlic residue obtained by extracting garlic juice in step (4) and the bletilla striata residue obtained by extracting bletilla striata gum in step (5), soaking in water, filtering, and collecting filtrate; mixing the filtrates to obtain dark brown Pu-Er ripe tea leaching solution. The waste residue after primary extraction is subjected to secondary extraction, so that the residual effective components in the waste residue can be extracted, and the method is more effective and economical.
In the step (6), the feed liquid ratio of the Pu-erh ripe tea leaves to the water is 4g:100 mL.
In the step (6), the material liquid proportion of the residues (Pu-erh ripe tea residues, garlic residues after garlic juice extraction and bletilla striata residues after bletilla striata gum extraction) and water is as follows: 6g, 50 mL.
In the step (6), warm water of 50 ℃ is used for soaking in the second step.
(7) Preparation of pricklyash seed hair sunscreen agent
(a) Adding the seed coat melanin of the prickly ash seed into the protein peptide solution of the prickly ash seed while stirring, and stirring uniformly to obtain a mixed solution A; (b) mixing extractive solutions of bletilla hyacinthine gum and semen Zanthoxyli kernel, adding cooked Pu-erh tea extract, heating to 80 deg.C, maintaining for 10min, and stirring to obtain mixed solution B; (d) adding the mixed solution B into the mixed solution A while stirring while the mixed solution B is hot, stirring uniformly, and cooling to room temperature under the condition of ultraviolet irradiation to obtain a mixed solution C; (e) under the condition of ultraviolet irradiation, adding VC (vitamin C) fine powder into the mixed solution C while stirring, uniformly stirring, adding deodorized garlic juice, uniformly stirring, adjusting the pH to 6.3, and finally stirring by magnetic force/oscillation for 30min to obtain the dark rattan pepper seed hair sunscreen agent.
2. The pepper seed hair sunscreen agent prepared according to the method of the embodiment is prepared from the following raw materials in parts by weight: 1.2 parts of vitamin C, 4 parts of pepper seed coat melanin, 31 parts of pepper seed protein peptide solution, 67 parts of pepper seed kernel extracting solution, 112 parts of deodorized garlic juice, 145 parts of bletilla hyacinthine gum and 475 parts of Pu-erh ripe tea leaching liquor. The pH value of the pepper seed hair sunscreen agent is controlled to be 6.0-6.5.
3. A pricklyash seed hair sunscreen spray: filling the pepper seed hair sunscreen agent prepared by the method in the embodiment into a vacuum spraying aluminum bottle with the volume of 30mL under the ultraviolet irradiation condition, and thus obtaining the sunscreen agent.
Example 3
A preparation method of a pricklyash seed hair sunscreen comprises the following steps:
(1) preparation of zanthoxylum seed coat melanin
S1, coarsely crushing the black pepper seed shells, leaching with absolute ethyl alcohol to remove oil, drying the shells after separation, finely crushing the shells, and sieving the shells with a 200-mesh sieve to obtain brown pepper seed shell powder;
in the step S1, leaching at constant temperature is leaching for 1h at 80 ℃;
in the step S1, the material-liquid ratio of the pepper seed shells and the absolute ethyl alcohol is as follows: 1g:5 mL.
S2, placing the pepper seed shell powder in NaOH solution to extract melanin, adjusting the pH value to 2.5-3, and performing acid precipitation to obtain dark brown amorphous powder, namely a crude product of pepper seed pigment;
s3, preparing the crude product of the prickly ash seed pigment into solution, mixing the solution with enzyme solution containing alkaline protease to carry out deproteinization by an enzymolysis method; adjusting pH to 2.5-3, and performing acid precipitation to obtain black semen Zanthoxyli seed coat melanin.
In step S2, the concentration of the NaOH solution is 1.3 moL/L.
In step S2, the ratio of the pepper seed shell powder to the NaOH solution is: 1g, 24.6 mL.
In step S2, the reaction conditions for extracting melanin are as follows: extracting at 70 deg.C for 2 hr for 2 times, and mixing extractive solutions; preferably, the pH is adjusted to 2.5 for acid precipitation.
In step S3, the alkaline protease (activity 10000U/g) solution has a concentration of 10g/L and is preserved at 4 ℃ before use.
In step S3, the concentration of the crude pricklyash seed pigment solution is 1 mg/mL; the input amount of the alkaline protease solution is 6 percent of the volume of the crude pepper seed pigment solution;
in step S3, the reaction conditions for deproteinization by the enzymatic hydrolysis method are that enzymolysis is performed for 2 hours at 50 ℃ and pH 9; finally, the pH value is adjusted to 2.5 for acid precipitation.
(2) Preparation of pricklyash seed extract
Coarsely pulverizing white semen Zanthoxyli, extracting with anhydrous ethanol at constant temperature, and separating to obtain deoiled white semen Zanthoxyli and extractive solution; distilling the leaching solution to remove ethanol to obtain light yellow semen Zanthoxyli extract.
In the step (2), the leaching at constant temperature is carried out for 2h at 80 ℃.
In the step (2), the material liquid ratio of the white pepper seed kernels to the absolute ethyl alcohol is as follows: 1g, 10 mL.
(3) Preparation of pricklyash seed protein peptide solution
Firstly, preparing white pepper seed protein from deoiled white pepper seed kernels by an alkali-soluble acid precipitation method; and then mixing the pepper seed protein with deionized water, preheating, adjusting the pH of the mixed solution to 2.5 after reaching a preset temperature, adding pepsin to extract the pepper seed protein peptide, performing enzyme deactivation after extraction, finally centrifuging, and adjusting the pH of the supernatant to be alkaline to obtain a transparent and viscous pepper seed protein peptide solution.
In the step (3), the substrate concentration of the pepper seed protein in the deionized water is 4.9%.
In the step (3), after the preset temperature is 32 ℃, the pH value of the mixed solution is adjusted to 2.5.
In the step (3), the mass ratio of the pepsin (specific activity 1:3000) to the pepper seed protein solution is 0.9:100, and the extraction time is 3 hours.
In the step (3), the enzyme deactivation treatment refers to heat preservation in a constant-temperature water bath at 90 ℃ for 15min, and cooling to room temperature.
In the step (3), the centrifugation refers to centrifugation for 10min at the rotating speed of 8000 r/min.
(4) Preparation method of deodorized Bulbus Allii solution
Peeling garlic, blanching for 10s, and mashing into pasty garlic juice with a material-water mass ratio of 1: 1; then mixing the garlic juice and the edible oil thoroughly, and soaking in a greenhouse (25 ℃) for 48 hours; extracting volatile matter with pungent odor from Bulbus Allii solution with edible oil, standing, centrifuging, and extracting middle light green clear liquid to obtain deodorized Bulbus Allii solution.
In the step (4), fresh, undamaged, ungerminated, full and glossy perfect garlic is selected as a raw material.
In the step (4), the edible oil is peanut oil.
In the step (4), the volume ratio of the garlic juice to the edible oil is 100: 15.
(5) Preparation of bletilla striata gum
Soaking rhizoma bletilla powder in deionized water, filtering, and concentrating the filtrate to obtain gel-like bletilla gum.
In the step (5), the addition amount of the deionized water is 20 times of the mass of the bletilla striata powder.
In the step (5), the soaking time is 2 hours, and the soaking temperature is 90 ℃.
In the step (5), the filtrate is concentrated to 1/5 times of the original volume, and the gelatinous bletilla hyacinthine gum is obtained.
(6) Preparation of Pu-Er ripe tea extract
Soaking Pu-Er ripe tea dried tea in 80 deg.C water, filtering, and collecting filtrate; mixing the residue of cooked Pu-Er tea, the garlic residue obtained by extracting garlic juice in step (4) and the bletilla striata residue obtained by extracting bletilla striata gum in step (5), soaking in water, filtering, and collecting filtrate; mixing the filtrates to obtain dark brown Pu-Er ripe tea leaching solution. The waste residue after primary extraction is subjected to secondary extraction, so that the residual effective components in the waste residue can be extracted, and the method is more effective and economical.
In the step (6), the feed liquid ratio of the Pu-erh ripe tea leaves to water is 5g:100 mL.
In the step (6), the ratio of the residues (Pu-erh ripe tea residues, garlic residues after garlic juice extraction and bletilla striata residues after bletilla striata gum extraction) to the water feed liquid is 7g to 50 mL.
In the step (6), the soaking in the second step is performed with warm water of 60 ℃.
(7) Preparation of pricklyash seed hair sunscreen agent
(a) Adding the seed coat melanin of the prickly ash seed into the protein peptide solution of the prickly ash seed while stirring, and stirring the mixture until the mixture is uniform to obtain a mixed solution A; (b) mixing extractive solutions of bletilla hyacinthine gum and semen Zanthoxyli kernel, adding cooked Pu-erh tea extract, heating to 80 deg.C, maintaining for 10min, and stirring to obtain mixed solution B; (d) adding the mixed solution B into the mixed solution A while stirring when the mixed solution B is hot, stirring uniformly, and cooling to room temperature under the condition of ultraviolet irradiation to obtain a mixed solution C; (e) under the condition of ultraviolet irradiation, adding VE (vitamin E) fine powder into the mixed solution C while stirring, uniformly stirring, adding deodorized garlic juice, uniformly stirring, adjusting the pH to 6.0, and finally stirring by magnetic force/oscillation for 30min to obtain the dark rattan pepper seed hair sunscreen agent.
2. The pepper seed hair sunscreen agent prepared according to the method of the embodiment is prepared from the following raw materials in parts by weight: 0.8 part of total vitamin E, 2 parts of pepper seed coat melanin, 25 parts of pepper seed protein peptide solution, 53 parts of pepper seed kernel extracting solution, 100 parts of deodorized garlic juice, 115 parts of bletilla hyacinthine gum and 425 parts of Pu-erh ripe tea leaching liquor. The pH value of the pepper seed hair sunscreen agent is controlled to be 6.0-6.5.
3. A pricklyash seed hair sunscreen spray: filling the pepper seed hair sunscreen agent prepared by the method in the embodiment into a vacuum spraying aluminum bottle with the volume of 30mL under the ultraviolet irradiation condition, and thus obtaining the sunscreen agent.
Effect testing of prickly ash seed Hair sunscreen product example 1
Before the performance test, the pricklyash seed hair-dyeing sun-screening agent product is subjected to an acute transdermal toxicity test of mice and a skin phototoxicity test of rabbits, and no adverse reaction is found. Therefore, the pepper seed hair dye sunscreen product is safe to use.
Experimental volunteers: selecting 30 people who have more white hairs and need to be dyed with tan hairs, randomly distributing 15 people to an experimental group and a comparison group. The same brand of pure natural hair dye was used to dye tan hair as required by the experiment and was shampooed once every 3 days as required (shampooing and conditioning using the same brand of shampoo).
The experimental method comprises the following steps: experimental volunteers were exposed to outdoor sunlight for at least 2 hours per day as required. The experimental group was sprayed with the prickly ash seed hair dye sunscreen product of the present invention from day 3 after hair dyeing, and the control group was sprayed with an equal amount of deionized water. The first wash after the first 3 shampooings was photographed during the experiment.
Statistics of experimental results after 30 days:
in the experimental group, 12 people with the hair dyeing color still being dark brown, 1 person with the hair dyeing color and 2 people with the hair dyeing color being light brown; in the control group, 4 persons with hair dyeing color of tan, 5 persons with brown color and 6 persons with light brown color (1 person has more white hair and needs re-dyeing treatment);
meanwhile, the hair quality of 8 people in the experimental group is obviously improved, the hair is relatively moist, and 1 case of discomfort reaction does not exist; the control group did not show the above-mentioned responses, and 2 persons (each man or woman) reported the dry hair and scalp itching after dyeing hair.
In addition, the color of the first water after the first three shampoos was observed, and the control group had a darker color than the water after the experimental group shampoos, especially the color of the water after the first and second shampoos after dyeing had significant differences.
The effect performance experiment result shows that the pricklyash seed hair-dyeing sun-screening agent product has multiple effects of sun screening, auxiliary hair dyeing, hair nourishing, hair restoration and the like.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (36)

1. A pricklyash seed hair sun-screening agent is characterized in that: the sun-screening agent is prepared from the following raw materials in parts by weight: 0.8-1.2 parts of vitamin C and/or vitamin E in total, 2-4 parts of pepper seed coat melanin, 25-31 parts of pepper seed protein peptide solution, 53-67 parts of pepper seed kernel extracting solution, 100 parts of deodorized garlic juice, 145 parts of bletilla striata gelatin and 475 parts of Pu-Er ripe tea extracting solution 425 and 475 parts.
2. The pepper seed hair sunscreen of claim 1 wherein: preferably, the sun-screening agent is prepared from the following raw materials in parts by weight: 1 part of vitamin C and/or vitamin E in total, 3 parts of pepper seed coat melanin, 28 parts of pepper seed protein peptide solution, 60 parts of pepper seed kernel extracting solution, 106 parts of deodorized garlic juice, 130 parts of bletilla striata gum and 450 parts of Pu-erh ripe tea extracting solution.
3. A pepper seed hair sunscreen as claimed in claim 1 or 2, characterized in that: the mass ratio of the vitamin C to the vitamin E is 5: 8; the pH value of the pepper seed hair sunscreen agent is controlled to be 6.0-6.5.
4. A method for preparing a pepper seed hair sunscreen as claimed in any one of the claims 1-3, characterized in that: the method comprises the following steps:
(1) preparing the seed coat melanin of prickly ash seeds: firstly, separating white pepper seed kernels and black pepper seed shells from pepper seeds;
s1, coarsely crushing the black pepper seed shells, leaching with absolute ethyl alcohol to remove oil, drying the shells after separation, finely crushing and sieving to obtain brown pepper seed shell powder;
s2, placing the pepper seed shell powder in NaOH solution to extract melanin, adjusting the pH value to 2.5-3, and performing acid precipitation to obtain dark brown amorphous powder, namely a crude product of pepper seed pigment;
s3, preparing the crude product of the prickly ash seed pigment into solution, mixing the solution with enzyme solution containing alkaline protease to carry out deproteinization by an enzymolysis method; adjusting pH to below 3, and performing acid precipitation to obtain black melanin of pericarpium Zanthoxyli seed coat;
(2) preparing a pepper seed kernel extracting solution: coarsely pulverizing white semen Zanthoxyli, extracting with anhydrous ethanol at constant temperature, and separating to obtain deoiled white semen Zanthoxyli and extractive solution; distilling the leaching solution to remove ethanol to obtain light yellow semen Zanthoxyli extract;
(3) preparing a pepper seed protein peptide solution: firstly, preparing white pepper seed protein from deoiled white pepper seed kernels by an alkali-soluble acid precipitation method; mixing the pepper seed protein with deionized water, preheating, adjusting the pH of the mixed solution to 2.5-3 after reaching a preset temperature, adding pepsin to extract the pepper seed protein peptide, performing enzyme deactivation after extraction, finally centrifuging, and adjusting the pH of a supernatant to be alkaline to obtain a transparent and viscous pepper seed protein peptide solution;
(4) preparation of deodorized garlic liquid: peeling garlic, blanching for 5-10s, and smashing the garlic into pasty garlic juice with a material-water mass ratio of 1: 1; then mixing the garlic juice and edible oil thoroughly, and soaking at 25-30 deg.C for 48 h; extracting volatile matter with pungent odor from garlic solution with edible oil, standing, centrifuging, and extracting middle light green clear liquid to obtain deodorized garlic solution;
(5) preparation of bletilla striata gum: soaking rhizoma bletilla powder in deionized water, filtering, and concentrating the filtrate to obtain gel-like bletilla gum;
(6) the preparation of Pu-Er ripe tea leaching liquor: soaking Pu-Er ripe tea dry tea in water, filtering, and collecting filtrate; mixing the residue of cooked Pu-Er tea, the garlic residue obtained by extracting garlic juice in step (4) and the bletilla striata residue obtained by extracting bletilla striata gum in step (5), soaking in water, filtering, and collecting filtrate; mixing the filtrates to obtain dark brown Pu-Er ripe tea extract;
(7) preparation of pepper seed hair sunscreen: (a) adding the seed coat melanin of the prickly ash seed into the protein peptide solution of the prickly ash seed while stirring, and stirring uniformly to obtain a mixed solution A; (b) mixing extractive solutions of bletilla hyacinthine gum and semen Zanthoxyli, adding cooked Pu-erh tea extract, heating, and stirring to obtain mixed solution B; (d) adding the mixed solution B into the mixed solution A while stirring, stirring uniformly, and cooling to obtain a mixed solution C; (e) and (2) adding the VC and/or VE mixed fine powder into the mixed solution C while stirring, uniformly stirring, adding deodorized garlic juice, uniformly stirring, adjusting the pH to 6.0-6.5, and finally stirring by magnetic force/oscillation for 30min to obtain the dark rattan pepper seed hair sunscreen agent.
5. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in step S1, the leaching at constant temperature is leaching at 80 ℃ for 1 h.
6. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step S1, the ratio of the pepper seed shells to the absolute ethyl alcohol is 1g to 5 mL.
7. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step S1, the sieving is performed by sieving with a 180-200 mesh sieve.
8. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in step S2, the concentration of the NaOH solution is 1.1-1.3 moL/L.
9. A method of preparing a pepper seed hair sunscreen as claimed in claim 8, characterized in that: the concentration of the NaOH solution is 1.2 moL/L.
10. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in step S2, the ratio of the ground black pepper seeds to the NaOH solution is 1g:24.6 mL.
11. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in step S2, the reaction conditions for extracting melanin are as follows: extracting at 70 deg.C for 2 hr for 2 times, and mixing extractive solutions.
12. A method of preparing a pepper seed hair sunscreen as claimed in claim 11, characterized in that: the pH was adjusted to 2.5 for acid precipitation.
13. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in step S3, the alkaline protease solution has a concentration of 10g/L and an activity of 10000U/g, and is stored at 4 ℃ before use.
14. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in step S3, the concentration of the crude pricklyash seed pigment solution is 1 mg/mL; the input amount of the alkaline protease solution is 6 percent of the volume of the crude pepper seed pigment solution.
15. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in step S3, the reaction conditions for deproteinization by the enzymatic hydrolysis method are that the enzymolysis is performed for 1-2h at 50 ℃ and pH = 9; finally, the pH value is adjusted to 2.5 for acid precipitation.
16. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (2), the leaching at constant temperature is carried out for 2h at 80 ℃.
17. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (2), the material liquid ratio of the white pepper seed kernels to the absolute ethyl alcohol is as follows: 1g, 10 mL.
18. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (3), the substrate concentration of the pepper seed protein in the deionized water is 4.9%.
19. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (3), after the preset temperature is 32 ℃, the pH value of the mixed solution is adjusted to 2.5.
20. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (3), the mass ratio of the pepsin to the pepper seed protein solution is 0.9:100, the extraction time is 3 hours, and the specific activity of the pepsin is 1: 3000-3500.
21. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (3), the enzyme deactivation treatment refers to heat preservation in a constant-temperature water bath at 90 ℃ for 15min, and cooling to room temperature.
22. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (3), the centrifugation refers to centrifugation for 10min at the rotating speed of 8000 r/min.
23. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (4), fresh, undamaged, ungerminated, full and glossy perfect garlic is selected as a raw material.
24. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (4), the edible oil comprises soybean oil, peanut oil and rapeseed oil.
25. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (4), the volume ratio of the garlic juice to the edible oil is 100: 1-15.
26. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (5), the addition amount of the deionized water is 15-20 times of the mass of the bletilla striata powder.
27. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (5), the soaking time is 1-2h, and the soaking temperature is 90-95 ℃.
28. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (5), the filtrate is concentrated to 1/4-1/5 times of the original volume, and the gelatinous bletilla hyacinthina gum is obtained.
29. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (6), the feed liquid ratio of the Pu-erh ripe tea leaves to water is 3-5g:100 mL.
30. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (6), the soaking is carried out by adopting hot water with the temperature of 80 ℃, which is beneficial to improving the soaking efficiency.
31. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (6), the material-liquid ratio of the residue to the water is as follows: 5-7g, 50 mL.
32. A method of preparing a pepper seed hair sunscreen as claimed in claim 31, wherein: the residue is Pu-Er ripe tea residue, Bulbus Allii residue after extracting Bulbus Allii juice, and rhizoma bletilla residue after extracting rhizoma bletilla gum.
33. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: in the step (6), warm water with the temperature of 40-60 ℃ is used for soaking in the second step.
34. A process for preparing a pepper seed hair sunscreen as claimed in claim 4, wherein: and (7) finally, stirring by adopting magnetic force/vibration for 30 min.
35. A pepper seed hair sunscreen spray, which is prepared by putting the pepper seed hair sunscreen agent as defined in any one of claims 1-3 or the pepper seed hair sunscreen agent prepared by the method as defined in any one of claims 4-34 in a vacuum spray aluminum bottle.
36. Use of a prickly ash seed hair sunscreen according to any of claims 1-3 or prepared according to the method of any of claims 4-34 in a sunscreen, auxiliary hair coloring 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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