Moisturizing anti-dandruff protein peptide shower gel and preparation method thereof
By using specific ingredients in the shower gel to form a protective film, the problem of existing shower gels being unable to suppress dandruff is solved, achieving the effect of suppressing dandruff during cleansing and moisturizing, and enhancing the skin barrier function.
Patent Information
- Application Number
- CN202610038583.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-13
- Publication Date
- 2026-02-17
AI Technical Summary
Existing shower gels cannot effectively inhibit the formation of dandruff during the cleansing and moisturizing process, especially for users with impaired skin barrier function or metabolic imbalance. Furthermore, the dandruff problem caused by the imbalance between the cleansing system and the hydration-dehydration dynamic has not been effectively resolved.
It employs a succinylated-arginine amphiphilic cleanser based on silk protein peptides, a menthol-modified jojoba ester mixed oil, trimethylglycine phytosterol ester, zein-chitosan genipin copolymer, and capryloyl allantoin glycyrrhizate to form a protective film. Through dynamic hydration locking, biomimetic lipid reconstruction, protease network regulation, and ion channel homeostasis regulation, it inhibits the formation of dandruff.
During the cleansing process, a pH-responsive moisturizing film is established, reducing moisture loss, promoting normal differentiation of the stratum corneum, reducing abnormal shedding, enhancing the skin barrier function, inhibiting the formation of dandruff, and improving skin health.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of daily hygiene and care technology, and particularly relates to a moisturizing and anti-dandruff protein peptide shower gel and a preparation method thereof. BACKGROUND
[0002] Showering can promote blood circulation, improve human microcirculation, enhance mitochondrial activity, reduce inflammation, help recover muscle soreness after exercise and labor, and is conducive to enhancing the regulation ability of the autonomic nervous system and relieving depression or anxiety. However, frequent showering and overuse of shower gel can have a negative impact on skin health, such as causing layered dandruff, dryness and itching, and the like.
[0003] In recent years, shower gel research and production enterprises have made a lot of exploration to solve such problems: (1) Selecting mild surfactants: such as sodium cocoyl glycinate, sodium lauroyl glutamate and other amino acid surfactants, which have moderate cleaning power and a pH close to the natural value of the skin, reducing irritation; such as cocamidopropyl betaine and other zwitterionic surfactants, which are mild and can reduce the irritation of other surfactants; such as APG surfactants of alkyl polyglycosides, which are derived from plants, are mild and environmentally friendly, and are suitable for sensitive skin; (2) Optimizing the pH value: adjusting the formula to a weakly acidic pH of 5.5-6.5, which matches the natural environment of the skin and reduces barrier damage; (3) Adding moisturizing and repairing ingredients: such as glycerin, urea, panthenol, hyaluronic acid and other natural moisturizing factors; such as ceramides, cholesterol, phytosterols and other lipid supplements that can repair the lipid structure of the stratum corneum; such as jojoba oil, shea butter, squalane and other natural oils that can simulate the function of the sebum film; such as bisabolol, oat extract, and gota kola extract, which can reduce the inflammatory response of anti-inflammatory soothing ingredients; (4) Reducing irritating additives: such as avoiding the use of high-concentration alcohol, strong preservatives, fragrances and pigments; (5) Technological innovation: such as liposome encapsulation technology, which encapsulates moisturizing ingredients in liposomes for slow release to extend the moisturizing effect; such as microencapsulated surfactants, which reduce the irritation of surfactants directly contacting the skin.
[0004] However, the currently marketed shower oils and natural mild surfactant-based shower gels still leave a large amount of layered dandruff after use, which is mainly due to: (1) Impaired skin barrier function and metabolic imbalance If the user has atopic dermatitis, ichthyosis or abnormal keratin metabolism, the natural surfactant's mild cleaning cannot completely regulate the abnormal desquamation process; in addition, the barrier repair cycle takes 28-56 days, and short-term use may not have shown the normalizing effect of the stratum corneum; (2) Dual-edged sword effect of the cleaning system The critical micelle concentration of natural surfactants is high, and a high dosage is required to effectively emulsify sebum; in addition, the polarity difference between the occlusive oil in the bath oil and the sebum can cause selective residue and form "false dandruff"; furthermore, the HLB value in the formula is not ideal, and there is a synergistic gap between the oil phase cleaning and the surfactant water phase cleaning; (3) Hydration-dehydration dynamic imbalance Excessive hydration during bathing causes the stratum corneum to swell, and after evaporation, it forms flaky exfoliation; water temperature exceeding 40℃ can activate serine proteases, accelerate desmosome degradation, and exacerbate desquamation; in hard water areas, calcium and magnesium ions form metal soaps with soap residues, causing secondary damage due to mechanical friction.
[0005] Therefore, the current moisturizing and anti-dandruff protein peptide shower gel needs to be further improved. SUMMARY
[0006] The first technical problem to be solved by the present application is to provide a moisturizing and anti-dandruff protein peptide shower gel that can form a protective film on the skin surface to inhibit dandruff based on cleaning and moisturizing.
[0007] The second technical problem to be solved by the present application is to provide a preparation method of the above-mentioned moisturizing and anti-dandruff protein peptide shower gel.
[0008] The technical solution adopted by the present application to solve at least one of the above technical problems is as follows: A moisturizing and anti-dandruff protein peptide shower gel, by weight, comprises the following components: Silk protein peptide-based succinylated-arginine amphiphilic skin cleanser 5-8 parts, Cocoglycoside 3-5 parts, Cocoyl hydrolyzed oat protein potassium 3-6 parts, Sodium lauroyl methyl amino alanine 2-5 parts, Trimethylglycine phytosteryl ester 1-2 parts, Peppermint alcohol modified jojoba ester alcohol mixed oil 2-5 parts, Zein-chitosan genipin copolymer 1-2 parts, Octanoyl allantoin glycyrrhizic acid salt 0.5-1 part, Caprylic / capric glycol ester GTCC 10-20 parts, Isoparaffin 8-12 parts, Polylysine 1-1.5 parts, Plant essential oil 0.3-0.5 parts, Citric acid 1-2 parts, Water 30-62.2 parts.
[0009] In this invention, the succinylated-arginine amphiphilic cleansing agent based on silk protein peptides is obtained through the following steps: (1) Raw material pretreatment Hydrolyzed silk protein peptides were vacuum dried at 40℃ until the moisture content was <1%. Arginine was ball-milled into micro powder with a particle size of <50μm and then dried and stored. Isoalkanes are dehydrated using molecular sieves; Pre-activation treatment of catalyst-immobilized lipase; (2) Amide reaction The dried hydrolyzed silk protein peptides were dispersed in isoalkanes and stirred at 500 rpm. Succinic anhydride was added at 1.2 times the molar ratio of free amino groups of the hydrolyzed silk protein peptides, and immobilized lipase was added at an amount equal to 8% of the protein peptide mass. The reaction is carried out in an ice bath at a controlled temperature of 5-10℃ for 36-48 hours under nitrogen protection and in the dark. After the reaction was completed, the immobilized lipase catalyst was recovered by filtration through a 0.22 μm filter membrane to obtain an isoalkane dispersion of succinylated silk protein peptides. (3) Neutralization reaction Slowly add arginine powder to the above dispersion, with a molar ratio of arginine to succinyl carboxylic acid group of 1:1. Disperse the arginine using a homogenizer at 10,000 rpm for 5 minutes, and then switch to low speed stirring at 200 rpm for 24 hours. The reaction was performed at room temperature, and the carboxylic acid peak at 1700 cm⁻¹ was confirmed by Fourier transform infrared spectroscopy (FTIR). -1 Disappeared, forming a carboxylate 1600 cm -1 The reaction reaches its endpoint; centrifuge at 8000 rpm for 10 min to remove unreacted arginine, and the resulting supernatant is the final product, a succinylated-arginine amphiphilic cleansing agent based on silk protein peptides, which is a pale yellow transparent to semi-transparent dispersion.
[0010] Preferably, the trimethylglycine phytosterol ester is obtained by the following steps: (1) Raw material preparation 1 mol of trimethylglycine, purity ≥98%; The phytosterol used was β-sitosterol, with a purity of ≥95%, 1.2 mol; The catalyst used is p-toluenesulfonic acid with a purity of ≥99%, and the addition amount is 5% of the total weight of trimethylglycine and β-sitosterol. Ethyl acetate was chosen as the solvent. (2) Construction of the reaction apparatus Assemble a reactor with stirring, thermometer, water separator and reflux condenser, and place it in an oil bath; (3) Reaction process Betaine, phytosterols, catalyst, and solvent are added to the reactor and stirred to mix. Heat to reflux, bring to a boil and reflux, turn on stirring at 300-500 rpm to maintain the reaction; collect the generated water through a water separator until the water content no longer increases; The reaction was monitored by TLC or HPLC until the starting material spot disappeared; (4) Post-processing Cool to room temperature, add 5% (v / v) NaHCO3 solution to neutralize the acidity, separate the layers; allow to stand and separate the layers, discard the aqueous phase, and transfer the organic layer to a rotary evaporator to remove the solvent, to obtain the crude product; (5) Purification Recrystallization: The crude product was recrystallized using a mixed solvent of ethanol and water with a volume ratio of 8:2. The product was dried in a vacuum drying oven at 40°C for 24 hours to obtain a white solid product, which is trimethylglycine phytosterol ester.
[0011] Based on its molecular structure, the above-mentioned trimethylglycine phytosterol ester exhibits a dual-effect synergistic effect. Trimethylglycine acts as a potent osmotic pressure regulator, enhancing stratum corneum hydration through the formation of a water-binding network (Humectant index > 0.85). Phytosterol esters, such as β-sitosterol ester, embed themselves in the intercellular lipid layer of keratinocytes via their hydrophobic ends, mimicking the structure of natural cholesterol (similarity > 72%) and reconstructing lamellar body structure. This creates a dual-channel barrier repair mechanism: the trimethylglycine phytosterol ester complex upregulates filaggrin expression (experiments show an increase of approximately 37%) and promotes ceramide EOS synthesis (in vitro, an increase of 19.6%). It also regulates keratin metabolism by inhibiting KLK5 protease activity (IC50 = 3.2 μM), regulating calcium ion gradients, and promoting normal differentiation signals. These mechanisms enable trimethylglycine phytosterol ester to perform the following functions in anti-dandruff shower gels: (1) Dynamic hydration and protection system: By forming a "trimethylglycine-phytosterol" complex with a binding energy of ΔG=-12.3 kcal / moL, a pH-responsive moisturizing film is established during the cleaning process to reduce moisture loss. (2) Biomimetic lipid reconstruction technology: using plant sterol esters as the backbone, C24-C28 alkyl chains, the molar ratio of cholesterol-ceramide-fatty acid in the stratum corneum is reorganized and optimized to a golden ratio of 1:1:1. (3) Protease network regulation: Abnormal desquamation is reduced by competitively inhibiting matrix metalloproteinase MMP-9, Ki=8.7nM; (4) Ion channel homeostasis regulation: Activation of TRPV3 channel, EC50=15μM, promotes calcium oscillation signal transduction, and restores the keratinocyte differentiation cycle to the normal rhythm of 28 days; (5) Enhancement of the microecological barrier: By regulating the expression of antimicrobial peptide hBD-2, it is increased by 2.3 times, inhibiting the formation of Staphylococcus aureus biofilm and blocking the vicious cycle of "itching-scratching-dandruff".
[0012] Preferably, the menthol-modified jojoba ester mixed oil is obtained by the following steps: (1) Material preparation Jojoba oil, purity ≥98%; L-Menthol, pharmaceutical grade; The catalyst is p-toluenesulfonic acid with a purity of ≥99%, and the addition amount is 0.5% of the total weight of jojoba oil and L-menthol.
[0013] (2) Reaction process Jojoba oil and molecular sieve were dehydrated at 100°C, under vacuum and -0.095 MPa for 2 hours. The above-mentioned dehydrated jojoba oil was added into the reactor, followed by the addition of p-toluenesulfonic acid. The reactor was purged with nitrogen three times to maintain a slight positive pressure. Ester exchange reaction: Heat the oil bath to 120°C, and slowly add menthol dropwise to the mixture of jojoba oil and p-toluenesulfonic acid. The molar ratio of jojoba oil to menthol is 1:0.3. The jojoba oil is calculated as eicosenoyl eicosenoic acid eicosenoyl ester, with an average molar mass of 600 g / mol. Maintain a stirring rate of 300 rpm and a reaction time of at least 4 hours. (3) Post-processing The mixture is cooled to 60°C, neutralized with a 2% sodium bicarbonate aqueous solution, allowed to stand and separate into layers, the lower aqueous phase is removed, and the upper oil phase is fed to a rotary evaporator and dehydrated at 40°C and -0.08 MPa until the water content is less than 0.1%, thus obtaining the menthol-modified jojoba ester alcohol mixed oil.
[0014] The aforementioned menthol-modified jojoba ester alcohol blend oil represents an improvement and enhancement of the rapid penetration properties of jojoba oil. Its five core principles for functioning in anti-dandruff body wash are explained, combining molecular mechanisms and clinical applications: (1) Enhanced transdermal delivery and targeting of active ingredients: The molecular weight of the modified ester is reduced to 450-500 Da, while the original jojoba oil is about 600 Da. Its LogP value is increased to 7.2-7.5, which can quickly penetrate through the free diffusion pathway of the lipid bilayer. (2) Dissolve lipid barrier and soften keratin plugs: The terpene structure of menthol can be inserted into the lamellar bodies of the stratum corneum, dissolve the C50-C60 chain length of triglycerides and squalene oxide accumulated at the hair follicle opening, reduce the formation of microcomedones on the scalp, and relieve inflammatory dandruff caused by hair follicle blockage. (3) Regulate the epidermal renewal cycle and resist abnormal keratinization: The menthol group in the modified ester is activated through the TRPM8 receptor, downregulates the STAT3 phosphorylation pathway of keratinocytes, and inhibits excessive proliferation; (4) Relieve inflammatory response and inhibit cytokine storm: In terms of signaling pathways, the modified esters reduce skin erythema and itching by activating PPAR-γ receptor, i.e. peroxisome proliferator-activated receptor, and inhibiting NF-κB-mediated IL-6 and TNF-α release, and are suitable for secondary dandruff in seborrheic dermatitis. (5) Optimize formulation stability and reduce surfactant irritation: The polar ester group of the modified ester forms a micelle complex with nonionic surfactants such as APG, which reduces the critical micelle concentration of anionic surfactants, thereby reducing the damage to the skin barrier during the cleansing process and avoiding the aggravation of dandruff due to excessive degreasing.
[0015] Preferably, the zein-chitosan genipin copolymer is obtained by the following steps: (1) Preparation of materials and reagents Zeat gliadin dissolves in an ethanol solution with a weight percentage of 60%-80%, pH 6.0-7.0, at a weight percentage of 2%-5%. Chitosan dissolves in a 1% (w / w) acetic acid solution at pH 4.0-5.0. For chitosan with a (w / w) concentration of 1%-3%, the degree of deacetylation must be ≥85%. Genipin is soluble in ethanol at a weight percentage concentration of 0.1%-1%, based on the mass of chitosan; PBS buffer, pH 7.4; Deionized water; Dialysis bag, MWCO 3.5-14 kDa; (2) Crosslinking process steps Slowly add the ethanol solution of zein to the chitosan acetate solution while stirring at 500-1000 rpm. Control the mixing mass ratio of zein to chitosan, with zein:chitosan = 1:1~1:2. Adjust the final ethanol volume concentration to ≤30%. After mixing, let stand for 10-20 minutes to eliminate air bubbles. Add genipin solution to the mixture and stir until homogeneous; adjust the pH of the reaction system to 7.5-8.5 with NaHCO3 solution to activate the ring-opening reaction of genipin; stir the reaction at 50-60℃ for 12-24 hours, cool to room temperature, and adjust the pH to neutral. The reaction solution was placed in a dialysis bag and dialyzed with deionized water or PBS buffer to remove unreacted genipin and small molecule byproducts. The dialyzed sample was pre-frozen at -80°C and then freeze-dried for 24-48 hours to obtain a porous complex. The porous complex was sterilized by ethylene oxide treatment to obtain the zein-chitosan-genipin copolymer.
[0016] The aforementioned zein-chitosan genipin copolymer can exert the following effects in anti-dandruff body wash through its unique physicochemical properties and bioactivity: Chitosan's cationic amino group -NH3 inhibits microbial growth to reduce dandruff. + By disrupting microbial cell membranes through electrostatic action, the free amino groups retained after cross-linking of genipin enhance its antibacterial durability, thereby reducing the risk of skin microenvironment flora imbalance and reducing stratum corneum shedding caused by excessive microbial proliferation. Gentle exfoliation promotes the removal of dead skin cells; the hydrophobic particles of zein assist in removing surface-accumulated dandruff through physical friction during bathing, while the mild chelating effect of chitosan softens the stratum corneum and reduces the adhesion of dead skin cells. This synergistic physical and chemical exfoliation avoids the irritation to sensitive skin caused by traditional abrasive particles. Long-lasting moisturizing and skin barrier repair are also provided. Chitosan's strong hydrophilicity forms a moisturizing film that locks in moisture, with a moisture absorption rate of up to 200% of its own weight. The hydrophobic film of zein reduces transepidermal water loss, alleviating dry dandruff and improving flaking caused by barrier damage. Genipin's own free radical scavenging ability, combined with the antioxidant properties of chitosan, delays skin oxidative stress. Soothing and anti-inflammatory, reducing skin irritation: Chitosan reduces the release of inflammatory factors such as IL-6 and TNF-α by inhibiting the NF-κB pathway. The low cytotoxicity of genipin cross-linked products reduces secondary irritation to damaged skin, alleviating inflammatory reactions such as itching and erythema, and reducing dandruff caused by scratching. Enhancing formula stability and improving the user experience: The cross-linked network of the rice extract-chitosan-genipin copolymer acts as a natural thickener, improving the rheological properties of the shower gel. Its cationic properties form a weakly electrostatic complex with anionic surfactants, simultaneously improving the fineness of the foam and the smoothness of rinsing, while reducing the degreasing damage to the skin caused by surfactants.
[0017] Preferably, the capryloyl allantoin glycyrrhizate is obtained by the following steps: (1) Synthesis of N-acylated allantoin 1 mol of allantoin, 1.2 mol of octanoyl chloride, and 1.5 mol of potassium carbonate were dissolved in 200 mL of 2-MeTHF and stirred at room temperature for 6 hours. The reaction endpoint was monitored by TLC. The potassium carbonate and byproduct salts were removed by filtration. The filtrate was concentrated to 1 / 3 of its original volume, and an ethanol / water mixture with a volume ratio of 8:2 was slowly added until a solid precipitated. The solid was filtered, washed with cold water, and dried under vacuum to obtain N-octanoyl allantoin. (2) Salt formation reaction 1 mol of N-octanoyl allantoin and 1 mol of glycyrrhizic acid were dissolved in 50 mL of an ethanol / water mixture with a volume ratio of 9:1. The pH was adjusted to 7.0 with citrate / sodium citrate buffer, stirred at 40°C for 4 hours, and cooled to room temperature to crystallize. The mixture was filtered, the filter cake was washed with 5 mL of cold ethanol, and the product was dried under vacuum to obtain octanoyl allantoin glycyrrhizate.
[0018] The above-mentioned allantoin glycyrrhizate capryloyl works through the following mechanism of action in anti-dandruff body washes: Allantoin softens the stratum corneum and repairs the skin barrier by promoting keratin hydration. The caprylyl group enhances lipid solubility, making it easier to penetrate the dense keratin structure. Glycyrrhizic acid reduces barrier damage by inhibiting inflammatory mediators such as TNF-α and IL-6, thereby alleviating dry dandruff, improving "scaly" desquamation, and repairing the skin's physical barrier. In terms of epidermal renewal regulation, allantoin upregulates filaggrin expression, promoting normal keratinocyte differentiation. The caprylyl group enhances lipid metabolism synergy by regulating PPARγ receptors, thereby reducing lamellar desquamation caused by abnormal keratinization and maintaining a homeostatic epidermal renewal cycle of approximately 28 days. For anti-inflammatory desquamation, glycyrrhizic acid inhibits phospholipase PLA2 and 5-lipoxygenase 5-LOX, blocking the arachidonic acid metabolic chain. It also inhibits the NF-κB pathway, reducing the release of pro-inflammatory factors such as IL-1β and IL-8, targeting psoriasis-like or seborrheic dermatitis-related scaling and reducing erythematous basal inflammation. Microecological regulation: The capryloyl chain C8 cell membrane sterol structure exerts antibacterial effects, while glycyrrhizic acid inhibits bacterial quorum sensing, thereby controlling dandruff caused by excessive fungal proliferation and maintaining the balance of the skin's resident flora. Long-lasting moisturizing synergy: The capryloyl group acts as a "molecular anchor" to enhance the retention of allantoin in the stratum corneum, while glycyrrhizic acid enhances epidermal hydration by activating AQP3 aquaporin. The salt forms of both create a liquid crystal phase sustained-release system, achieving continuous moisturizing for over 24 hours after showering through hydrophilic-hydrophobic balance, breaking the vicious cycle of "dryness-flaking-barrier damage."
[0019] The aforementioned cocoyl glucoside, cocoyl hydrolyzed oat protein potassium, sodium lauroyl methylaminoalanine, caprylic / capric glyceride GTCC, isoparaffin, polylysine, citric acid, and plant essential oils are all commercially available cosmetic-grade products. Among them, cocoyl glucoside, through a three-dimensional mechanism of "gentle cleansing - moisturizing and stabilizing - synergistic active ingredients," serves both as a basic cleansing function and a functional carrier to enhance the overall formula efficacy in anti-dandruff products, making it suitable for long-term care of chronic dandruff problems. Cocoyl hydrolyzed oat protein potassium, through four-dimensional regulation of "cleansing - barrier - immunity - microecology," combines the functions of reducing dandruff and long-term barrier reconstruction. Sodium lauroyl methylaminoalanine is widely used in the field of anti-lamellar dandruff. Caprylic / capric glyceride GTCC, through multiple dimensions such as physical filling, molecular regulation, and biochemical regulation, achieves rapid penetration, long-lasting barrier construction, and maintenance of stratum corneum homeostasis, making it particularly suitable for dry skin, damaged barrier, and abnormal keratinization.
[0020] A method for preparing the above-mentioned moisturizing and anti-dandruff protein peptide shower gel includes the following steps: (1) Pre-mixing preparation Prepare oil phase A material: Caprylic / capric acid glycoside oil ester GTCC is heated to 50-55℃, and while stirring, cocoyl glucoside, succinylated-arginine amphiphilic cleansing agent based on silk protein peptides, cocoyl hydrolyzed oat protein potassium, trimethylglycine phytosterol ester, capryloyl allantoin glycyrrhizate, and menthol-modified jojoba ester mixed oil are added. Stir for at least 1 hour until the system is completely transparent, cool to 30-40℃, add isoparaffin and stir until transparent, then set aside. Prepare aqueous phase B material: Add citric acid to water under stirring until completely dissolved, then add zein-chitosan genipin copolymer and polylysine in batches, and stir at room temperature for at least 3 hours until homogeneous. Add sodium lauroyl methyl amino alanine and stir until completely dissolved. Set aside for later use. (2) Preparation of microemulsion thickener Add oil phase A to a seasoning pot. At 42–45°C and 200 rpm, pour water phase B into A over 30 minutes. Stir at a constant temperature for at least 10 minutes until the material is homogeneous. Then, at 5000–8000 rpm, homogenize at high speed for at least 15 minutes to perform microemulsification and thickening until the material is a thick, semi-transparent microemulsion. Cool to below 35°C, add plant essential oil, and stir for at least 20 minutes until the material is a thick, homogeneous state. The pH of the system is 6.0–6.2. (3) Aging The material obtained in step (2) is aged at room temperature for 20 to 30 hours to obtain the moisturizing and anti-dandruff protein peptide shower gel.
[0021] Compared with existing technologies, the advantages of this invention are as follows: This invention targets the formation mechanism of layered dandruff, creating an electronegative environment with a pH value of 6.0-6.2 on the skin surface. Without damaging the sebum film, a specially formulated succinylated-arginine amphiphilic cleanser based on silk protein peptides is first used to clean the skin surface of dirt. Then, menthol and jojoba oil with natural and rapid penetration properties are used to enhance the transdermal effect, while increasing the oil dispersibility of capryloyl allantoin glycyrrhizate. Thus, moisturizing and anti-allergic ingredients are introduced into the skin in a very short bathing process. Combined with the cationic properties of zein-chitosan genipin copolymer, it flocculates and precipitates together with other substances with potential cationic characteristics during rinsing to form a film that adheres to the skin surface, thereby achieving the effect of inhibiting dandruff formation. Detailed Implementation
[0022] To make the above-mentioned objects, features, and advantages of the present invention more apparent and understandable, specific embodiments of the present invention are described in detail below. Many specific details are set forth in the following description to provide a thorough understanding of the present invention. However, the present invention can be practiced in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below. Example 1
[0023] By weight, the moisturizing and anti-dandruff protein peptide shower gel of this embodiment comprises the following components: 6 kg of succinylated-arginine amphiphilic cleansing agent based on silk protein peptides 5 kg of cocoyl glucoside 5 kg of potassium cocoyl hydrolyzed oat protein 3 kg of sodium lauroyl methyl amino alanine. 2 kg of trimethylglycine phytosterol ester 5 kg of menthol-modified jojoba ester mixed oil, 1 kg of zein-chitosan genipin copolymer 1 kg of capryloyl allantoin glycyrrhizate Caprylic / decanoic acid glycoside oil ester GTCC 15 kg, 8 kg of isoparaffins 1 kg of polylysine 0.3 kg of chamomile essential oil 2 kg of citric acid 45.7 kg of purified water.
[0024] The succinylated-arginine amphiphilic cleansing agent based on silk protein peptides is obtained through the following steps: (1) Raw material pretreatment Hydrolyzed silk protein peptides were vacuum dried at 40℃ until the moisture content was <1%. Arginine was ball-milled into micro powder with a particle size of <50μm and then dried and stored. Isododecane was dehydrated using a molecular sieve. The catalyst was pre-activated by immobilizing the lipase Novozym 435; detailed procedures are as follows: Based on the feed amount, accurately weigh the required mass of Novozym 435 catalyst, which is 8% of the protein peptide mass. Transfer the weighed Novozym 435 to a clean, dry container, add sufficient amount of Isododecane that has been dehydrated by molecular sieves, the volume of the solvent should at least completely submerge the enzyme particles, and leave 3-5 times the volume of space for stirring. In this example, the ratio is controlled to 1 g of enzyme to 10-20 mL of solvent. Constant temperature stirring activation involves sealing the container and placing it on a magnetic stirrer or shaker. Under gentle stirring, avoiding abrasion of the immobilized enzyme carrier due to vigorous stirring, activate at 30-40℃ for 4-8 hours. 30-40℃ can effectively promote the conformational adjustment and activation of the enzyme catalyst, while short-term activation at this temperature will not lead to enzyme inactivation. After activation, the activated enzyme-solvent slurry is directly transferred quantitatively to the stirring reaction system, i.e., the isoparaffin dispersion containing protein peptides, using a pipette or spatula, to ensure complete transfer and reduce loss.
[0025] (2) Amide reaction, introducing oily groups The dried hydrolyzed silk protein peptides were dispersed in isoalkanes and stirred at 500 rpm. Succinic anhydride was added in batches at a ratio of 1.2 times the molar ratio of free amino groups in the hydrolyzed silk protein peptides to avoid local overheating. Immobilized lipase was then added at an amount equal to 8% of the peptide mass. The reaction was carried out in an ice bath at a controlled temperature of 5-10℃ for 40 hours under nitrogen protection and in the dark. After the reaction was completed, the immobilized lipase catalyst was recovered by filtration through a 0.22 μm filter membrane to obtain an isoalkane dispersion of succinylated silk protein peptides. (3) Neutralization reaction, imparting surface activity Slowly add arginine powder to the above dispersion, with a molar ratio of arginine to succinyl carboxylic acid group of 1:1. Disperse the arginine using a homogenizer at 10,000 rpm for 5 minutes, and then switch to low speed stirring at 200 rpm for 24 hours. The reaction was carried out at room temperature (25°C), and the carboxylic acid peak at 1700 cm⁻¹ was confirmed by Fourier transform infrared spectroscopy (FTIR). -1Disappeared, forming a carboxylate 1600 cm -1 The reaction reaches its endpoint; centrifuge at 8000 rpm for 10 min to remove unreacted arginine, and the resulting supernatant is the final product, a succinylated-arginine amphiphilic cleansing agent based on silk protein peptides, which is a pale yellow transparent to semi-transparent dispersion with a particle size <200 nm.
[0026] Trimethylglycine phytosterol ester is obtained through the following steps: (1) Raw material preparation 1 mol of trimethylglycine, purity ≥98%; The phytosterol used was β-sitosterol, with a purity ≥95%; 1.2 mol / L. The catalyst used is p-toluenesulfonic acid with a purity of ≥99%, and the addition amount is 5% of the total weight of trimethylglycine and β-sitosterol. Ethyl acetate was chosen as the solvent; it was used for azeotropic dehydration. (2) Construction of the reaction apparatus Assemble a reactor with stirring, thermometer, water separator and reflux condenser, and place it in an oil bath; (3) Reaction process Betaine, phytosterols, catalyst, and solvent are added to the reactor and stirred to mix. Heat to reflux, bring to a boil and reflux, turn on stirring at 300-500 rpm to maintain the reaction; collect the generated water through a water separator until the water content no longer increases; The reaction was monitored by TLC, with petroleum ether / ethyl acetate as the developing solvent at a ratio of 3:1, until the starting spot disappeared. (4) Post-processing Cool to room temperature, add 5% (v / v) NaHCO3 solution to neutralize the acidity, separate the layers; allow to stand and separate the layers, discard the aqueous phase, and transfer the organic layer to a rotary evaporator to remove the solvent, to obtain the crude product; (5) Purification Recrystallization: The crude product was recrystallized using a mixed solvent of ethanol and water with a volume ratio of 8:2. The product was dried in a vacuum drying oven at 40°C for 24 hours to obtain a white solid product, which is trimethylglycine phytosterol ester.
[0027] Menthol-modified jojoba ester alcohol-oil mixture is obtained by the following steps: (1) Material preparation Jojoba oil, purity ≥98%; L-Menthol, pharmaceutical grade; The catalyst is p-toluenesulfonic acid, with a purity ≥99%, added at a rate of 0.5% of the total weight of jojoba oil and L-menthol. (2) Reaction process Jojoba oil and molecular sieve were dehydrated at 100°C, under vacuum and -0.095 MPa for 2 hours. The above-mentioned dehydrated jojoba oil was added into the reactor, followed by the addition of p-toluenesulfonic acid. The reactor was purged with nitrogen three times to maintain a slight positive pressure. Ester exchange reaction: Heat the oil bath to 120°C, and slowly add menthol dropwise to the mixture of jojoba oil and p-toluenesulfonic acid. The molar ratio of jojoba oil to menthol is 1:0.3. The jojoba oil is calculated as eicosenoyl eicosenoic acid eicosenoyl ester, with an average molar mass of 600 g / mol. Maintain a stirring rate of 300 rpm and a reaction time of at least 4 hours. (3) Post-processing The mixture is cooled to 60°C, neutralized with a 2% sodium bicarbonate aqueous solution, allowed to stand and separate into layers, the lower aqueous phase is removed, and the upper oil phase is fed to a rotary evaporator and dehydrated at 40°C and -0.08 MPa until the water content is less than 0.1%, thus obtaining the menthol-modified jojoba ester alcohol mixed oil.
[0028] Verification: FT-IR analysis, original 1725cm -1 The carbonyl peak of the ester is directed towards 1740 cm⁻¹ -1 Offset, added 1260cm -1 COC characteristic peak.
[0029] The zein-chitosan genipin copolymer is obtained by the following steps: (1) Preparation of materials and reagents Zein is dissolved in a 60% (v / v) ethanol solution at pH 6.0-7.0, with a weight percentage of 2%. Chitosan is dissolved in a 1% (v / v) acetic acid solution at pH 4.0-5.0, with a weight percentage of 2%. The degree of deacetylation of chitosan needs to be ≥85% to increase the amino content and crosslink the active groups. Genipin is dissolved in ethanol at a weight percentage of 0.5%, based on the mass of chitosan; PBS buffer, pH 7.4; Deionized water; Dialysis bag, MWCO 3.5-14 kDa; (2) Crosslinking process steps A zein ethanol solution (60% ethanol, pH 6.5) was slowly added dropwise to a chitosan acetate solution while stirring at 800 rpm. The weight ratio of zein to chitosan was controlled at 1:1. The final ethanol concentration was adjusted to ≤30% to prevent chitosan precipitation. After mixing, the mixture was allowed to stand for 20 minutes to eliminate air bubbles. Add genipin solution to the mixture and stir until homogeneous; adjust the pH of the reaction system to 7.5-8.5 with NaHCO3 solution to activate the ring-opening reaction of genipin; stir the reaction at 60℃ for 15 hours and observe the color change from colorless to light blue to dark blue; cool to room temperature and adjust the pH to neutral 7.0. The reaction solution was placed in a dialysis bag and dialyzed with deionized water or PBS buffer for 3 days, changing the solution 3 times a day to remove unreacted genipin and small molecule byproducts. The dialyzed sample was pre-frozen at -80°C and then freeze-dried for 35 hours to obtain a porous complex. The porous complex was sterilized by ethylene oxide treatment to obtain the zein-chitosan genipin copolymer.
[0030] Capryloyl allantoin glycyrrhizate is obtained by the following steps: (1) Synthesis of N-acylated allantoin 1 mol of allantoin, 1.2 mol of octanoyl chloride, and 1.5 mol of potassium carbonate were dissolved in 200 mL of 2-MeTHF and stirred at room temperature for 6 hours. The reaction endpoint was monitored by TLC with ethyl acetate / methanol as the developing solvent (9:1). The potassium carbonate and byproduct salts were removed by filtration. The filtrate was concentrated to 1 / 3 of its original volume, and an ethanol / water mixture with a volume ratio of 8:2 was slowly added until a solid precipitated. The solid was filtered, washed with cold water, and dried under vacuum to obtain N-octanoyl allantoin with a yield ≥85%. (2) Salt formation reaction 1 mol of N-octanoyl allantoin and 1 mol of glycyrrhizic acid were dissolved in 50 mL of an ethanol / water mixture with a volume ratio of 9:1. The pH was adjusted to 7.0 with citrate / sodium citrate buffer, and the mixture was stirred at 40°C for 4 hours. After cooling to room temperature, crystals were precipitated. The mixture was filtered, and the filter cake was washed with 5 mL of cold ethanol. The product was dried under vacuum to obtain octanoyl allantoin glycyrrhizate with a yield ≥90%. The mother liquor was dehydrated by molecular sieve, and the ethanol was recovered and recycled.
[0031] The above-mentioned cocoyl glucoside, cocoyl hydrolyzed oat protein potassium, lauroyl methyl amino alanine sodium, caprylic / capric acid glycoside ester GTCC, isoparaffin, polylysine, citric acid and plant essential oils are all commercially available cosmetic products.
[0032] The preparation method of the moisturizing and anti-dandruff protein peptide shower gel in this embodiment includes the following steps: (1) Pre-mixing preparation Prepare oil phase A material: Caprylic / capric acid glycoside oil ester GTCC is heated to 50-55℃, and while stirring, cocoyl glucoside, succinylated-arginine amphiphilic cleansing agent based on silk protein peptides, cocoyl hydrolyzed oat protein potassium, trimethylglycine phytosterol ester, capryloyl allantoin glycyrrhizate, and menthol-modified jojoba ester mixed oil are added. Stir for at least 1 hour until the system is completely transparent, cool to 30-40℃, add isoparaffin and stir until transparent, then set aside. Prepare aqueous phase B material: Add citric acid to water under stirring until completely dissolved, then add zein-chitosan genipin copolymer and polylysine in batches, and stir at room temperature for at least 3 hours until homogeneous. Add sodium lauroyl methyl amino alanine and stir until completely dissolved. Set aside for later use. (2) Preparation of microemulsion thickener Add oil phase A to a seasoning pot. At 42-45°C and 200 rpm, pour water phase B into A over 30 minutes. Stir at a constant temperature for at least 10 minutes until the material is homogeneous. Then, at 6000 rpm, homogenize at high speed for at least 15 minutes to perform microemulsification and thickening until the material is a thick, semi-transparent microemulsion. Cool to below 35°C, add plant essential oil, and stir for at least 20 minutes until the material is a thick, homogeneous state. The pH of the system is 6.0-6.2. (3) Aging The material obtained in step (2) is aged at room temperature for 25 hours to obtain a moisturizing and anti-dandruff protein peptide shower gel. Example 2
[0033] By weight, the moisturizing and anti-dandruff protein peptide shower gel of this embodiment comprises the following components: 5 kg of succinylated-arginine amphiphilic cleansing agent based on silk protein peptides. 4 kg of cocoyl glucoside 3 kg of potassium cocoyl hydrolyzed oat protein 2 kg of sodium lauroyl methyl amino alanine 1 kg of trimethylglycine phytosterol ester 3 kg of menthol-modified jojoba ester mixed oil 1.2 kg of zein-chitosan genipin copolymer 0.6 kg of allantoin glycyrrhizate (capryloyl allantoin). Caprylic / decanoic acid glycoside oil ester GTCC 12 kg, 9 kg of isomeric dodecane 1.2 kg of polylysine 0.4 kg of jasmine essential oil 1.2 kg of citric acid 56.4 kg of purified water.
[0034] The methods for obtaining each component and the preparation method of the moisturizing and anti-dandruff protein peptide shower gel in this embodiment are the same as in Example 1. Example 3
[0035] By weight, the moisturizing and anti-dandruff protein peptide shower gel of this embodiment comprises the following components: 8 kg of succinylated-arginine amphiphilic cleansing agent based on silk protein peptides. 3 kg of cocoyl glucoside 6 kg of potassium cocoyl hydrolyzed oat protein 5 kg of sodium lauroyl methyl amino alanine 1.5 kg of trimethylglycine phytosterol ester 4 kg of menthol-modified jojoba ester mixed oil 2 kg of zein-chitosan genipin copolymer 0.8 kg of allantoin glycyrrhizate (capryloyl allantoin). Caprylic / decanoic acid glycoside oil ester GTCC 20 kg, 10 kg of hexadecane 1.5 kg of polylysine 0.5 kg of rose essential oil 1.8 kg of citric acid 35.9 kg of purified water.
[0036] The methods for obtaining each component and the preparation method of the moisturizing and anti-dandruff protein peptide shower gel in this embodiment are the same as in Example 1.
[0037] The performance of the moisturizing and anti-dandruff protein peptide shower gel prepared in Example 1 of this invention was tested. The specific test results are as follows: Evaluation 1. Skin smoothness and moisture level after cleansing The basic skincare properties of the moisturizing and anti-dandruff protein peptide shower gel prepared in Example 1 of this invention were measured compared with those of the commercially available Shubolan peptide refreshing shower gel. The results are shown in Table 1. As can be seen from the test results in Table 1, the moisturizing and anti-dandruff protein peptide shower gel of this invention is superior to the commercially available Shubolan peptide refreshing shower gel in terms of skin smoothness, moisturizing effect, and other skincare indicators.
[0038] Table 1. Measurement of core skincare indicators
[0039] Evaluation 2. Skin irritation after cleansing The irritation of the present invention's cleansing and beauty combination was compared with that of the commercially available Silizi Skin-Soothing Cleansing Gel using the zeaxanthin method: Zein, which is almost completely insoluble in water, interacts with surfactants, increasing its water solubility. Stronger surfactants dissolve zein more readily than weaker ones. Therefore, the solubility of zein after surfactant interaction is determined by observing the change in nitrogen content in aqueous solution before and after surfactant action. The nitrogen content (Zein value in g / L) in the dissolved zein is directly proportional to the skin irritation caused by the surfactant, thus indicating the degree of surfactant irritation. Judgment criteria: Zein > 4, strong irritation; 2 < Zein < 4, low irritation; Zein < 2, no irritation.
[0040] The test results are shown in Table 2. As can be seen from the results in Table 2, the moisturizing and anti-dandruff protein peptide shower gel of the present invention has a much lower skin irritation rate than commercially available Shubolan peptide refreshing shower gel products.
[0041] Table 2. Skin irritation test
[0042] Evaluation 3: Verification of the anti-dandruff effect of the moisturizing and anti-dandruff protein peptide shower gel. I. Testing Methods The anti-dandruff effect was verified using the D-Squame tape method, which involved counting skin flakes on the human skin surface under a microscope.
[0043] Details are as follows: (a) Material preparation D-Squame tape, transparent tape, smooth surface with no sticky residue, 2.2cm in diameter.
[0044] Microscope, equipped with a digital camera and image analysis software.
[0045] Glass slides and coverslips.
[0046] Staining agent: 0.1% methylene blue.
[0047] Fixative: ethanol.
[0048] Tweezers, timer, marker.
[0049] Skin cleansing products, 75% alcohol wipes.
[0050] (II) Operating Procedures 1. Skin preparation Cleanse the skin: Clean the area to be tested, the inside of the arm, with an alcohol swab and let it air dry.
[0051] Leave the skin still: After cleansing, wait 20 minutes to avoid sebum secretion or environmental interference.
[0052] 2. Applying tape Applying the tape: Tear off the D-Squame tape and gently press it onto the target skin area, avoiding air bubbles.
[0053] Pressure standardization: Use uniform pressure, press a 200g weight for 5 seconds to ensure consistency.
[0054] Duration of stay: 5 minutes.
[0055] Removing the tape: Slowly peel off the tape, avoiding folding or contamination.
[0056] 3. Sample Processing Fixation: Place the adhesive side of the tape face up on the glass slide, and add 1-2 drops of acetone or ethanol to fix for 1 minute.
[0057] Staining: Add staining solution, 0.1% methylene blue, to cover the sample and let stand for 3 minutes.
[0058] Cleaning: Gently wash with distilled water to remove excess dye, then air dry or blot dry with filter paper.
[0059] 4. Microscopic observation Microscope settings: Use a 40× objective lens and adjust the light source and contrast.
[0060] Image acquisition: The system scans the tape area and randomly selects at least 5 fields of view to take pictures.
[0061] Skin flake identification: Distinguish skin flakes from impurities based on their shape (such as scaly or translucent) and the depth of their staining.
[0062] 5. Counting and Analysis Manual counting: Directly count the number of dandruff cells in each field of view.
[0063] Software assistance: Use ImageJ software to automatically identify and calculate the dandruff density per unit area.
[0064] Data recording: Record the size, quantity, and distribution characteristics of dandruff.
[0065] II. Test Data (a) Short-term anti-dandruff effect test 1. Experimental Design After washing your body with shower gel, rinse thoroughly, dry, and wait 20 minutes. Then, examine the size, shape, and quantity of the layered skin flakes on the inside of your arm.
[0066] Thirty subjects were included in a two-arm controlled trial. Their ages ranged from 25 to 45 years. The room temperature was 22±1℃ and the RH was 50%. After sampling with D-squame tape, the results were analyzed by ImageJ. The statistical significance of the difference was p<0.01.
[0067] Table 3. Differences in dandruff behavior between the two shower gels under the D-Squame tape method test.
[0068] (II) Long-term anti-dandruff effect test Experimental Design Table
[0069] Table 4. Dandruff Quantity Comparison Table (pieces / mm) 2 Test results
[0070] illustrate: 1. Data format: mean ± standard deviation (counted by microscopy using the D-Squame tape method). 2. Significance markers: * indicates a significant difference between the experimental group and the control group (p<0.05); ** indicates a highly significant difference (p<0.01); 3. Results Analysis: The amount of dandruff in the experimental group of the moisturizing and anti-dandruff protein peptide shower gel of this invention decreased significantly over time, with a 79% reduction from baseline on day 28. The commercially available Suppurant Peptide Refreshing Shower Gel showed no significant improvement in the control group, and some subjects experienced a slight increase in dandruff due to over-cleaning.
[0071] in conclusion: As can be seen from Tables 3 and 4, the moisturizing and anti-dandruff protein peptide shower gel of the present invention has an excellent anti-dandruff effect.
[0072] Evaluation 4. Film-forming coverage and moisturizing effect of the moisturizing and anti-dandruff protein peptide shower gel product. A comparative analysis of the film-forming coverage and moisturizing effect of moisturizing and anti-dandruff protein peptide shower gel and commercially available products was conducted using confocal Raman spectroscopy. Key points of experimental design 1. Sample and Conditions Experimental group: Moisturizing and anti-dandruff protein peptide shower gel of the present invention.
[0073] Control group: Commercially available Suppository Peptide Refreshing Shower Gel.
[0074] Sample size: 30 healthy volunteers, half male and half female, aged 25-45 years, were divided into two groups for cross-testing.
[0075] Environmental control: temperature 22±1°C, humidity 50±5%, uniform rinsing time 2 minutes and drying method.
[0076] 2. Detection Method Film coverage: Confocal Raman spectroscopy at 785nm laser analysis of skin surface characteristic peaks, zein: 1650cm⁻¹ -1 Amide I band; Chitosan: 1080cm -1 COC vibration.
[0077] Moisturizing-related indicators: Simultaneous measurement of transepidermal water loss (TEWL, unit: g / m³) 2 / h) and stratum corneum moisture content (Corneometer® units).
[0078] Table 5. Comparison of Experimental Results on Film-Forming Coverage and Moisturizing Effect of Shower Gel Products
[0079] in conclusion 1. Film-forming advantages: The film coverage of the moisturizing and anti-dandruff protein peptide shower gel microemulsion formulation of this invention is significantly higher than that of commercially available products (92.3% vs. 47.8%), which is attributed to the synergistic film-forming properties of the zein-chitosan copolymer and the uniform distribution resulting from the small particle size (<50nm) of the microemulsion.
[0080] 2. Moisturizing mechanism: The moisturizing and anti-dandruff protein peptide shower gel of this invention creates a high coverage film layer that effectively reduces moisture loss (TEWL is reduced by 43.8%), and maintains the moisture content of the stratum corneum through water-locking.
[0081] 3. Technical advantages: The moisturizing and anti-dandruff protein peptide shower gel microemulsion system of this invention enhances the permeability of active ingredients and prolongs the stability of the film layer, which is significantly better than traditional emulsifiers.
[0082] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0083] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.
Claims
1. A moisturizing and anti-dandruff protein peptide shower gel, characterized in that, By weight, it includes the following components: 5-8 parts of a succinylated-arginine amphiphilic cleansing agent based on silk protein peptides. 3-5 parts of cocoyl glucoside, 3-6 parts of potassium cocoyl hydrolyzed oat protein. Sodium lauroyl methyl amino alanine, 2-5 parts 1-2 parts of trimethylglycine phytosterol ester 2-5 parts of menthol-modified jojoba ester mixed oil 1-2 parts of zein-chitosan genipin copolymer Capryloyl allantoin glycyrrhizate 0.5–1 part, Caprylic / decanoic acid glycoside oil ester GTCC 10-20 parts, 8-12 parts of isoparaffins, Polylysine 1-1.5 parts, 0.3-0.5 parts of plant essential oil, Citric acid 1-2 parts, Water 30-62.2 parts.
2. The moisturizing and anti-dandruff protein peptide shower gel according to claim 1, characterized in that, The succinylated-arginine amphiphilic cleansing agent based on silk protein peptides is obtained by the following steps: (1) Raw material pretreatment Hydrolyzed silk protein peptides were vacuum dried at 40℃ until the moisture content was <1%. Arginine was ball-milled into micro powder with a particle size of <50μm and then dried and stored. Isoalkanes are dehydrated using molecular sieves; Pre-activation treatment of catalyst-immobilized lipase; (2) Amide reaction The dried hydrolyzed silk protein peptides were dispersed in isoalkanes and stirred at 500 rpm. Succinic anhydride was added at 1.2 times the molar ratio of free amino groups of the hydrolyzed silk protein peptides, and immobilized lipase was added at an amount equal to 8% of the protein peptide mass. The reaction is carried out in an ice bath at a controlled temperature of 5-10℃ for 36-48 hours under nitrogen protection and in the dark. After the reaction was completed, the immobilized lipase catalyst was recovered by filtration through a 0.22 μm filter membrane to obtain an isoalkane dispersion of succinylated silk protein peptides. (3) Neutralization reaction Slowly add arginine powder to the above dispersion, with a molar ratio of arginine to succinyl carboxylic acid group of 1:
1. Disperse the arginine using a homogenizer at 10,000 rpm for 5 minutes, and then switch to low speed stirring at 200 rpm for 24 hours. The reaction was performed at room temperature, and the carboxylic acid peak at 1700 cm⁻¹ was confirmed by Fourier transform infrared spectroscopy (FTIR). -1 Disappeared, forming a carboxylate 1600 cm -1 The reaction reaches its endpoint; centrifuge at 8000 rpm for 10 min to remove unreacted arginine, and the resulting supernatant is the final product, a succinylated-arginine amphiphilic cleansing agent based on silk protein peptides, which is a pale yellow transparent to semi-transparent dispersion.
3. The moisturizing and anti-dandruff protein peptide shower gel according to claim 1, characterized in that, The trimethylglycine phytosterol ester is obtained by the following steps: (1) Raw material preparation 1 mol of trimethylglycine, purity ≥98%; The phytosterol used was β-sitosterol, with a purity of ≥95%, 1.2 mol; The catalyst used is p-toluenesulfonic acid with a purity of ≥99%, and the addition amount is 5% of the total weight of trimethylglycine and β-sitosterol. Ethyl acetate was chosen as the solvent. (2) Construction of the reaction apparatus Assemble a reactor with stirring, thermometer, water separator and reflux condenser, and place it in an oil bath; (3) Reaction process Betaine, phytosterols, catalyst, and solvent are added to the reactor and stirred to mix. Heat to reflux, bring to a boil and reflux, turn on stirring at 300-500 rpm to maintain the reaction; collect the generated water through a water separator until the water content no longer increases; The reaction was monitored by TLC or HPLC until the starting material spot disappeared; (4) Post-processing Cool to room temperature, add 5% (v / v) NaHCO3 solution to neutralize the acidity, separate the layers; allow to stand and separate the layers, discard the aqueous phase, and transfer the organic layer to a rotary evaporator to remove the solvent, to obtain the crude product; (5) Purification Recrystallization: The crude product was recrystallized using a mixed solvent of ethanol and water with a volume ratio of 8:
2. The product was dried in a vacuum drying oven at 40°C for 24 hours to obtain a white solid product, which is trimethylglycine phytosterol ester.
4. The moisturizing and anti-dandruff protein peptide shower gel according to claim 1, characterized in that, The menthol-modified jojoba ester alcohol mixture oil is obtained by the following steps: (1) Material preparation Jojoba oil, purity ≥98%; L-Menthol, pharmaceutical grade; The catalyst is p-toluenesulfonic acid, with a purity ≥99%, added at a rate of 0.5% of the total weight of jojoba oil and L-menthol. (2) Reaction process Jojoba oil and molecular sieve were dehydrated at 100°C, under vacuum and -0.095 MPa for 2 hours. The above-mentioned dehydrated jojoba oil was added into the reactor, followed by the addition of p-toluenesulfonic acid. The reactor was purged with nitrogen three times to maintain a slight positive pressure. Ester exchange reaction: Heat the oil bath to 120°C, and slowly add menthol dropwise to the mixture of jojoba oil and p-toluenesulfonic acid. The molar ratio of jojoba oil to menthol is 1:0.
3. The jojoba oil is calculated as eicosenoyl eicosenoic acid eicosenoyl ester, with an average molar mass of 600 g / mol. Maintain a stirring rate of 300 rpm and a reaction time of at least 4 hours. (3) Post-processing The mixture is cooled to 60°C, neutralized with a 2% sodium bicarbonate aqueous solution, allowed to stand and separate into layers, the lower aqueous phase is removed, and the upper oil phase is fed to a rotary evaporator and dehydrated at 40°C and -0.08 MPa until the water content is less than 0.1%, thus obtaining the menthol-modified jojoba ester alcohol mixed oil.
5. The moisturizing and anti-dandruff protein peptide shower gel according to claim 1, characterized in that, The zein-chitosan-genipin copolymer is obtained through the following steps: (1) Preparation of materials and reagents Zeat gliadin dissolves in an ethanol solution with a volume concentration of 60%-80%, pH 6.0-7.0, and a weight percentage concentration of 2%-5%. Chitosan is dissolved in a 1% (v / v) acetic acid solution at pH 4.0-5.0, with a weight percentage of 1%-3%; the degree of deacetylation of chitosan must be ≥85%. Genipin is soluble in ethanol at a weight percentage concentration of 0.1%-1% w / w, based on chitosan mass; PBS buffer, pH 7.4; Deionized water; Dialysis bag, MWCO 3.5-14 kDa; (2) Crosslinking process steps Slowly add the ethanol solution of zein to the chitosan acetate solution while stirring at 500-1000 rpm. Control the mixing mass ratio of zein to chitosan, with zein:chitosan = 1:1~1:
2. Adjust the final ethanol volume concentration to ≤30%. After mixing, let stand for 10-20 minutes to eliminate air bubbles. Add genipin solution to the mixture and stir until homogeneous; adjust the pH of the reaction system to 7.5-8.5 with NaHCO3 solution to activate the ring-opening reaction of genipin; stir the reaction at 50-60℃ for 12-24 hours, cool to room temperature, and adjust the pH to neutral. The reaction solution was placed in a dialysis bag and dialyzed with deionized water or PBS buffer to remove unreacted genipin and small molecule byproducts. The dialyzed sample was pre-frozen at -80°C and then freeze-dried for 24-48 hours to obtain a porous complex. The porous complex was sterilized by ethylene oxide treatment to obtain the zein-chitosan-genipin copolymer.
6. The moisturizing and anti-dandruff protein peptide shower gel according to claim 1, characterized in that, The capryloyl allantoin glycyrrhizate is obtained by the following steps: (1) Synthesis of N-acylated allantoin 1 mol of allantoin, 1.2 mol of octanoyl chloride, and 1.5 mol of potassium carbonate were dissolved in 200 mL of 2-MeTHF and stirred at room temperature for 6 hours. The reaction endpoint was monitored by TLC. The potassium carbonate and byproduct salts were removed by filtration. The filtrate was concentrated to 1 / 3 of its original volume, and an ethanol / water mixture with a volume ratio of 8:2 was slowly added until a solid precipitated. The solid was filtered, washed with cold water, and dried under vacuum to obtain N-octanoyl allantoin. (2) Salt formation reaction 1 mol of N-octanoyl allantoin and 1 mol of glycyrrhizic acid were dissolved in 50 mL of an ethanol / water mixture with a volume ratio of 9:
1. The pH was adjusted to 7.0 with citrate / sodium citrate buffer, stirred at 40°C for 4 hours, and cooled to room temperature to crystallize. The mixture was filtered, the filter cake was washed with 5 mL of cold ethanol, and the product was dried under vacuum to obtain octanoyl allantoin glycyrrhizate.
7. A method for preparing the moisturizing and anti-dandruff protein peptide shower gel according to any one of claims 1 to 6, characterized in that, Includes the following steps: (1) Pre-mixing preparation Prepare oil phase A material: Caprylic / capric acid glycoside oil ester GTCC is heated to 50-55℃, and while stirring, cocoyl glucoside, succinylated-arginine amphiphilic cleansing agent based on silk protein peptides, cocoyl hydrolyzed oat protein potassium, trimethylglycine phytosterol ester, capryloyl allantoin glycyrrhizate, and menthol-modified jojoba ester mixed oil are added. Stir for at least 1 hour until the system is completely transparent, cool to 30-40℃, add isoparaffin and stir until transparent, then set aside. Prepare aqueous phase B material: Add citric acid to water under stirring until completely dissolved, then add zein-chitosan genipin copolymer and polylysine in batches, and stir at room temperature for at least 3 hours until homogeneous. Add sodium lauroyl methyl amino alanine and stir until completely dissolved. Set aside for later use. (2) Preparation of microemulsion thickener Add oil phase A to a seasoning pot. At 42–45°C and 200 rpm, pour water phase B into A over 30 minutes. Stir at a constant temperature for at least 10 minutes until the material is homogeneous. Then, at 5000–8000 rpm, homogenize at high speed for at least 15 minutes to perform microemulsification and thickening until the material is a thick, semi-transparent microemulsion. Cool to below 35°C, add plant essential oil, and stir for at least 20 minutes until the material is a thick, homogeneous state. The pH of the system is 6.0–6.
2. (3) Aging The material obtained in step (2) is aged at room temperature for 20 to 30 hours to obtain the moisturizing and anti-dandruff protein peptide shower gel.