Scalp care composition for helping rapid growth of hair as well as preparation method and application of scalp care composition

Abstract

The invention belongs to the technical field of daily chemicals, and particularly relates to a scalp care composition for helping rapid growth of hair as well as a preparation method and application of the scalp care composition. The scalp care composition is prepared from the following components in parts by mass: 12 to 25 parts of recombinant XVII type collagen, 20 to 30 parts of glucosyl hesperidin, 25 to 42 parts of caffeine seed extract, 12 to 20 parts of troxerutin and 5 to 12 parts of PEG-5 (Polyethylene Glycol) ethylhexanoate. Through synergism of multiple components, a good effect of helping hair to grow rapidly is achieved through multiple aspects of promoting hair growth, enhancing transdermal absorption of active components, maintaining scalp steady state, resisting inflammation, relieving and providing nutrition for scalp and hair; comprehensively, breakthrough is realized in four aspects of transdermal delivery of active ingredients, hair growth regulation and control, scalp microenvironment repair and use safety.

Description

Technical Field

[0001] This invention belongs to the field of daily chemical products technology, specifically relating to a scalp care composition that helps hair grow quickly, its preparation method, and its application. Background Technology

[0002] The hair growth cycle is typically divided into the anagen (growth) phase, catagen (transitional) phase, and telogen (resting) phase. The growth and health of hair directly reflect the stability of the scalp's microenvironment, which is in dynamic equilibrium under healthy conditions. With the accelerated pace of modern life, increased mental stress, worsening environmental pollution, irregular sleep patterns, and genetic factors, the imbalance of the scalp's microenvironment is becoming increasingly prominent. Specific manifestations of this imbalance include slowed scalp blood circulation, insufficient nutrient supply to hair follicles, accumulation of inflammatory factors, increased oxidative stress, and collagen loss. These problems directly lead to an increased proportion of hair entering the telogen phase and a shortened anagen phase, resulting in thinning, fine, and slow-growing hair, as well as hair loss, affecting a person's appearance and, in severe cases, impacting mental health.

[0003] Currently, the market offers a wide variety of scalp care and hair growth products targeting the aforementioned hair health issues, with varying mechanisms of action and active ingredients. In terms of their mode of action, they mainly include topical application, oral supplements, and medical interventions. Among these, topical application products are the mainstream choice for consumers due to their convenience and relatively high safety profile. The core active ingredients in existing topical products mainly fall into the following categories: First, ingredients that promote blood circulation, such as minoxidil, which improves blood supply to hair follicles by dilating scalp blood vessels, but have side effects such as strong dependence and scalp irritation or hirsutism in some users; Second, ingredients that inhibit 5α-reductase, such as saw palmetto extract and pumpkin seed extract, which alleviate androgenetic alopecia by reducing the conversion of testosterone to dihydrotestosterone (DHT), but have a slow onset of action and limited effect when used alone; Third, anti-inflammatory and antioxidant ingredients, such as vitamin E and panthenol, which can improve scalp inflammation, but have a weak direct activating effect on hair follicle activity; Fourth, nutritional supplement ingredients, such as amino acids and biotin, which can provide raw materials for hair synthesis, but are difficult to penetrate the scalp barrier and be efficiently absorbed by hair follicles.

[0004] Chinese patent CN118221802A discloses a recombinant type XVII collagen for promoting hair growth, its preparation method, and its application. The recombinant type XVII collagen has a high serine content in its amino acid sequence, indicating a good hair growth promoting effect. However, this patent only utilizes one active ingredient, recombinant type XVII collagen, and its absorption effect is unknown. Although the protein itself has a good hair growth effect when well absorbed, its effectiveness in practical applications is uncertain. Furthermore, this patent does not explore multi-pathway synergistic effects; its mechanism is singular and cannot effectively care for overall scalp health. Chinese patent CN115054557A discloses an anti-hair loss composition and its application. The main active ingredients are camellia seed extract and small-fruited coffee seed extract, which have a strong synergistic effect in alleviating androgenetic alopecia. However, this patent only uses cell experiments for verification, and its absorption effect in practical applications is unknown. Moreover, this patent does not disclose the pathways used to promote the absorption of its active ingredients, nor does it explore multi-pathway synergistic effects. Furthermore, the caffeine in the small-fruit coffee seed extract has a certain degree of irritation. Without explaining how to alleviate its irritation, the irritation of the scalp by this patent is unknown.

[0005] As mentioned above, although existing scalp care products have made some progress in improving hair health, many shortcomings still exist. Therefore, developing a scalp care composition with multi-target synergistic effects, high safety, good permeability, and the ability to effectively activate hair follicle activity and promote rapid hair growth has become an urgent technical problem to be solved in the current scalp care field. Summary of the Invention

[0006] To address the problems of existing anti-hair loss products being highly irritating, slow-acting, having poor follicle activation, and poor absorption, the first aspect of this invention provides a scalp care composition that helps hair grow rapidly, specifically comprising the following ingredients: by weight, 12-25 parts recombinant type XVII collagen, 20-30 parts glucosyl hesperidin, 25-42 parts small-fruit coffee seed extract, 12-20 parts troxerutin, and 5-12 parts PEG-5 ethylhexanoate.

[0007] Type XVII collagen is a transmembrane protein located in the basement membrane region of the epidermis. Structurally, it is mainly divided into an intracellular region, a transmembrane structural region, and an extracellular region. Type XVII collagen can exist in vivo in transmembrane or shed form, thus possessing the dual functions of cell membrane surface receptors and extracellular matrix components. Type XVII collagen is also a component of hemidesmosomes in cells, playing an important role in the epithelial cell-basement membrane process, including regulating epithelial cell adhesion, migration, development, and differentiation; regulating keratinocyte differentiation and regeneration; and maintaining the homeostasis and differentiation of related stem cells in the skin. Coffee seed extract is rich in active substances such as chlorogenic acid, caffeine, and polyphenols. Caffeine has a bidirectional regulatory effect on vasoconstriction and vasodilation, which can increase the nutrient supply to hair follicles (such as oxygen, protein, vitamins, etc.), improve the "barren" state of hair follicles, provide sufficient nutrients to hair strands, and enhance hair strand toughness.

[0008] Glucosyl hesperidin is a water-soluble derivative of hesperidin, which has been chemically modified to incorporate a glucose group, thus improving its bioavailability. Existing data indicate that it has a positive effect on promoting blood circulation. Glucosyl hesperidin promotes blood circulation by improving vascular endothelial function, exhibiting antioxidant and anti-inflammatory effects, and enhancing capillary resilience.

[0009] Troxerutin is a natural flavonoid compound extracted from plants such as Sophora japonica buds. It is a hydroxyethyl ether derivative of rutin. In cosmetics, troxerutin is a multifunctional active ingredient, particularly adept at anti-oxidation, anti-inflammatory soothing, strengthening capillaries, and aiding in sun protection and repair. In terms of anti-oxidation, it can significantly eliminate reactive oxygen free radicals produced by cells, maintaining normal cell metabolism; its effect far surpasses that of vitamin E. In terms of anti-inflammatory soothing, it can inhibit microbial growth and play an anti-allergic role by disrupting the integrity of microbial cell membranes and cell walls, hindering the release of components from microbial cells, thereby affecting membrane electron transport, nutrient absorption, nucleotide synthesis, and ATP activity. In terms of enhancing capillary resilience, it can increase capillary resistance, reduce capillary permeability, and restore the elasticity of dilated capillaries, thus helping to inhibit the formation of redness.

[0010] The molecular structure of PEG-5 ethylhexanoate contains both hydrophilic polyethylene glycol chains and lipophilic ethylhexanoate groups, which can reduce interfacial tension in water-oil two-phase systems. PEG-5 ethylhexanoate can increase the concentration of poorly soluble active ingredients in hair products, helping to maintain system stability. The polyethylene glycol chains in PEG-5 ethylhexanoate can interact with the negatively charged groups (such as carboxyl groups) of hair keratin, neutralizing static electricity on the hair surface, reducing "flakes," lowering the coefficient of friction of the hair cuticle, and making the hair softer and smoother.

[0011] This invention utilizes a compound of recombinant type XVII collagen, glucosyl hesperidin, small-fruit coffee seed extract, troxerutin, and PEG-5 ethylhexanoate to achieve a synergistic effect across multiple components. It works by promoting hair growth, enhancing transdermal absorption of active ingredients, maintaining scalp homeostasis, providing anti-inflammatory and soothing effects, and nourishing the scalp and hair strands to promote rapid hair growth. Firstly, this invention abandons the traditional model of stimulating hair growth with a single component. Through the synergistic action of multiple components on key nodes in the hair follicle growth cycle, it significantly shortens the telogen phase and accelerates the hair growth process. Recombinant type XVII collagen, as a key transmembrane protein maintaining the stability of the scalp basement membrane structure, directly determines the scalp repair and hair growth support effects through its bioavailability. However, the transdermal absorption of large-molecule protein components has always been a technical challenge in the industry. This invention uses glucosyl hesperidin, coffee seed extract, troxerutin, and PEG-5 ethylhexanoate as auxiliary components in the composition, which can promote the transdermal absorption of recombinant type XVII collagen, strengthen the structural integrity of the basement membrane, establish a nutrient delivery channel from the dermis to the epidermis, provide a stable growth support environment for hair follicles, and improve scalp health from the root.

[0012] The glucosyl hesperidin, coffee seed extract, troxerutin, and PEG-5 ethylhexanoate used in this invention not only promote the absorption of recombinant type XVII collagen, but also play an important role in the hair growth process. Specifically, glucosyl hesperidin promotes scalp blood circulation and has antioxidant and anti-inflammatory effects; coffee seed extract is rich in chlorogenic acid, caffeine, and polyphenols, which promote the formation of capillaries around hair follicles, providing them with sufficient oxygen and nutrients, and driving the transformation of hair follicles from the telogen phase to the anagen phase; troxerutin exerts antioxidant, anti-inflammatory, and soothing effects, effectively reducing the toxic damage of inflammatory factors to hair follicles, preventing them from entering the pathological telogen phase, and reducing discomfort symptoms such as scalp redness and itching, providing a healthy environment free from inflammation for hair growth; PEG-5 ethylhexanoate, as a highly efficient emulsifier, enables the oil-phase active ingredients to form a stable and homogeneous emulsion structure with the aqueous phase system, promoting the transdermal absorption of the active ingredients and playing a key role in the effective delivery of active substances to the scalp. The combined effect of these five ingredients accelerates hair growth and maintains the health of the scalp and hair.

[0013] In some embodiments, the scalp care composition for promoting rapid hair growth comprises: 16.70 parts of recombinant type XVII collagen, 25.05 parts of glucosyl hesperidin, 33.40 parts of small-fruit coffee seed extract, 16.70 parts of troxerutin, and 8.15 parts of PEG-5 ethylhexanoate.

[0014] In some embodiments, the preparation method of the small-fruited coffee seed extract includes: S1. Mix coffee grounds and water to obtain a mixture; S2. The mixture is placed in a reaction vessel for extraction, and the extract is obtained after filtration. S3. The extract is dried to obtain small-fruit coffee seed extract.

[0015] In some embodiments, the coffee grounds powder in step S1 is the dried coffee grounds remaining after oil extraction.

[0016] In some embodiments, the particle size of the coffee grounds powder in step S1 is between 8 and 15 μm.

[0017] In some embodiments, the mass ratio of coffee grounds in step S1 to water in step S1 is 1:(6-12).

[0018] In some embodiments, the extraction in step S2 is subcritical extraction, wherein the temperature of the subcritical extraction is 160–200°C, the pressure is 3–5 MPa, and the extraction time is 60–120 min.

[0019] In some embodiments, the drying is spray drying, wherein the inlet air temperature of the spray drying is 100-120°C and the outlet air temperature is 50-70°C.

[0020] In some embodiments, the molecular weight of the recombinant type XVII collagen is 22kDa to 25kDa.

[0021] In a second aspect, the present invention provides a serum comprising the above-mentioned scalp care composition for promoting rapid hair growth.

[0022] In some embodiments, the serum comprises: 0.5–10% of the scalp care composition that promotes rapid hair growth, 8–13% butylene glycol, 0.01–0.1% adenosine, 0.2–1.0% 9010, 0.2–1.5% UKfinecare® D68, 0.05–0.5% tridecyl alcohol polyether-9, 0.001–0.01% hydroxyphenylpropionamide benzoic acid, and the balance being water.

[0023] In some embodiments, the serum comprises: 1.2% scalp care composition, 10% butylene glycol, 0.05% adenosine, 0.5% 9010, 0.5% UKfinecare® D68, 0.1575% tridecyl alcohol polyether-9, 0.0045% hydroxyphenylpropionamide benzoic acid, and the balance being water.

[0024] Thirdly, the present invention provides a method for preparing the serum, comprising: A1. Add butanediol, adenosine, 9010, UKfinecare® D68, tridecyl alcohol polyether-9 and hydroxyphenyl propionamide benzoic acid to water, heat, and stir until homogeneous to obtain mixture 1; A2. Cool down, add the scalp care composition that helps hair grow quickly to the mixture 1, and stir evenly to obtain the essence.

[0025] In some embodiments, the heating in step A1 is heating to 80-85°C.

[0026] In some embodiments, the cooling in step A2 is to cool down to 35-45°C.

[0027] Fourthly, the present invention provides the use of the above-mentioned scalp care composition that promotes rapid hair growth in the preparation of daily chemical products.

[0028] The daily chemical products described in this invention are any formulations conventionally prepared in the field of hair care products, and can be formulated into, for example, solutions, suspensions, emulsions, pastes, gels, creams, water, powders, soaps, surfactant-containing detergents, oils, creams, and sprays.

[0029] Preferably, the daily chemical product of the present invention is at least one of hair conditioner, hair nourishing cream, hair massage cream, hair essence, hair cleansing cream, hair cleansing foam, hair cleanser, hair moisturizing cream, shampoo, and conditioner.

[0030] Compared with the prior art, the present invention has the following beneficial effects: (1) This invention scientifically combines five active ingredients—recombinant type XVII collagen, glucosyl hesperidin, small-fruit coffee seed extract, troxerutin, and PEG-5 ethylhexanoate—to form a synergistic system, abandoning the traditional model of stimulating hair growth with a single ingredient. The multi-component synergistic action targets key nodes in the hair follicle growth cycle, significantly shortening the hair growth resting phase and accelerating the hair growth process. This overcomes the technical bottlenecks of existing technologies, such as low utilization rate of active ingredients, single target, and difficulty in balancing safety and efficacy. This invention achieves breakthroughs in transdermal delivery of active ingredients, hair growth regulation, scalp microenvironment repair, and safety of use.

[0031] (2) This invention utilizes the dried coffee grounds remaining after oil extraction to prepare small-fruit coffee seed extract, significantly reducing the production cost of the extract. In addition, the reuse of the dried coffee grounds remaining after oil extraction helps reduce the pressure of waste disposal, and has outstanding environmental benefits.

[0032] (3) This invention has passed the eye irritation test, is highly safe, mild and non-irritating, suitable for a wide range of people, expands the application scenarios, is easy to promote, and has high market value. Attached Figure Description

[0033] Figure 1 The fluorescence spectrum of the control group in the transdermal absorption test after 8 hours; Figure 2 The fluorescence spectrum of Example 2 after 8 hours in the transdermal absorption test; Figure 3 The hair growth on the back of mice in the saline group during the mouse hair growth test (day 15). Figure 4 Hair growth on the back of mice in the minoxidil group during a mouse hair growth test (day 15). Figure 5 The hair growth on the back of mice in the matrix essence group during the mouse hair growth test (day 15). Figure 6 The hair growth on the back of mice in Example 8 (day 15) in the mouse hair growth test. Figure 7 The hair growth on the back of mice in Example 9 (day 15) in the mouse hair growth test. Figure 8 The hair growth on the back of mice in Example 10 (day 15) in the mouse hair growth test. Figure 9 The hair growth on the back of mice in Example 11 group during the mouse hair growth test (day 15). Figure 10 The hair growth on the back of mice in Example 12 group during the mouse hair growth test (day 15). Figure 11 This is an example of hair growth on the back of a mouse during a hair growth test. Figure 11 A indicates a mild case. Figure 11 B is moderate. Figure 11 C indicates severe. Detailed Implementation

[0034] The technical solutions of the present invention are described in detail below with reference to embodiments. These embodiments are merely illustrative of the present invention to those skilled in the art, and are not intended to limit the technical solutions of the present invention. Simple modifications or equivalent substitutions made to the technical solutions of the embodiments of the present invention without departing from the basic concept of the present invention still fall within the protection scope of the present invention.

[0035] Unless otherwise specified, all experimental methods described below are conventional methods. All materials and reagents mentioned below are commercially available unless otherwise specified. Unless otherwise specified, all percentages mentioned in this invention are mass percentages.

[0036] The recombinant type XVII collagen, recombinant type III collagen, and recombinant type I collagen used in this invention are derived from Jiangsu Chuangjian Medical Technology Co., Ltd.

[0037] The 9010 used in this invention is from Ashland (China) Investment Co., Ltd.

[0038] The UKfinecare® D68 used in this invention is sourced from Nanjing Urban Agriculture Technology Development Co., Ltd.

[0039] The minoxidil tincture used in the comparative or control groups of this invention is a commercially available product, branded as Faji, and sourced from Xiamen Meishang Pharmaceutical Co., Ltd.

[0040] The coffee grounds powder involved in the embodiments and comparative examples of this invention is prepared from raw Arabica coffee beans.

[0041] The mice used in this invention are all 7-week-old female C57 mice.

[0042] Examples 1-7: A scalp care composition to promote rapid hair growth The components and their contents in Examples 1 to 7 are shown in Table 1.

[0043] Table 1. Information on components and their contents in Examples 1-7

[0044] in, The preparation methods of the small-fruit coffee seed extracts in Examples 1-5 specifically include the following steps: S1. Mix coffee grounds powder with a particle size of 10μm with 9 times its weight of water to obtain a mixture; S2. Place the mixture in a reaction vessel and perform subcritical extraction at a temperature of 180℃ and a pressure of 4 MPa for 90 min. After filtration, the extract is obtained. S3. Spray dry the extract (conditions: inlet air temperature 110℃, outlet air temperature 60℃) to obtain small-fruit coffee seed extract.

[0045] The preparation method of the small-fruit coffee seed extract in Example 6 specifically includes the following steps: S1. Mix coffee grounds powder with a particle size of 8μm with 6 times the mass of water to obtain a mixture; S2. Place the mixture in a reaction vessel and perform subcritical extraction at a temperature of 160℃ and a pressure of 3 MPa for 60 min. After filtration, the extract is obtained. S3. Spray dry the extract (conditions: inlet air temperature 120℃, outlet air temperature 70℃) to obtain small-fruit coffee seed extract.

[0046] The preparation method of the small-fruit coffee seed extract in Example 7 specifically includes the following steps: S1. Mix coffee grounds powder with a particle size of 15μm and 12 times the mass of water to obtain a mixture; S2. Place the mixture in a reaction vessel and perform subcritical extraction at a temperature of 200℃ and a pressure of 5 MPa for 120 min. After filtration, the extract is obtained. S3. Spray dry the extract (conditions: inlet air temperature 100℃, outlet air temperature 50℃) to obtain small-fruit coffee seed extract.

[0047] Comparative Examples 1-5: A scalp care composition to promote rapid hair growth The components and their contents in Comparative Examples 1–5 are shown in Table 2.

[0048] Table 2. Components and contents of Comparative Examples 1–5

[0049] The preparation methods of the small-fruit coffee seed extracts in Comparative Examples 1-5 are the same as those in Example 2.

[0050] The preparation methods of the compositions in Comparative Examples 1 to 5 are the same as those in Example 2.

[0051] Comparative Example 6: A scalp care composition to promote rapid hair growth The process is basically the same as in Example 2, except that in Comparative Example 6, recombinant type XVII collagen is replaced with recombinant type III collagen. The remaining steps and parameters are the same as in Example 2.

[0052] Comparative Example 7: A scalp care composition to promote rapid hair growth The process is basically the same as in Example 2, except that in Comparative Example 7, recombinant type XVII collagen is replaced with recombinant type I collagen. The remaining steps and parameters are the same as in Example 2.

[0053] Comparative Example 8: A scalp care composition to promote rapid hair growth The process is basically the same as in Example 2, except that in Comparative Example 8, glucosyl hesperidin is replaced with biotin. The rest of the steps and parameters are the same as in Example 2.

[0054] Comparative Example 9: A scalp care composition to promote rapid hair growth The process is basically the same as in Example 2, except that in Comparative Example 9, the small-fruit coffee seed extract is replaced with caffeine. The remaining steps and parameters are the same as in Example 2.

[0055] Comparative Example 10: A scalp care composition to promote rapid hair growth The process is basically the same as in Example 2, except that in Comparative Example 10, the small-fruit coffee seed extract is replaced with chlorogenic acid. The rest of the steps and parameters are the same as in Example 2.

[0056] Comparative Example 11: A scalp care composition to promote rapid hair growth It is basically the same as Example 2, except that the preparation method of the small-fruit coffee seed extract in Comparative Example 11 is different. The rest of the steps and parameters are the same as those in Example 2.

[0057] The preparation method of the small-fruit coffee seed extract of Comparative Example 11 includes: S1. Place raw Arabica coffee beans (green) in a freeze dryer and freeze dry at -50°C for 24 hours. After drying, grind them with a grinder and sieve them. The lower layer of powder is the coffee powder used in this invention.

[0058] S2. Add 10 times the mass of butanediol solution (30wt%) to coffee powder, mix well, and then extract by ultrasonication at 60℃ for 60 min. After filtration, obtain residue and filtrate 1. S3. Add 10 times the mass of deionized water and 0.5% of the mass of cellulase and pectinase (mass ratio of cellulase to pectinase is 1:1) to the filter residue. Enzymatically hydrolyze at 50℃ for 3 hours, then inactivate at 80℃ for 20 minutes. After filtration, obtain filtrate 2. S4. Mix filtrate 1 and filtrate 2 and sterilize at 85°C for 25 minutes to obtain coffee extract.

[0059] Comparative Example 12: A scalp care composition to promote rapid hair growth The process is basically the same as in Example 2, except that in Comparative Example 12, troxerutin is replaced with rutin, and the rest of the steps and parameters are the same as in Example 2.

[0060] Comparative Example 13: A scalp care composition to promote rapid hair growth The process is basically the same as in Example 2, except that in Comparative Example 13, troxerutin is replaced with panthenol. The rest of the steps and parameters are the same as in Example 2.

[0061] Comparative Example 14: A scalp care composition to promote rapid hair growth The process is basically the same as in Example 2, except that in Comparative Example 14, PEG-5 ethylhexanoate is replaced with PEG-5 glyceryl stearate. The remaining steps and parameters are the same as in Example 2.

[0062] Examples 8-12: A serum containing the aforementioned scalp care composition that promotes rapid hair growth. The components and contents of Examples 8 to 12 are shown in Table 3.

[0063] Table 3. Component and content information for Examples 8-12

[0064] in: The preparation method of the serum in Examples 8-10 specifically includes the following steps: (1) Butylene glycol, adenosine, 9010, UKfinecare® D68, tridecyl alcohol polyether-9 and hydroxyphenyl propionamide benzoic acid were added to water, heated to 83°C and stirred until homogeneous to obtain mixture 1; (2) Cool down to 40°C, add a scalp care composition that helps hair grow quickly to the mixture 1, stir well to obtain the essence.

[0065] The preparation method of the serum in Example 11 specifically includes the following steps: (1) Butylene glycol, adenosine, 9010, UKfinecare® D68, tridecyl alcohol polyether-9 and hydroxyphenyl propionamide benzoic acid were added to water, heated to 85°C and stirred until homogeneous to obtain mixture 1; (2) Cool down to 45°C, add a scalp care composition that helps hair grow quickly to the mixture 1, stir well to obtain the essence.

[0066] The preparation method of the serum in Example 12 specifically includes the following steps: (1) Butylene glycol, adenosine, 9010, UKfinecare® D68, tridecyl alcohol polyether-9 and hydroxyphenyl propionamide benzoic acid were added to water, heated to 80°C and stirred until homogeneous to obtain mixture 1; (2) Cool down to 35°C, add a scalp care composition that helps hair grow quickly to the mixture 1, stir well to obtain the essence.

[0067] Experimental Example 1: Transdermal Absorption Test (1) Sample The experimental group consisted of compositions prepared from fluorescently labeled recombinant type XVII collagen in Examples 1-7, Comparative Examples 1-5, and 8-14, as well as compositions prepared from fluorescently labeled recombinant type III collagen in Comparative Example 6 and compositions prepared from fluorescently labeled recombinant type I collagen in Comparative Example 7. The control group consisted of fluorescently labeled recombinant type XVII collagen at the same concentration as the fluorescently labeled recombinant type XVII collagen in Example 2.

[0068] (2) Method ① Preparation of fluorescently labeled recombinant type XVII collagen: Weigh Cy5-COOH (52 mg) and dissolve it in phosphate buffer solution (0.1 mol / L) at pH=5.5. Add EDC (22 mg) and NHS (16 mg) at 0℃. After reacting for 2 h, add 0.5 g of human recombinant type XVII collagen and react for 12 h. Then remove unreacted Cy5-COOH and byproducts by dialysis. After freeze-drying, obtain fluorescently labeled recombinant type XVII collagen.

[0069] ② Preparation of compositions of fluorescently labeled recombinant type XVII collagen in examples and comparative examples: The compositions of each example and comparative example were prepared by fluorescently labeled recombinant type XVII collagen according to the methods in the above examples and comparative examples.

[0070] ③ Use the composition obtained in step ② to prepare an essence for transdermal absorption experiments. The formula is shown in Table 4.

[0071] Table 4. Information on the ingredients and content of the serum used in the transdermal absorption experiment.

[0072] Using the fluorescently labeled composition or recombinant type XVII collagen (control group) as the research subjects, serums for transdermal absorption experiments were prepared according to Table 4. The amount of recombinant type XVII collagen added to the control group was 0.835 wt% (not 5%), ensuring that the amount of recombinant type XVII collagen added to the control group was consistent with the corresponding concentration of recombinant type XVII collagen in the serum in Example 2. Live C57 mice were used as research subjects. Different samples were applied to the mouse skin, with 6 mice in each group. After 8 hours, the mice were euthanized by cervical dislocation, and approximately 0.5 cm of the central area of ​​the applied sample was excised. 0.5cm skin tissue was rinsed with PBS solution, the surface moisture was blotted dry with filter paper, and the tissue was flash-frozen in liquid nitrogen for 15 seconds and then stored overnight at -80℃. After OCT embedding (Optimal Cutting Temperature Compound), the tissue was frozen and sectioned, stained with DAPI, mounted, and photographed.

[0073] ④ Statistical analysis of fluorescence intensity.

[0074] (3) Results The test results are shown in Table 5. The fluorescence imaging results of the control group are shown in Table 5. Figure 1 The fluorescence imaging results of Example 2 are as follows: Figure 2The results showed that the scalp care compositions of Examples 1-7 of the present invention had better transdermal absorption performance. This indicates that the combined use of glucosyl hesperidin, small-fruit coffee seed extract, troxerutin, and PEG-5 ethylhexanoate in the present invention improved the transdermal absorption performance of recombinant type XVII collagen and enhanced its efficacy in scalp care. Comparative Examples 1-4 lacked glucosyl hesperidin, small-fruit coffee seed extract, troxerutin, and PEG-5 ethylhexanoate, respectively, resulting in significantly poorer transdermal absorption. Comparative Examples 8-14 replaced glucosyl hesperidin, small-fruit coffee seed extract, troxerutin, and PEG-5 ethylhexanoate with analogues, or changed the preparation method of small-fruit coffee seed extract, respectively, and their transdermal absorption performance also decreased. These differences all indicate that the combined use of glucosyl hesperidin, small-fruit coffee seed extract, troxerutin, and PEG-5 ethylhexanoate can effectively promote the transdermal absorption of recombinant type XVII collagen. Although glucosyl hesperidin, coffee seed extract, and troxerutin do not individually enhance penetration, the penetration-enhancing effect of PEG-5 ethylhexanoate strengthens the absorption of troxerutin, coffee seed extract, and glucosyl hesperidin. Troxerutin and glucosyl hesperidin synergistically improve subcutaneous microcirculation and capillary health in the scalp, ensuring efficient absorption and utilization of the composition's ingredients. At the same time, both synergistically improve skin blood circulation with coffee seed extract, further enhancing the absorption effect of the composition and forming a stable virtuous cycle.

[0075] Table 5. Fluorescence intensity detection results of Examples 1-7, Comparative Examples 1-4, and Comparative Examples 8-14

[0076] Experimental Example 2: Eye Irritation Test (1) Sample The compositions of Examples 1-7 and Comparative Examples 1-14 were prepared into scalp care compositions with a mass concentration of 10% using physiological saline.

[0077] (2) Method ①Standard: This test protocol is based on the standard SN / T 2329-2009 "Test on Chicken Embryo Villi Allantoic Membrane for Irritation and Corrosivity of Cosmetics".

[0078] ②Steps: Incubate the eggs for the experiment in an incubator until day 9. Mark the air cell location of the eggs with a pencil, and observe whether the embryos are developing well and whether the blood vessels are growing normally. Determine the number of eggs that can be used for testing and allocate the eggs needed for the test samples. For the experiment, use 3 embryos per sample. Along the marked air cell, use a tool to remove the marked eggshell part. Add physiological saline with a pipette to moisten the egg membrane, pour out the physiological saline, and remove the inner membrane with tweezers, ensuring that the blood vessels are not damaged. Observe the embryos for obvious bleeding or turbidity, and if there is no obvious bleeding or turbidity, it can be judged as suitable for the experiment. The reaction time method is used for the experiment. Use a pipette to add 300μL of scalp care composition to the chorioallantoic membrane (CAM membrane), start timing, and take a picture to record the state at the beginning of sample addition. Observe the changes in blood vessels within the circle. When bleeding, hemolysis, coagulation, or other changes occur, record the time and take a picture to record the state of the embryo. After 5 minutes of sample addition, take a picture to record the state of the embryo and end the observation.

[0079] ③ Data analysis: The reaction time method was used for the experiment, and the irritation score (IS) was calculated according to the following formula.

[0080]

[0081] In the formula: H is the average time for the onset of bleeding observed on the CAM membrane; L is the average time for the onset of vascular lysis observed on the CAM membrane; C is the average time for the onset of coagulation observed on the CAM membrane; the unit is seconds (s).

[0082] The test samples were classified according to the values ​​in Table 6 to determine their eye irritation.

[0083] Table 6. Eye Irritation Assessment Criteria

[0084] (3) Results The test results are shown in Table 7. The results show that the scalp repair compositions prepared using the compositions of Examples 1-7 of this invention are all non-irritating at a concentration of 10 wt%, proving that Examples 1-7 of this invention have high safety and fully meet the standards for raw materials used in daily chemical products. Comparative Examples 1-14 mostly showed no irritation, but in Comparative Example 9, replacing the small-fruit coffee seed extract in the composition with caffeine, and in Comparative Example 14, replacing PEG-5 ethylhexanoate with PEG-5 glyceryl stearate, the irritation significantly increased. This is because the small-fruit coffee seed extract prepared by this invention also contains chlorogenic acid, polyphenols, and other water-soluble natural anti-inflammatory agents, which can alleviate the local scalp inflammation caused by caffeine itself and balance the irritation of caffeine. After replacement, single caffeine is more likely to irritate the scalp. The increased irritation in Comparative Example 14 after replacement with PEG-5 glyceryl stearate is due to the inherent properties of the substances themselves; each component has different irritation levels, and the synergistic effects of the components in the composition differ, resulting in different levels of irritation. The synergistic effect between the compositions changes; the combination of PEG-5 glyceryl stearate with recombinant type XVII collagen, glucosyl hesperidin, small-fruit coffee seed extract, and troxerutin is more irritating than the use of PEG-5 ethylhexanoate.

[0085] Table 7. Results of Irritation Assessment for Examples 1-7 and Comparative Examples 1-14

[0086] Experimental Example 3: Scalp Repair Performance Test (1) Principle IL-17 is a pro-inflammatory cytokine primarily produced by the TH17 subset of T helper cells. Overexpressed IL-17 can disrupt the scalp barrier through multiple mechanisms, becoming a core driver of scalp inflammation. For example, IL-17 binds to the IL-17 receptor (IL-17R) on the surface of keratinocytes (KCs), initiating downstream inflammatory signaling pathways (such as NF-κB and MAPK), triggering a series of pro-inflammatory responses that directly or indirectly damage the scalp barrier. IL-17A stimulates excessive KC proliferation, inhibiting normal differentiation, leading to parakeratosis and acanthosis, thus disrupting the physical structural integrity of the barrier. Reduced IL-17 gene expression decreases IL-17 protein secretion, thereby alleviating its destructive effect on the scalp barrier. In this experiment, we obtained cell supernatants containing endogenously expressed inflammatory factors from mouse macrophage Raw264.7 cells. These cell supernatants were used to induce human dermal papilla cells (HDPCs) as an in vitro inflammatory cell model to simulate the inflammatory effects of inflammatory factors on the skin / scalp. The efficacy of test samples in repairing the scalp was evaluated by measuring the relative expression levels of inflammatory factor (IL-17) mRNA.

[0087] (2) Sample Test samples: The compositions of Examples 1-7 and Comparative Examples 1-14 were prepared into 1% solutions by mass concentration using DMEM culture medium containing 10% FBS and 1% double antibiotics.

[0088] Stimulants: Cell supernatant containing endogenously expressed inflammatory factors obtained from the culture of mouse macrophages Raw264.7 was used as the stimulant for the in vitro inflammatory cell model.

[0089] (3) Method ① Preparation of stimulants: Raw264.7 mouse macrophage cell suspension was seeded into 6-well cell culture plates and cultured for 18–24 h. The original culture medium was then replaced with medium containing 5 μg / mL LPS. LPS stimulates Raw264.7 cells to produce inflammatory factors. After 6 h of culture, the culture plates were removed, and the cells were broken up by pipetting. The liquid was transferred to centrifuge tubes and centrifuged (8000 rpm, 10 min). The supernatant was collected as the lysis buffer. The supernatant was dissolved in DMEM medium containing 10% FBS and 1% penicillin-dextrin to prepare a 10% (w / w) solution.

[0090] ② Stimulation Test: Human dermal papilla cell suspension was seeded into 6-well cell culture plates and cultured in DMEM medium containing 10% FBS and 1% penicillin antibody at 37°C and 5% CO2 for 24 hours. After culture, the culture medium was discarded. The test sample group and model control group were cultured in medium containing 10% lysis buffer as a stimulant, while the negative control group was cultured in DMEM medium containing 10% FBS and 1% penicillin antibody. After 4 hours of culture, the medium was replaced with DMEM medium containing 10% FBS and 1% penicillin antibody. After another 24 hours of culture, RNA was extracted from each group of cells (RNA extraction kit purchased from Beijing Lanjieke Technology Co., Ltd.), reverse transcribed into cDNA (reverse transcription kit purchased from Beijing Lanjieke Technology Co., Ltd.), and stored at -80°C. Finally, the expression level of IL-17 was determined by quantitative real-time PCR (quantitative real-time PCR kit purchased from Beijing Lanjieke Technology Co., Ltd.). Each group was repeated in triplicate, and the average value of the results was taken.

[0091] The forward primer sequence for the real-time PCR used to detect IL-17 is 5'-TAATGGCCCTGAGGAATGGC-3'. The reverse primer sequence is: 5'-AGGAAGCCTGAGTCTAGGGG-3'.

[0092] (4) Results The test results are shown in Table 8. The results indicate that the relative expression level of IL-17 mRNA in human dermal papilla cells increased sharply after stimulation. After adding the test sample, compared with the model control group, the IL-17 gene expression in Examples 1-7 and Comparative Examples 1-14 was reduced. Among them, the scalp repair effect of Examples 1-7 was significantly better than that of Comparative Examples 1-5, indicating that the compositions of Examples 1-7 of this invention can better inhibit the overexpression of IL-17 pro-inflammatory factors, resulting in superior scalp repair efficacy. This proves that the combined use of the five components of this invention—recombinant type XVII collagen, glucosyl hesperidin, small-fruit coffee seed extract, troxerutin, and PEG-5 ethylhexanoate—results in a stronger synergistic effect and better scalp repair efficacy. The absence of any one of these components worsens the scalp repair effect of the composition.

[0093] The scalp repair effects of Examples 1-7 were also better than those of Comparative Examples 6-14, further demonstrating that even if recombinant type XVII collagen, glucosyl hesperidin, coffee seed extract, troxerutin, and PEG-5 ethylhexanoate were replaced with similar components, or if the preparation method of coffee seed extract was changed, the changes in components would affect the synergistic effect between different components and thus affect the scalp repair effect of the final product.

[0094] Table 8. Results of relative IL-17 gene expression levels in Examples 1-7 and Comparative Examples 1-14

[0095] Experiment 4: Mouse Hair Growth Test (1) Sample Experimental group: The serum and base serum of Examples 8-12 (by mass percentage, composed of 10% butylene glycol, 0.05% adenosine, 0.5% 9010, 0.5% UKfinecare® D68, 0.1575% tridecyl alcohol polyether-9, 0.0045% hydroxyphenyl propionamide benzoic acid, and water to 100.00%).

[0096] Positive control group: commercially available minoxidil solution (concentration 5%).

[0097] (2) Method: ① Experimental subjects and period: The mice used were 7-week-old C57 mice (at this time, the mice's hair is in the resting phase and will remain in the resting phase for a long time without stimulation and will not enter the growth phase), 4 mice in each group, and the test period was 15 days.

[0098] ② Administration method and dosage: The essence, matrix essence, physiological saline and minoxidil tincture of Examples 8 to 12 are administered by applying to the skin on the back, with a single dose of 0.3 mL.

[0099] ③ Dosage frequency: All samples were administered daily, once a day.

[0100] ④ Observation indicators: After 0 days from the start of the experiment, the mice did not lose hair. After the drug was administered, the color change of the back was continuously observed and the phenomenon of entering the growth phase was observed and recorded continuously. After 7 days from the start of the experiment, the mice lost hair. After that, the drug was administered again to observe whether the hair on the back of the mice entered the growth phase, the area of ​​the hair entering the growth phase, and the speed at which the hair on the back of the mice entered the growth phase.

[0101] ⑤ The final experimental results were evaluated using a scoring method based on the hair growth on the backs of the mice, as shown in Table 9. Each test sample consisted of 4 mice, and the test score was the average of the 4 mice.

[0102] Table 9. Criteria for Judging Hair Growth on the Back of Mice

[0103] (3) Results The test results are shown in the table below. The results of hair growth on the backs of mice in the saline group are as follows: Figure 3 The results of hair growth on the backs of mice in the minoxidil tincture group were as follows: Figure 4 The results of hair growth on the backs of mice in the matrix essence group were as follows: Figure 5 The results of hair growth on the backs of mice in Examples 8-12 are shown in the following figures. Figures 6-10 Test results show that the serum containing the scalp repair composition of the present invention has a stronger effect on promoting hair growth. The composition of the present invention can effectively help hair growth. Using only saline solution or only the base serum resulted in poor hair growth in mice. Comparing the results of Examples 8-11, it is clear that, under the same dosage conditions, Example 2 showed a better effect in promoting hair growth.

[0104] Table 10 Results of hair growth scores on the backs of mice in Examples 8-12 and the control group

[0105] In summary, the scalp care composition provided by this invention, through the rational combination of 12-25 parts recombinant type XVII collagen, 20-30 parts glucosyl hesperidin, 25-42 parts small-fruit coffee seed extract, 12-20 parts troxerutin, and 5-12 parts PEG-5 ethylhexanoate, effectively enhances the transdermal absorption capacity of the scalp care composition through the synergistic effect of multiple components; it has low irritation, wide applicability, and is suitable for sensitive individuals; it has excellent hair growth promotion ability, can significantly increase hair growth rate, and simultaneously promotes scalp homeostasis and maintains hair health through multiple mechanisms.

Claims

1. A scalp care composition to help hair grow quickly, characterized in that, By mass parts, including 12-25 parts of recombinant collagen type XVII, 20-30 parts of glucosyl hesperidin, 25-42 parts of coffee cherries extract, 12-20 parts of troxerutin, 5-12 parts of PEG-5 ethylhexanoate.

2. A scalp care composition according to claim 1 characterised in that, The coffee cherries extract is prepared by the following steps: S1, mixing coffee residue powder and water to obtain a mixture; S2, placing the mixture in a reaction kettle for extraction, and obtaining an extract after filtration; S3, drying the extract to obtain the coffee cherries extract.

3. A scalp care composition according to claim 2 characterised in that, The coffee residue powder in step S1 is dry coffee residue left after oil extraction; the particle size of the coffee residue powder in step S1 is between 8-15 μm; the mass ratio of the coffee residue powder in step S1 to water in step S1 is 1: (6-12) ; The extraction in step S2 is subcritical extraction; the temperature of the subcritical extraction is 160-200 ℃, the pressure is 3-5 MPa, and the extraction time is 60-120 min; The drying in step S3 is spray drying, and the inlet air temperature of the spray drying is 100-120 ℃, and the outlet air temperature is 50-70 ℃.

4. The scalp care composition according to claim 1, characterized in that, The molecular weight of the recombinant collagen type XVII is 22 kDa-25 kDa.

5. A serum comprising the scalp care composition according to any one of claims 1 to 4, characterized in that, By mass percentage, containing 0.5-10% of the scalp care composition for helping hair grow fast, 8-13% of butylene glycol, 0.01-0.1% of adenosine, 0.2-1.0% of 9010, 0.2-1.5% of UKfinecare® D68, 0.05-0.5% of tridecane alcohol polyether-9, 0.001-0.01% of hydroxyphenylpropanamide benzoic acid, and the balance of water.

6. A method of preparing the serum according to claim 5, characterized in that, Specifically comprising the following steps: A1, adding butylene glycol, adenosine, 9010, UKfinecare® D68, tridecane alcohol polyether-9, and hydroxyphenylpropanamide benzoic acid to water, heating, and stirring to obtain a mixture 1; A2, cooling, adding the scalp care composition for helping hair grow fast to the mixture 1 in step A1, and stirring to obtain the serum.

7. The method of claim 6, wherein The heating in step A1 is heating to 80-85 ℃; the cooling in step A2 is cooling to 35-45 ℃.

8. Use of the scalp care composition according to any one of claims 1-4 in the preparation of a daily chemical.

9. Use according to claim 8, characterized in that, The daily chemical is any one of a solution, a suspension, an emulsion, a paste, a gel, a cream, water, a powder, a soap, a surfactant-containing cleaner, an oil, a powder cream, a spray.

10. Use according to claim 8, characterized in that, The daily chemical is at least one of a hair conditioner, a hair nourishing cream, a hair massage cream, a hair essence, a hair cleanser, a hair foam, a hair water, a hair moisturizing cream, a shampoo, and a hair conditioner. The daily chemical is at least one of a hair conditioner, a hair nourishing cream, a hair massage cream, a hair essence, a hair cleanser, a hair foam, a hair water, a hair moisturizing cream, a shampoo, and a hair conditioner.

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