Anti-hair loss shampoo and preparation method thereof

Abstract

The invention discloses anti-hair loss shampoo and a preparation method thereof, and belongs to the technical field of daily chemical products. The anti-hair loss shampoo is prepared from the following components in parts by weight: 80 to 100 parts of sodium lauroyl methyl aminopropionate, 40 to 50 parts of cocamidopropyl betaine, 10 to 20 parts of PEG-7 glyceryl cocoate, 40 to 50 parts of an anti-hair loss active composition, 4 to 6 parts of modified simmondsia chinensis seed oil microbeads, 1 to 3 parts of modified silk fibroin nanofibers, 1 to 3 parts of modified prebiotics, 15 to 25 parts of glycerol, 4 to 6 parts of panthenol, 6 to 10 parts of a preservative, 4 to 6 parts of sodium chloride and 0.5 to 1 part of citric acid, 1 to 3 parts of essence and 700 to 800 parts of deionized water; the anti-hair-loss shampoo is mild in cleaning system, multiple anti-hair-loss effects are achieved through the anti-hair-loss active composition, and the hair nourishing and protecting effects of the shampoo are improved through the synergistic interaction of the three modified substances including the modified simmondsia chinensis seed oil microbeads, the modified silk fibroin nanofibers and the modified prebiotics; the shampoo is especially suitable for people with alopecia caused by scalp sensitivity, dryness and micro-ecological imbalance.

Description

Technical Field

[0001] This invention belongs to the technical field of daily chemical products, specifically relating to an anti-hair loss shampoo and its preparation method. Background Technology

[0002] Hair loss has become a global health concern, affecting hundreds of millions of people worldwide and showing an increasingly younger trend. This huge market demand has spurred a booming market for anti-hair loss shampoos and conditioners, with shampoo, as the most direct and frequently used product, becoming the preferred choice for consumers and a core battleground for market competition.

[0003] Currently, anti-hair loss shampoos on the market can be mainly divided into the following categories according to their mechanism of action: Nutritional replenishment type: These add vitamins (such as biotin and panthenol), amino acids, peptides, etc., aiming to provide nutrition to hair follicles and strengthen hair roots. These products are generally mild but lack specificity, their absorption efficiency is questionable, and their anti-hair loss effect is not significant. Blood circulation stimulation type: These add ingredients such as ginger extract, menthol, niacinamide, etc., to stimulate blood circulation in the scalp capillaries, delivering more oxygen and nutrients to the hair follicles. This method has a certain auxiliary effect, but it only treats the symptoms and not the root cause of hair loss. DHT inhibition type: These add ingredients such as finasteride (banned in some countries), saw palmetto fruit extract, pumpkin seed oil, etc., aiming to inhibit 5α-reductase activity and reduce the production of dihydrotestosterone (DHT), the culprit that causes hair follicle atrophy. This is currently recognized as one of the most effective pathways, but the transdermal absorption rate and efficiency of the ingredients are key bottlenecks. Antibacterial and anti-dandruff type: Contains ingredients such as ketoconazole, zinc pyrithione (ZPT), and salicylic acid. These products reduce scalp inflammation and improve dandruff and itching by inhibiting microorganisms associated with hair loss, such as Malassezia. While these products may have an auxiliary effect on seborrheic alopecia, their ingredients are highly irritating and may indiscriminately kill beneficial bacteria on the scalp, disrupting the microecological balance.

[0004] Therefore, most anti-hair loss shampoos on the market are currently only at the stage of simple compound ingredients, and have significant shortcomings in terms of efficacy, gentleness and long-lasting effect, failing to meet consumers' comprehensive needs for "effective, gentle and long-lasting". Summary of the Invention

[0005] To address the shortcomings mentioned in the background art, the present invention aims to provide an anti-hair loss shampoo and its preparation method. The anti-hair loss shampoo has a gentle cleansing system, and its anti-hair loss active composition provides multiple anti-hair loss measures, including inhibiting DHT, activating hair follicles, promoting microcirculation, nourishing and strengthening hair roots, and inhibiting bacteria and inflammation. Through the synergistic effect of three modified substances—modified jojoba seed oil microbeads, modified silk fibroin nanofibers, and modified prebiotics—the shampoo improves its hair care effects by balancing cleansing power and gentleness, providing immediate and long-lasting hair repair, and regulating the scalp microecology. It is especially suitable for people with hair loss caused by sensitive, dry, or imbalanced scalps.

[0006] The objective of this invention can be achieved through the following technical solutions:

[0007] A hair loss prevention shampoo comprises the following components in parts by weight: 80-100 parts sodium lauroyl methyl aminopropionate, 40-50 parts cocamidopropyl betaine, 10-20 parts PEG-7 glyceryl cocoate, 40-50 parts anti-hair loss active composition, 4-6 parts modified jojoba seed oil microbeads, 1-3 parts modified silk fibroin nanofibers, 1-3 parts modified prebiotics, 15-25 parts glycerin, 4-6 parts panthenol, 6-10 parts preservative, 4-6 parts sodium chloride, 0.5-1 part citric acid, 1-3 parts fragrance, and 700-800 parts deionized water;

[0008] Modified jojoba seed oil microspheres are made by encapsulating natural jojoba seed oil in microcapsules using interfacial polymerization technology, and modifying the outer shell of the microcapsules with the zwitterionic polymer polysulfobetaine; modified silk fibroin nanofibers are made by electrospinning silk fibroin into nanofibers and then functionalizing them with cationic quaternization reaction; modified prebiotics are formed by synthesizing prebiotics and terpinene-4-ol through enzymatic catalysis to form a conjugated product.

[0009] Preferably, the anti-hair loss active composition comprises the following components in parts by weight: 2-4 parts caffeine, 0.5-1.5 parts nicotinamide, 0.5-1.5 parts biotin, 8-12 parts saw palmetto fruit extract, 8-12 parts rosemary extract, 8-12 parts arborvitae leaf extract, 3-5 parts propylene glycol, and 1-3 parts deionized water.

[0010] Preferably, the preservative is a mixture of phenoxyethanol and octyl glycol in a mass ratio of 3:1.

[0011] Preferably, the preparation method of modified jojoba seed oil microspheres includes the following steps:

[0012] A1. Dissolve α-octenyl succinic acid starch ester in deionized water at 60℃ and stir until homogeneous to form an aqueous phase. Mix jojoba seed oil and Tween-80 until homogeneous to form an oil phase.

[0013] A2. Under high-speed shearing, the oil phase is slowly added to the aqueous phase, and shearing is performed for 4 to 6 minutes to form a crude emulsion. The crude emulsion is then homogenized by a high-pressure homogenizer at a pressure of 40 to 60 MPa to obtain a fine microemulsion.

[0014] A3. Add calcium chloride as a crosslinking agent to the microemulsion, stir slowly in a 60°C water bath for 1-3 hours, cool the reaction system to 40°C, add polysulfobetaine, and continue the reaction for 3-5 hours.

[0015] A4. After the reaction is complete, the microbeads are collected by centrifugation and washed three times with deionized water to remove unreacted substances, thus obtaining modified jojoba seed oil microbeads.

[0016] Preferably, the mass ratio of α-octenyl succinate starch ester, jojoba seed oil, calcium chloride, and polysulfobetaine is 1:20:0.5:1.

[0017] Preferably, the preparation method of modified silk fibroin nanofibers includes the following steps:

[0018] B1. Boil the shredded silkworm cocoons in sodium carbonate solution for 20-40 minutes to remove sericin. Wash the degummed silk fibers with water and dissolve them in lithium bromide solution. Place them in a dialysis bag and dialyze against deionized water for 3 days to remove lithium bromide. Centrifuge to remove impurities and obtain a pure silk fibroin aqueous solution.

[0019] B2. Mix the silk fibroin solution with glycidyltrimethylammonium chloride, adjust the pH to 10-11 with NaOH, and react at 60℃ for 4-6 hours;

[0020] B3. The modified silk fibroin solution was loaded into a syringe with a metal needle for electrospinning. The spinning parameters were set as follows: voltage 15-20kV, feed speed 0.5mL / h, and receiving distance 15cm. The nanofiber membrane was collected on the receiving roller.

[0021] B4. The nanofiber membrane was mixed with deionized water and broken up using a probe-type ultrasonic disruptor. The time and power were controlled to obtain a nanofiber dispersion with a length of about 1 to 5 μm. The nanofiber dispersion was centrifuged, filtered, and then vacuum dried to obtain modified silk fibroin nanofibers.

[0022] Preferably, in step B2, the molar ratio of silk fibroin to glycidyltrimethylammonium chloride is 1:0.8.

[0023] Preferably, the preparation method of modified prebiotics includes the following steps:

[0024] C1. Add tert-butanol to a closed reactor, then add fructooligosaccharides, terpinen-4-ol and molecular sieve in sequence, and finally add immobilized lipase. Place the reactor in a constant temperature shaking shaker at 50°C and shake at 150 rpm for 36-48 hours.

[0025] C2. After the reaction is complete, the enzyme and molecular sieve are recovered by filtration, tert-butanol is removed by rotary evaporation, the residue is dissolved in a small amount of deionized water, and the mixture is extracted three times with ether to remove unreacted terpinene-4-ol. The aqueous phase is then freeze-dried to obtain the modified prebiotic.

[0026] Preferably, the mass ratio of fructooligosaccharide, terpinen-4-ol, and immobilized lipase is 10:2:1.

[0027] A method for preparing an anti-hair loss shampoo includes the following steps:

[0028] S1. Under stirring, propylene glycol and deionized water are mixed, and caffeine, nicotinamide and biotin are added in sequence. Stir until completely dissolved, then add saw palmetto fruit extract, rosemary extract and arborvitae leaf extract. Homogenize to fully disperse evenly and prepare an anti-hair loss active composition for later use.

[0029] S2. Add sodium lauroyl methyl aminopropionate, cocamidopropyl betaine, and PEG-7 glyceryl cocoate to deionized water, heat to 75°C, stir until completely dissolved and transparent, and homogenize.

[0030] S3. Cool to below 45°C, slowly add modified jojoba seed oil microspheres, modified silk fibroin nanofibers, modified prebiotics, glycerin, panthenol and preservatives and stir evenly. Then add the anti-hair loss active composition prepared in S1 and stir slowly for 15 minutes to ensure even distribution.

[0031] S4. Add sodium chloride to adjust to a suitable viscosity, adjust the pH to 5.5-6.0 with citric acid, cool to below 35℃, add fragrance, and homogenize to obtain anti-hair loss shampoo.

[0032] The beneficial effects of this invention are:

[0033] This invention's anti-hair loss shampoo utilizes a gentle cleansing system constructed from sodium lauroyl methylaminopropionate, cocamidopropyl betaine, and PEG-7 glyceryl cocoate to provide cleansing power while ensuring gentleness and avoiding irritation to the scalp barrier. The core ingredient is an anti-hair loss active composition. Caffeine penetrates the hair follicles, inhibits 5α-reductase, combats androgenetic alopecia, and stimulates hair follicle growth; niacinamide improves scalp blood circulation, strengthens hair follicles, and reduces inflammation; biotin provides nutrition to hair follicles and improves hair fragility; saw palmetto fruit extract provides a plant-derived 5α-reductase inhibitor, helping to reduce DHT production and synergizing with caffeine; rosemary extract has an anti-hair loss effect comparable to minoxidil, provides antioxidant benefits, and improves blood circulation; and arborvitae leaf extract is used for hair strengthening and has certain anti-inflammatory and cooling effects.

[0034] In addition, the anti-hair loss shampoo of this invention also utilizes three modified substances—modified jojoba seed oil microbeads, modified silk fibroin, and modified prebiotics—to synergistically enhance the hair care effect of the shampoo from three dimensions: balancing cleansing power and gentleness, providing immediate and long-lasting hair repair, and regulating the scalp's microecology. It is especially suitable for people with hair loss caused by sensitive, dry, or imbalanced scalps.

[0035] This invention, modified jojoba seed oil microbeads, addresses the pain points of traditional jojoba seed oil applications. Traditional jojoba seed oil, being a liquid oil, tends to float in shampoo, affecting its appearance, and is easily washed away, resulting in a short duration of effectiveness. In contrast, the modified microbeads, modified using interfacial polymerization and polysulfobetaine, possess slow-release and high adhesion properties. The outer shell of the microbeads protects the internal jojoba seed oil from premature emulsification. Upon contact with the scalp, the oil is slowly released under body temperature and friction, providing long-lasting nourishment to the scalp and hair. The polysulfobetaine-modified outer shell carries zwitterionic properties, allowing it to adhere to the scalp and hair surface through electrostatic attraction, preventing rapid rinsing with running water and extending the moisturizing and repairing time.

[0036] This invention utilizes modified silk fibroin nanofibers to achieve a dual effect of scalp antibacterial and hair repair. Based on its "cationic modification + nanofiber structure" characteristics, its effect in shampoo is precise and efficient: the cationic function, through electrostatic attraction, adheres to the negatively charged scalp surface; the quaternary ammonium cations can destroy the cell membranes of harmful bacteria, and the rosemary extract assists in enhancing the antibacterial effect of the scalp, reducing dandruff and inflammation; the high specific surface area of ​​the nanofiber structure allows it to evenly cover the hair surface, forming a breathable repair film, filling the gaps in damaged hair cuticles, and reducing frizz; at the same time, the natural amino acid components of silk fibroin can nourish the hair, improve hair resilience, and reduce breakage.

[0037] This invention's modified prebiotics improve the scalp environment from the root of "microecology." Traditional prebiotics, when added directly to shampoo, are easily rinsed away and have no antibacterial activity. However, the modified prebiotics' oligofructose-terpinene-4-ol conjugate achieves synergistic microecological regulation and antibacterial effects. The oligofructose fragments can selectively promote the proliferation of beneficial bacteria on the scalp (such as beneficial strains of Staphylococcus) and inhibit harmful bacteria (Malassezia, Staphylococcus aureus), thus balancing the scalp microecology. The terpinene-4-ol fragments can directly inhibit the growth of harmful bacteria, forming a "double protection" with the cationic antibacterial properties of modified silk fibroin. At the same time, its anti-inflammatory properties can help relieve scalp sensitivity.

[0038] The modified jojoba seed oil microbeads of this invention create a balanced charge environment in the hair after cleaning, resulting from the zwitterionic shell. This provides a more uniform and perfect adsorption platform for the strongly positively charged modified silk fibroin nanofibers, avoiding the uneven adsorption of cationic polymers on damaged and healthy hair. The jojoba oil released by the modified jojoba seed oil microbeads can combine with the nanofiber network of the modified silk fibroin nanofibers to form a flexible "oil-encased fiber" protective layer, combining lubrication and support for a more natural and non-stiff repair effect. The gentle cleansing properties of the modified jojoba seed oil microbeads maximize the protection of the scalp barrier, creating a healthy initial environment for the modified prebiotics to regulate the microecology. The antistatic and moisturizing effects of the modified jojoba seed oil microbeads reduce the illusion of scalp itching caused by dryness, making the soothing effect of the modified prebiotics more noticeable. Modified silk fibroin nanofibers and modified prebiotics work synergistically, one focusing on long-lasting hair repair and the other on the root cause of scalp health, addressing hair problems from both internal and external perspectives. A healthy scalp is the foundation for healthy hair growth, while strong hair reduces breakage and makes hair appear fuller.

[0039] Of course, any product implementing this invention does not necessarily need to achieve all of the advantages described above at the same time. Detailed Implementation

[0040] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0041] Example 1

[0042] A modified jojoba seed oil microsphere is prepared by encapsulating natural jojoba seed oil in microcapsules using interfacial polymerization technology, and modifying the microcapsule shell with the zwitterionic polymer polysulfobetaine. The preparation method includes the following steps:

[0043] A1. Dissolve 1g of α-octenyl succinic acid starch ester in 100mL of deionized water at 60℃ and stir until homogeneous to form an aqueous phase. Mix 20g of jojoba seed oil with 0.5g of Tween-80 until homogeneous to form an oil phase.

[0044] A2. Under high-speed shearing (10000 rpm), the oil phase is slowly added to the aqueous phase and sheared for 5 min to form a crude emulsion. The crude emulsion is then homogenized by a high-pressure homogenizer at a pressure of 50 MPa to obtain a fine microemulsion.

[0045] A3. Add 0.2g of calcium chloride as a crosslinking agent to the microemulsion, stir slowly in a 60℃ water bath for 2h, cool the reaction system to 40℃, add 1g of polysulfobetaine, and continue the reaction for 4h.

[0046] A4. After the reaction is complete, the microbeads are collected by centrifugation and washed three times with deionized water to remove unreacted substances, thus obtaining the modified jojoba seed oil microbeads.

[0047] Example 2

[0048] A modified silk fibroin nanofiber is prepared by electrospinning silk fibroin into nanofibers and then functionalizing them with cations using a quaternization reaction. The preparation method includes the following steps:

[0049] B1. Boil the shredded silkworm cocoons in sodium carbonate solution for 30 minutes to remove sericin. Wash the degummed silk fibers with water and dissolve them in 9.5 mol / L lithium bromide solution. Put the solution into a dialysis bag and dialyze against deionized water for 3 days to remove lithium bromide. Centrifuge to remove impurities and obtain a pure silk fibroin aqueous solution.

[0050] B2. Mix silk fibroin solution with glycidyltrimethylammonium chloride at a molar ratio of 1:0.8, adjust the pH to 10-11 with NaOH, and react at 60℃ for 5 hours to allow the epoxy groups of glycidyltrimethylammonium chloride to undergo a ring-opening reaction with the amino and hydroxyl groups of silk fibroin, thereby introducing quaternary ammonium cations.

[0051] B3. The modified silk fibroin solution was loaded into a syringe with a metal needle for electrospinning. The spinning parameters were set as follows: voltage 18kV, feed speed 0.5mL / h, and receiving distance 15cm. The nanofiber membrane was collected on the receiving roller.

[0052] B4. The nanofiber membrane is mixed with deionized water and broken up using a probe-type ultrasonic disruptor. The time and power are controlled to obtain a nanofiber dispersion with a length of about 1 to 5 μm. The nanofiber dispersion is centrifuged, filtered, and then vacuum dried to obtain the modified silk fibroin nanofibers.

[0053] Example 3

[0054] A modified prebiotic is prepared by synthesizing a conjugated product of a prebiotic and terpinene-4-ol via enzymatic catalysis, and the preparation method includes the following steps:

[0055] C1. Add 100 mL of tert-butanol (anhydrous solvent) to a closed reactor, then add 10 g of oligofructose, 2 g of terpinen-4-ol and 5 g of molecular sieve (water produced by adsorption reaction) in sequence, and finally add 1 g of immobilized lipase. Place the reactor in a constant temperature shaking shaker at 50 °C and shake at 150 rpm for 42 h.

[0056] C2. After the reaction is complete, the enzyme and molecular sieve are recovered by filtration, tert-butanol is removed by rotary evaporation, the residue is dissolved in a small amount of deionized water, and the mixture is extracted three times with diethyl ether to remove unreacted terpinene-4-ol. The aqueous phase is then freeze-dried to obtain the modified prebiotic.

[0057] Example 4

[0058] A hair loss prevention shampoo comprises the following components in parts by weight: 80 parts sodium lauroyl methylaminopropionate, 50 parts cocamidopropyl betaine, 10 parts PEG-7 glyceryl cocoate, 50 parts anti-hair loss active composition, 4 parts modified jojoba seed oil microbeads, 3 parts modified silk fibroin nanofibers, 1 part modified prebiotic, 25 parts glycerin, 4 parts panthenol, 7.5 parts phenoxyethanol, 2.5 parts caprylyl glycol, 4 parts sodium chloride, 1 part citric acid, 1 part fragrance, and 800 parts deionized water; the modified jojoba seed oil microbeads were prepared in Example 1, the modified silk fibroin nanofibers were prepared in Example 2, and the modified prebiotic was prepared in Example 3.

[0059] The anti-hair loss active composition comprises the following components in parts by weight: 4 parts caffeine, 1.5 parts nicotinamide, 1.5 parts biotin, 12 parts saw palmetto fruit extract, 12 parts rosemary extract, 12 parts arborvitae leaf extract, 4.5 parts propylene glycol, and 2.5 parts deionized water;

[0060] The preparation method of the above-mentioned anti-hair loss shampoo includes the following steps:

[0061] S1. Under stirring, propylene glycol and deionized water are mixed, and caffeine, nicotinamide and biotin are added in sequence. Stir until completely dissolved, then add saw palmetto fruit extract, rosemary extract and arborvitae leaf extract. Homogenize to fully disperse evenly and prepare an anti-hair loss active composition for later use.

[0062] S2. Add sodium lauroyl methyl aminopropionate, cocamidopropyl betaine, and PEG-7 glyceryl cocoate to deionized water, heat to 75°C, stir until completely dissolved and transparent, and homogenize.

[0063] S3. Cool to below 45°C, slowly add modified jojoba seed oil microspheres, modified silk fibroin nanofibers, modified prebiotics, glycerin, panthenol, phenoxyethanol and octyl glycol and stir evenly. Then add the anti-hair loss active composition prepared in S1 and stir slowly for 15 minutes to ensure even distribution.

[0064] S4. Add sodium chloride to adjust to a suitable viscosity, adjust the pH to 5.5-6.0 with citric acid, cool to below 35°C, add fragrance, and homogenize to obtain the anti-hair loss shampoo.

[0065] Example 5

[0066] A hair loss prevention shampoo comprises the following components in parts by weight: 100 parts sodium lauroyl methylaminopropionate, 40 parts cocamidopropyl betaine, 20 parts PEG-7 glyceryl cocoate, 40 parts anti-hair loss active composition, 6 parts modified jojoba seed oil microbeads, 1 part modified silk fibroin nanofibers, 3 parts modified prebiotics, 15 parts glycerin, 6 parts panthenol, 4.5 parts phenoxyethanol, 1.5 parts caprylyl glycol, 6 parts sodium chloride, 0.5 parts citric acid, 3 parts fragrance, and 700 parts deionized water; the modified jojoba seed oil microbeads were prepared in Example 1, the modified silk fibroin nanofibers were prepared in Example 2, and the modified prebiotics were prepared in Example 3.

[0067] The anti-hair loss active composition comprises the following components in parts by weight: 2 parts caffeine, 0.5 parts nicotinamide, 0.5 parts biotin, 12 parts saw palmetto fruit extract, 8 parts rosemary extract, 12 parts arborvitae leaf extract, 3.5 parts propylene glycol, and 1.5 parts deionized water;

[0068] The preparation method of the above-mentioned anti-hair loss shampoo includes the following steps:

[0069] S1. Under stirring, propylene glycol and deionized water are mixed, and caffeine, nicotinamide and biotin are added in sequence. Stir until completely dissolved, then add saw palmetto fruit extract, rosemary extract and arborvitae leaf extract. Homogenize to fully disperse evenly and prepare an anti-hair loss active composition for later use.

[0070] S2. Add sodium lauroyl methyl aminopropionate, cocamidopropyl betaine, and PEG-7 glyceryl cocoate to deionized water, heat to 75°C, stir until completely dissolved and transparent, and homogenize.

[0071] S3. Cool to below 45°C, slowly add modified jojoba seed oil microspheres, modified silk fibroin nanofibers, modified prebiotics, glycerin, panthenol, phenoxyethanol and octyl glycol and stir evenly. Then add the anti-hair loss active composition prepared in S1 and stir slowly for 15 minutes to ensure even distribution.

[0072] S4. Add sodium chloride to adjust to a suitable viscosity, adjust the pH to 5.5-6.0 with citric acid, cool to below 35°C, add fragrance, and homogenize to obtain the anti-hair loss shampoo.

[0073] Example 6

[0074] A hair loss prevention shampoo comprises the following components in parts by weight: 90 parts sodium lauroyl methylaminopropionate, 45 parts cocamidopropyl betaine, 15 parts PEG-7 glyceryl cocoate, 45 parts anti-hair loss active composition, 5 parts modified jojoba seed oil microbeads, 2 parts modified silk fibroin nanofibers, 2 parts modified prebiotics, 20 parts glycerin, 5 parts panthenol, 6 parts phenoxyethanol, 2 parts caprylyl glycol, 5 parts sodium chloride, 0.8 parts citric acid, 2 parts fragrance, and 750 parts deionized water; the modified jojoba seed oil microbeads were prepared in Example 1, the modified silk fibroin nanofibers were prepared in Example 2, and the modified prebiotics were prepared in Example 3.

[0075] The anti-hair loss active composition comprises the following components in parts by weight: 3 parts caffeine, 1 part nicotinamide, 1 part biotin, 12 parts saw palmetto fruit extract, 12 parts rosemary extract, 10 parts arborvitae leaf extract, 4 parts propylene glycol, and 2 parts deionized water.

[0076] The preparation method of the above-mentioned anti-hair loss shampoo includes the following steps:

[0077] S1. Under stirring, propylene glycol and deionized water are mixed, and caffeine, nicotinamide and biotin are added in sequence. Stir until completely dissolved, then add saw palmetto fruit extract, rosemary extract and arborvitae leaf extract. Homogenize to fully disperse evenly and prepare an anti-hair loss active composition for later use.

[0078] S2. Add sodium lauroyl methyl aminopropionate, cocamidopropyl betaine, and PEG-7 glyceryl cocoate to deionized water, heat to 75°C, stir until completely dissolved and transparent, and homogenize.

[0079] S3. Cool to below 45°C, slowly add modified jojoba seed oil microspheres, modified silk fibroin nanofibers, modified prebiotics, glycerin, panthenol, phenoxyethanol and octyl glycol and stir evenly. Then add the anti-hair loss active composition prepared in S1 and stir slowly for 15 minutes to ensure even distribution.

[0080] S4. Add sodium chloride to adjust to a suitable viscosity, adjust the pH to 5.5-6.0 with citric acid, cool to below 35°C, add fragrance, and homogenize to obtain the anti-hair loss shampoo.

[0081] Comparative Example 1

[0082] A hair loss prevention shampoo, without the addition of modified jojoba seed oil microbeads, with other components and contents the same as in Example 6, and the components of the hair loss prevention active composition are also the same as in Example 6;

[0083] The preparation method of the above-mentioned anti-hair loss shampoo is the same as that in Example 6, except that modified jojoba seed oil microbeads are not added in step S3.

[0084] Comparative Example 2

[0085] A hair loss prevention shampoo, without added modified silk fibroin nanofibers, with other components and contents the same as in Example 6, and the components of the hair loss prevention active composition are also the same as in Example 6;

[0086] The preparation method of the above-mentioned anti-hair loss shampoo is the same as that in Example 6, except that modified silk fibroin nanofibers are not added in step S3.

[0087] Comparative Example 3

[0088] A hair loss prevention shampoo, without added modified prebiotics, with other components and contents the same as in Example 6, and the components of the hair loss prevention active composition are also the same as in Example 6;

[0089] The preparation method of the above-mentioned anti-hair loss shampoo is the same as that in Example 6, except that modified prebiotics are not added in step S3.

[0090] Comparative Example 4

[0091] A hair loss prevention shampoo, without modified jojoba seed oil microbeads and modified silk fibroin nanofibers, with other components and contents the same as in Example 6, and the components of the hair loss prevention active composition are also the same as in Example 6;

[0092] The preparation method of the above-mentioned anti-hair loss shampoo is the same as that in Example 6, except that modified jojoba seed oil microspheres and modified silk fibroin nanofibers are not added in step S3.

[0093] Comparative Example 5

[0094] A hair loss prevention shampoo, without added modified silk fibroin nanofibers and modified prebiotics, with other components and contents the same as in Example 6, and the components of the hair loss prevention active composition are also the same as in Example 6;

[0095] The preparation method of the above-mentioned anti-hair loss shampoo is the same as that in Example 6, except that modified silk fibroin nanofibers and modified prebiotics are not added in step S3.

[0096] Comparative Example 6

[0097] A hair loss prevention shampoo, without modified jojoba seed oil microbeads and modified prebiotics, with other components and contents the same as in Example 6, and the components of the hair loss prevention active composition are also the same as in Example 6;

[0098] The preparation method of the above-mentioned anti-hair loss shampoo is the same as that in Example 6, except that modified jojoba seed oil microbeads and modified prebiotics are not added in step S3.

[0099] Comparative Example 7

[0100] A hair loss prevention shampoo, without modified jojoba seed oil microbeads, modified silk fibroin nanofibers and modified prebiotics, with other components and contents the same as in Example 6, and the components of the hair loss prevention active composition are also the same as in Example 6;

[0101] The preparation method of the above-mentioned anti-hair loss shampoo is the same as that in Example 6, except that modified jojoba seed oil microspheres, modified silk fibroin nanofibers and modified prebiotics are not added in step S3.

[0102] Performance testing

[0103] The anti-hair loss shampoos prepared in Example 6 and Comparisons 1-7 were left to stand for 24 hours at 25°C and 50% relative humidity, and then the following tests were performed:

[0104] I. Basic Performance Testing

[0105] pH measurement: A pH meter (accuracy ±0.01) was used. 20 mL of the sample dilution (1:10) was taken, and the average value was calculated in triplicate at 25℃. Viscosity measurement: A rotational viscometer (NDJ-5S) was used. The viscosity was measured at 60 rpm at 25℃, and the reading was taken after equilibration for 3 minutes. The measurement was repeated in triplicate. Foaming properties: The Roche foam analyzer method was used. 50 mL of 1% sample solution (hard water hardness 150 ppm) was used. The initial foam volume (mL) and foam retention rate (%) after 5 minutes were measured at 30℃. Thermal cycling test: -5℃ freezing for 24 hours → 25℃ recovery for 2 hours → 45℃ heating for 24 hours → 25℃ recovery for 2 hours, repeated for 5 cycles. The appearance, layering, and viscosity changes were observed. Centrifugation stability: Centrifugation at 3000 rpm for 30 minutes was performed, and layering or precipitation was observed. The data obtained are shown in Table 1 below.

[0106] Table 1. Test Results of Basic Performance of Anti-Hair Loss Shampoo

[0107]

[0108]

[0109] The data in Table 1 shows that:

[0110] All groups had pH values ​​between 5.5 and 5.7 (the slightly acidic environment of the scalp), and the differences in viscosity and foaming properties were small, indicating that the addition of modified materials did not affect the basic performance of the shampoo. Comparative Example 7 showed slight stratification and precipitation, indicating that the three modified materials (especially jojoba microbeads and silk fibroin) have a positive effect on improving the stability of the formula.

[0111] II. Hair loss prevention and hair care effect test

[0112] (1) Anti-hair loss efficacy test

[0113] To investigate the telogen effluvium rate, 40 volunteers aged 25-45 with seborrheic alopecia were recruited, with an equal number of men and women. They were randomly divided into 8 groups of 5 people each, and there were no significant differences in age, gender, and baseline scalp moisture levels among the participants in each group. They used the corresponding shampoo continuously for 4 weeks, and hair loss during shampooing was collected weekly. The proportion of telogen effluvium hairs (hair roots that are white and club-shaped) to the total amount of hair loss was calculated to determine the telogen effluvium rate.

[0114] Hair follicle survival rate was determined by taking hair follicles from the scalp of healthy individuals (donations), dividing them into 8 groups for culture, and adding a corresponding shampoo dilution solution (1:100, simulating the residual concentration on the scalp) to each group. After 7 days of culture, the activity of hair follicle cells was detected by the MTT assay, and the survival rate was calculated.

[0115] (2) Scalp repair effect test

[0116] Scalp moisture content was measured using the German CKMPA580 multifunctional skin analyzer. Forty volunteers aged 25-45 years, with equal numbers of men and women, and no history of scalp inflammation, wounds, or allergies, were recruited. They had not used other anti-hair loss / moisturizing shampoos in the past month, and their baseline scalp moisture value was within the "normal range (moisture index 40-60)" or "mildly dry (moisture index 30-40)" (to avoid extreme dryness / oiliness affecting data comparison). They were randomly divided into 8 groups of 5 people each, and there were no significant differences in age, gender, or baseline scalp moisture value among the groups. Participants were required to stop washing their hair 12 hours in advance and enter the laboratory 30 minutes before the test to acclimatize to the environment. Before shampooing, the original scalp moisture content was measured. After shampooing according to standard methods, the scalp was rinsed with warm water and the scalp was gently patted with a lint-free towel until semi-dry (to avoid friction damage). 24 hours after shampooing (during which time participants lived normal lives, avoiding shampooing, strenuous exercise, and sweating), the same area was tested again.

[0117] To investigate scalp microbiota balance, 40 volunteers aged 25-45 years with no history of scalp inflammation, wounds, or allergies were recruited. The volunteers were divided into 8 groups of 5 people each. There were no significant differences in age, gender, or baseline scalp moisture levels among the groups. The volunteers used the corresponding shampoo continuously for 4 weeks. Scalp samples were collected from the volunteers before and 2 weeks after shampoo use. Microbial DNA was extracted, and the ratio of Staphylococcus (beneficial bacteria) to Malassezia (harmful bacteria) was analyzed by 16S rRNA sequencing.

[0118] To investigate the levels of scalp inflammatory factors, 40 healthy adult volunteers aged 25-45 years with mild scalp sensitivity (such as occasional itching and redness) were recruited, with an equal number of men and women. Those with scalp diseases (such as seborrheic dermatitis and psoriasis) or who had used anti-inflammatory / hormonal products or oral medications within the past month were excluded. The scalp was uniformly selected from the top and back of the head. One day before the experiment, the scalp was cleaned with sterile saline solution and left to air dry for 30 minutes for the first sample collection. Participants then used a standardized shampoo (once daily, lathering and leaving on for 3 minutes before rinsing) for 28 consecutive days (the metabolic cycle of scalp inflammatory factors is approximately 4 weeks, allowing for long-term effects). On the 28th day, a second sample was collected 24 hours after shampooing. A sterile cotton swab dipped in 0.9% sterile saline solution was used to gently wipe the collection site (approximately 2 cm in diameter). (m area) Remove surface dirt, take a sterile polyvinylidene fluoride (PVDF) membrane (pore size 0.22μm), moisten it with sterile physiological saline and attach it to the collection site. Apply slight pressure (about 50g) for 10 minutes to transfer the exudate (containing inflammatory factors) from the scalp surface to the membrane. Place the PVDF membrane in a centrifuge tube containing 1mL of sterile phosphate buffered saline (PBS, pH 7.4, containing protease inhibitors to prevent degradation of inflammatory factors), shake at 4℃ for 30 minutes to fully dissolve the inflammatory factors, centrifuge at 4℃ and 12000rpm for 10 minutes, collect the supernatant, aliquot and freeze at -80℃. Use enzyme-linked immunosorbent assay (ELISA) to detect the concentration of tumor necrosis factor-α (TNF-α) pro-inflammatory factor, and calculate the ratio of the concentration after intervention to the concentration after use.

[0119] The scalp tightness rating assay recruited 40 volunteers aged 25-45 years with no history of scalp inflammation, wounds, or allergies, and an equal number of men and women. They were randomly divided into 8 groups of 5 participants each. There were no significant differences in age, gender, or baseline scalp moisture levels among the groups. Participants were required to use the corresponding shampoo continuously for 7 days (once daily, always in the evening) to avoid the randomness of a single use and to reflect changes in tightness after long-term use. A standardized score was used: 1 point indicates no tightness, the scalp is completely relaxed, and there is no dryness, pulling, or tightness. 1. Soft and smooth to the touch; 2. Slight tightness, occasional slight dryness of the scalp, no obvious pulling sensation, does not affect daily activities; 3. Moderate tightness, the scalp is constantly dry and tight, slightly rough to the touch, and occasionally has a slight pulling sensation; 4. Obvious tightness, the scalp is obviously dry and tight, accompanied by slight pulling pain, and requires conscious adjustment of posture (such as avoiding looking down) during daily activities; 5. Severe tightness, the scalp is extremely tight and dry, accompanied by obvious pulling pain, and may even cause scalp peeling, affecting normal life.

[0120] (3) Hair care effect test

[0121] Hair strands of the same type (healthy medium-length hair, diameter 0.05-0.06mm) were selected, with 100 strands processed in each sample group. After washing with the corresponding shampoo, the breaking strength, frizziness, and moisture retention rate were tested under standard conditions, and the average value was taken. The breaking strength test used a fiber strength tester (YG001A) to measure the force required for the hair strand to break in a wet state. The frizziness test used a laser particle size analyzer (MalvernMastersizer3000) to detect the surface roughness of the hair strand. The moisture retention rate was measured by placing the hair strand in a constant temperature and humidity chamber (25℃, RH40%) for 24 hours to determine the residual moisture rate.

[0122] The obtained data is shown in Table 2 below:

[0123] Table 2. Results of the test on the anti-hair loss shampoo and hair care effects.

[0124]

[0125] The data in Table 2 shows that:

[0126] Example 6 showed that the scalp moisture content was 4.3 g / cm³ higher than that of Comparative Example 1. 2 The tightness score of Example 6 was 1.1 points higher than that of Comparative Example 1, indicating that the slow-release moisturizing properties of jojoba microbeads can significantly improve scalp hydration and relieve tightness after cleansing. Traditional jojoba seed oil is easily lost, while the adsorption and slow-release function of microbeads prolongs the moisturizing time. At the same time, the hair breaking strength of Example 6 was 1.6 cN higher than that of Comparative Example 1, and the moisturizing rate was 16.2% higher than that of Comparative Example 1, indicating that the oil released by the microbeads can repair the hair cuticle and enhance the toughness and water retention of the hair. The hair performance of Comparative Example 3 was similar to that of Example 6, further proving that jojoba microbeads are the core contributor to hair care.

[0127] Example 6 showed a 1.7-fold higher bacterial balance and a 9.3 pg / mL lower TNF-α content than Comparative Example 2, indicating that the cationic antibacterial function of silk fibroin can inhibit harmful bacteria and reduce the release of inflammatory factors. Comparative Example 4 showed a slightly lower bacterial balance than Comparative Example 2, further verifying the antibacterial advantage of silk fibroin. Meanwhile, Example 6 showed a 0.53 μm lower hair frizz than Comparative Example 2, a significant difference, indicating that the film-forming properties of nanofibers can cover the hair surface, fill the gaps in the hair cuticle, and reduce frizz. Comparative Example 7 showed the highest frizz, proving that silk fibroin is the key to improving hair smoothness.

[0128] Example 6 showed a 14.4% lower telogen effluvium rate and a 20.9% higher hair follicle survival rate than Comparative Example 3, with the most significant difference. This indicates that the microecological regulation of prebiotics can improve the hair follicle environment from the root. The telogen effluvium rate of Comparative Example 5 was close to that of Comparative Example 7, proving that prebiotics are the core synergist of the anti-hair loss system. The bacterial flora balance of Example 6 was 2.6 higher than that of Comparative Example 3, indicating that prebiotics can promote the proliferation of beneficial bacteria. Although the bacterial flora balance of Comparative Example 2 was lower than that of Example 6, it was higher than that of Comparative Example 3, reflecting the synergistic effect of silk fibroin antibacterial and prebiotics promoting beneficial bacteria.

[0129] The telogen effluvium rate in Comparative Example 7 was 26.9% higher than that in Example 6, while the hair loss rate in Comparative Example 3 was significantly higher than that in Example 6, indicating that prebiotics are the core of hair loss prevention. However, the nourishing properties of jojoba microbeads (3.3% higher in Comparative Example 1 than in Example 6) and the anti-inflammatory properties of silk fibroin (7.1% higher in Comparative Example 2 than in Example 6) can help improve the hair loss prevention effect. The TNF-α content in Example 6 was 22.4 pg / mL lower than that in Comparative Example 5, demonstrating the synergistic effect of antibacterial properties of silk fibroin and anti-inflammatory properties of prebiotics. The moisturizing properties of jojoba microbeads further enhanced the scalp barrier function. The hair breakage strength in Example 6 was 3.0 cN higher than that in Comparative Example 4, indicating that the nourishing properties of jojoba and the film-forming properties of silk fibroin provide dual repair, with an effect far superior to that of a single material.

[0130] The above description is merely an example and illustration of the concept of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described or use similar methods to replace them, as long as they do not deviate from the concept of the invention or exceed the scope defined in the claims, they should all fall within the protection scope of the present invention.

Claims

1. A hair loss prevention shampoo, characterized in that: The product comprises the following components by weight: 80-100 parts sodium lauroyl methyl aminopropionate, 40-50 parts cocamidopropyl betaine, 10-20 parts PEG-7 glyceryl cocoate, 40-50 parts anti-hair loss active composition, 4-6 parts modified jojoba seed oil microbeads, 1-3 parts modified silk fibroin nanofibers, 1-3 parts modified prebiotics, 15-25 parts glycerin, 4-6 parts panthenol, 6-10 parts preservative, 4-6 parts sodium chloride, 0.5-1 part citric acid, 1-3 parts fragrance, and 700-800 parts deionized water. The modified jojoba seed oil microspheres are made by encapsulating natural jojoba seed oil in microcapsules using interfacial polymerization technology, and modifying the microcapsule shell with the zwitterionic polymer polysulfobetaine; the modified silk fibroin nanofibers are made by electrospinning silk fibroin into nanofibers and then functionalizing them with cationic quaternization reaction; the modified prebiotics are formed by synthesizing prebiotics and terpinene-4-ol through enzymatic catalysis to form a conjugated product.

2. The anti-hair loss shampoo according to claim 1, characterized in that: The anti-hair loss active composition comprises the following components in parts by weight: 2-4 parts caffeine, 0.5-1.5 parts nicotinamide, 0.5-1.5 parts biotin, 8-12 parts saw palmetto fruit extract, 8-12 parts rosemary extract, 8-12 parts arborvitae leaf extract, 3-5 parts propylene glycol, and 1-3 parts deionized water.

3. The anti-hair loss shampoo according to claim 1, characterized in that: The preservative is a mixture of phenoxyethanol and octyl glycol in a mass ratio of 3:

1.

4. The anti-hair loss shampoo according to claim 1, characterized in that: The preparation method of the modified jojoba seed oil microspheres includes the following steps: A1. Dissolve α-octenyl succinic acid starch ester in deionized water at 60℃ and stir until homogeneous to form an aqueous phase. Mix jojoba seed oil and Tween-80 until homogeneous to form an oil phase. A2. Under high-speed shearing, the oil phase is slowly added to the aqueous phase, and shearing is performed for 4 to 6 minutes to form a crude emulsion. The crude emulsion is then homogenized by a high-pressure homogenizer at a pressure of 40 to 60 MPa to obtain a fine microemulsion. A3. Add calcium chloride as a crosslinking agent to the microemulsion, stir slowly in a 60°C water bath for 1-3 hours, cool the reaction system to 40°C, add polysulfobetaine, and continue the reaction for 3-5 hours. A4. After the reaction is complete, the microbeads are collected by centrifugation and washed three times with deionized water to remove unreacted substances, thus obtaining the modified jojoba seed oil microbeads.

5. The anti-hair loss shampoo according to claim 4, characterized in that: The mass ratio of α-octenyl succinic starch ester, jojoba seed oil, calcium chloride, and polysulfobetaine is 1:20:0.5:

1.

6. The anti-hair loss shampoo according to claim 1, characterized in that: The preparation method of the modified silk fibroin nanofibers includes the following steps: B1. Boil the shredded silkworm cocoons in sodium carbonate solution for 20-40 minutes to remove sericin. Wash the degummed silk fibers with water and dissolve them in lithium bromide solution. Place them in a dialysis bag and dialyze against deionized water for 3 days to remove lithium bromide. Centrifuge to remove impurities and obtain a pure silk fibroin aqueous solution. B2. Mix the silk fibroin solution with glycidyltrimethylammonium chloride, adjust the pH to 10-11 with NaOH, and react at 60℃ for 4-6 hours; B3. The modified silk fibroin solution was loaded into a syringe with a metal needle for electrospinning. The spinning parameters were set as follows: voltage 15-20kV, feed speed 0.5mL / h, and receiving distance 15cm. The nanofiber membrane was collected on the receiving roller. B4. The nanofiber membrane is mixed with deionized water and broken up using a probe-type ultrasonic disruptor. The time and power are controlled to obtain a nanofiber dispersion with a length of about 1 to 5 μm. The nanofiber dispersion is centrifuged, filtered, and then vacuum dried to obtain the modified silk fibroin nanofibers.

7. The anti-hair loss shampoo according to claim 6, characterized in that: In step B2, the molar ratio of silk fibroin to glycidyltrimethylammonium chloride is 1:0.

8.

8. The anti-hair loss shampoo according to claim 1, characterized in that: The method for preparing the modified prebiotic includes the following steps: C1. Add tert-butanol to a closed reactor, then add fructooligosaccharides, terpinen-4-ol and molecular sieve in sequence, and finally add immobilized lipase. Place the reactor in a constant temperature shaking shaker at 50°C and shake at 150 rpm for 36-48 hours. C2. After the reaction is complete, the enzyme and molecular sieve are recovered by filtration, tert-butanol is removed by rotary evaporation, the residue is dissolved in a small amount of deionized water, and the mixture is extracted three times with diethyl ether to remove unreacted terpinene-4-ol. The aqueous phase is then freeze-dried to obtain the modified prebiotic.

9. The anti-hair loss shampoo according to claim 8, characterized in that: The mass ratio of the oligofructose, terpinen-4-ol, and immobilized lipase is 10:2:

1.

10. A method for preparing an anti-hair loss shampoo as described in any one of claims 1 to 9, characterized in that: Includes the following steps: S1. Under stirring, propylene glycol and deionized water are mixed, and caffeine, nicotinamide and biotin are added in sequence. Stir until completely dissolved, then add saw palmetto fruit extract, rosemary extract and arborvitae leaf extract. Homogenize to fully disperse evenly and prepare an anti-hair loss active composition for later use. S2. Add sodium lauroyl methyl aminopropionate, cocamidopropyl betaine, and PEG-7 glyceryl cocoate to deionized water, heat to 75°C, stir until completely dissolved and transparent, and homogenize. S3. Cool to below 45°C, slowly add modified jojoba seed oil microspheres, modified silk fibroin nanofibers, modified prebiotics, glycerin, panthenol and preservatives and stir evenly. Then add the anti-hair loss active composition prepared in S1 and stir slowly for 15 minutes to ensure even distribution. S4. Add sodium chloride to adjust to a suitable viscosity, adjust the pH to 5.5-6.0 with citric acid, cool to below 35°C, add fragrance, and homogenize to obtain the anti-hair loss shampoo.

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