A complex composition having a scalp care effect and use thereof

Abstract

The application discloses a composite composition with a scalp care effect and application thereof, and the composite composition is composed of cypress leaf extract, yucca extract, lagenaria siceraria roem extract and sargassum pallidum extract. A preparation process thereof is prepared through composite enzymolysis, ultrasonic extraction and high-pressure homogenization treatment, so that excellent stability and permeability are ensured. The composite composition provided by the application effectively solves problems of difficult penetration of active ingredients, promotion of hair follicle growth and the like, and is suitable for development of hair products such as shampoo, hair conditioner, hair growth liquid and scalp essence.

Description

Technical Field

[0001] This invention relates to the field of hair care products, and more particularly to a composite composition with scalp care function and its application. Background Technology

[0002] Developing all-natural plant-based hair growth and care products is an important direction in current technological research. Extracts from plants such as arborvitae leaves, yucca, and Sargassum fusiforme, rich in quercetin, saponins, and seaweed polysaccharides, show promising application potential in oil control, hair growth, and hair follicle repair. Arborvitae leaves, the dried tender branches and leaves of the arborvitae plant (Platycladus orientalis), are a traditional Chinese medicine. They are cold in nature, bitter and astringent in taste, and enter the lung, liver, and spleen meridians. Their main functions are cooling the blood and stopping bleeding, resolving phlegm and relieving cough, and promoting hair growth and darkening hair. They are commonly used to treat hematemesis, epistaxis, hemoptysis, hematochezia, alopecia due to blood heat, and premature graying of hair. Modern research shows that they have anti-inflammatory, antibacterial, and scalp-circulating effects. Yucca (scientific name: Yucca) is an evergreen plant of the genus Yucca in the family Asparagaceae (formerly Liliaceae), and has shown significant medicinal potential in both traditional medicine and modern research. Its main active ingredients include saponins and various polyphenolic compounds; Sargassum muticum, a widely distributed large brown seaweed, is rich in polyphenols (such as tannins), fucoxanthin, and vitamins C, E, and K. These ingredients can scavenge free radicals, reduce cellular oxidative stress, and help prevent chronic diseases. Sargassum muticum extract is frequently found in modern skincare product ingredient lists; it can promote hyaluronic acid production, enhance the skin barrier's water-retention capacity, and as a skin conditioner, help soothe environmental damage and improve skin texture. In addition, Luffa Cylindrica Fruit / Stem Extract, due to its gentle yet highly effective properties, is known as "Heavenly Water" or "Beauty Water," possessing natural anti-inflammatory properties that can effectively relieve sunburn redness, allergic itching, or skin instability during seasonal changes.

[0003] However, in practical applications, the aforementioned natural extracts still face the following technical bottlenecks: traditional extracts often exist in the form of large molecules or disordered fragments. Due to the barrier effect of the skin, the active ingredients have difficulty penetrating the epidermis and reaching the deep hair follicles, resulting in low bioavailability. In addition, the active ingredients in the extract (such as quercetin) are easily oxidized and degraded by the environment, and precipitation and aggregation are prone to occur when multiple extracts are mixed, affecting the product's sensory properties and efficacy. High concentrations of plant extracts often lead to dryness and roughness in the hair after use, lacking ideal smoothness and repair, and it is difficult to form an effective physical protective film on the hair surface. Therefore, how to construct a delivery system that is highly stable, has strong penetrability, and combines deep hair follicle repair with surface smoothness is a pressing problem to be solved in the field of scalp care. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art and provide a composition and hair product that has a hair-protecting and repairing effect.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is as follows: In a first aspect, the present invention provides a composite composition with scalp care function, comprising, by weight, the following components: 15-35 parts of Platycladus orientalis leaf extract, 10-25 parts of Yucca extract, 10-20 parts of Luffa extract, and 5-15 parts of Sargassum extract; wherein the composition contains a nanomicelle encapsulation structure formed by the self-assembly of Yucca saponins and Sargassum polysaccharides through hydrogen bonds, and the average particle size of the nanomicelles is 100-300 nm.

[0006] Furthermore, HPLC analysis showed that the mass fraction of quercetin in the Platycladus orientalis leaf extract of this invention was ≥1.5%.

[0007] Secondly, the present invention provides a method for preparing a composite composition, characterized by comprising the following steps: (1) Pretreatment: Prepare extracts of Platycladus orientalis leaf, Yucca florida, Luffa cylindrica and Sargassum fusiforme, dissolve them in water respectively to prepare extracts of Platycladus orientalis leaf, Yucca florida, Luffa cylindrica and Sargassum fusiforme. (2) Compound enzymatic hydrolysis: Mix the loofah extract and the Sargassum extract, add the compound enzyme, and enzymatically hydrolyze at 45-55℃ for 3-6 h to inactivate the enzyme and obtain the first extract; (3) Ultrasonic extraction: The extracts of Platycladus orientalis leaves and Yucca extract were combined and subjected to ultrasonic extraction at a frequency of 40-60 kHz at 35-45℃ to obtain a second extract; (4) Self-assembly construction: The first extract and the second extract are mixed and sheared at a high speed of 5000-8000 r / min for 15-30 min. The polarity difference between yucca saponins and blunt horsetail polysaccharides is used to induce self-assembly to form nano micelles.

[0008] Further, the complex enzyme in step (2) is composed of cellulase, papain and alginate lyase in a mass ratio of 3:(1-1.5):2, and the amount of the complex enzyme added is 0.5%-2.0% of the total mass of the raw materials.

[0009] Furthermore, in step (4), during the high-speed shearing process, a natural antioxidant with a mass fraction of 0.1%-0.5% is added dropwise, wherein the antioxidant is selected from at least one of rosemary extract, tea polyphenols, or vitamin E.

[0010] Furthermore, after the high-speed shearing in step (4) is completed, a high-pressure homogenization process is also included, wherein the pressure of the high-pressure homogenization is 40-80 MPa and the number of cycles is 2-4, so that the particle size distribution index (PDI) of the nanomicelles is less than 0.2.

[0011] Thirdly, the present invention provides the use of the composite composition in the preparation of cosmetics or personal care products with the function of repairing damaged hair follicles.

[0012] Furthermore, the personal care products are selected from shampoos, conditioners, hair growth serums, or scalp serums.

[0013] Fourthly, the present invention provides a scalp care product capable of promoting hair follicle growth, characterized in that, by weight percentage, it comprises 0.5%-10.0% of the composite composition described in any one of the preceding claims, with the remainder being a base acceptable for scalp care products.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows: First, a nano-targeted delivery system based on the self-assembly of saponins and polysaccharides. This invention overcomes the bottlenecks of poor stability and low absorption rate of traditional plant extracts. Utilizing the natural amphiphilicity of yucca saponins as a structure-activity backbone, it induces small-molecule polysaccharides from Sargassum fusiforme to self-assemble through hydrogen bonds into core-shell structured nanomicelles, encapsulating water-insoluble quercetin from Platycladus orientalis and active peptides from Luffa cylindrica within a hydrophobic core. The small particle size of 100-300 nm allows it to easily penetrate the infundibulum of hair follicles, achieving deep penetration and sustained release of active ingredients.

[0015] Secondly, this invention promotes hair follicle growth and scalp microcirculation reconstruction. The composition of this invention can synergistically promote hair follicle growth and nourish and activate the scalp microenvironment. Experimental data show that this composite composition can significantly improve hair follicle reconstruction, achieving substantial repair and hair growth promotion effects. Attached Figure Description

[0016] Figure 1 This is the negative control group showing hair follicle growth. Figure 2 This shows the hair follicle growth status of the experimental group. Detailed Implementation

[0017] To better illustrate the purpose, technical solution, and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0018] Example 1: Preparation of Nanomicelle Composite Composition (Self-Assembled Assembly) 1-1, Raw material preparation Sample preparation: 25g of Platycladus orientalis leaf extract, 15g of Yucca florida extract, 15g of Luffa cylindrica extract, and 10g of Sargassum fusiforme extract. (The Platycladus orientalis leaf extract was purchased from Guangzhou Tainuo Biotechnology Co., Ltd., the Yucca florida extract and Sargassum fusiforme extract were purchased from Guangdong Mingtong Biotechnology Co., Ltd., and the Luffa cylindrica extract was purchased from Guangzhou Xufan Biotechnology Co., Ltd.). The above raw materials were dissolved in purified water at a mass-to-volume ratio of 1:3 to obtain the corresponding extract extracts.

[0019] 1-2, Preparation steps Step S1 (compound enzymatic hydrolysis): Mix the loofah extract with Sargassum extract, add 0.8g of compound enzyme (cellulase:papain:alginate lyase = 3:1:2), hydrolyze at 50℃ for 4.5h, inactivate the enzyme (90℃, 10min), and filter to obtain the first extract.

[0020] Step S2 (Ultrasonic Extraction): Mix the extracts from Platycladus orientalis leaves and Yucca filamentosa leaves, and extract by ultrasonication at 40℃ and 50 kHz for 40 min to obtain the second extract.

[0021] Step S3 (Induced self-assembly): Mix the first and second extracts and add 0.2g of rosemary extract as an antioxidant.

[0022] Step S4 (High-speed shearing and homogenization): Turn on the high-speed shearing machine, set the speed to 7000 r / min, shear for 20 min, then transfer to the high-pressure homogenizer and cycle 3 times under a pressure of 60 MPa to obtain a pale yellow microemulsion liquid, which is the composite composition containing nano micelles.

[0023] Comparative Example 1: Ordinary Physics Mixed Group Same as Example 1, except for the preparation steps: the four extracts were mixed, collected and concentrated to the same solid content as in Example 1, 0.2g of rosemary extract was added, and the mixture was stirred for 30 minutes at room temperature and pressure using a regular stirrer (300r / min) to make it uniformly mixed, resulting in a dark brown slightly turbid liquid with no nanomicelles formed.

[0024] Comparative Example 2: Single Extract Mixture Group Same as Example 1, except that: no yucca extract is added during raw material preparation, and the missing part is made up with purified water. The preparation steps are exactly the same as those in Example 1, including enzymatic hydrolysis, ultrasonication and high-pressure homogenization. Due to the lack of yucca saponins as a hydrophobic framework, it is impossible to induce self-assembly to generate a stable micelle structure, thus obtaining a slightly turbid liquid.

[0025] Performance testing 1.1 The sample to be tested was observed using a dynamic light scattering instrument (DLS, Malvern Zetasizer Nano ZS90) and a transmission electron microscope (TEM, JEOL JEM-2100). The operation steps were performed in accordance with the instrument instructions and reagent instructions.

[0026] The results are shown in Table 1. Table 1 Microscopic characterization tests Average particle size (nm) 185.4 1200+ (unstable) 650.2 PDI (Particle Size Distribution Index) 0.142 0.658 0.485 Zeta potential (mV) -38.5 -5.2 -12.4 Micromorphology Regular spherical core-shell structure Irregular extract fragments Dispersed large particle aggregates 1.2 Coating rate determination Quercetin (purchased from Sichuan Weikeqi Biotechnology Co., Ltd.) from Platycladus orientalis leaves was used as the detection target. The micelles and free liquid were separated by ultracentrifugation, and the content was determined by HPLC. Specific methods included: a. Preparation of micelles: Mix 10 mg of quercetin with surfactant Tween-80 at a ratio of 1:10 (w / w), add approximately 10 mL of ultrapure water, and sonicate in a 40°C water bath for 30 minutes (power 200 W, frequency 40 kHz) to fully dissolve the quercetin and coat it into the micelle core, forming a clear and transparent micelle solution. b. Place the above micelle solution in an ultracentrifuge tube and centrifuge at 15000 rpm at 4°C for 30 minutes. Carefully aspirate the upper free liquid, avoiding disturbance of the bottom micelle precipitate. c. HPLC content determination: A standard curve was plotted, and the upper free liquid after centrifugation was filtered through a 0.22 μm microporous membrane. 20 μL of the filtrate was injected, and the free quercetin content was calculated according to the standard curve (Agilent 1260; chromatographic conditions: C18, mobile phase: acetonitrile-0.1% phosphoric acid aqueous solution (35:65, v / v), detection wavelength: 360 nm, flow rate: 1.0 mL / min, column temperature: 30℃). d. Coating rate calculation formula: Coating rate (%) = (total dosage - free drug content) / total dosage × 100%. The results are shown in Table 2.

[0027] Table 2. Measurement Results Example 1 88.6% Comparative Example 1 Effective encapsulation structures are almost impossible to detect. Comparative Example 2 Effective encapsulation structures are almost impossible to detect. Therefore, by combining ultracentrifugation with HPLC determination, the quercetin coating rate in Example 1 reached 88.6%, indicating that the micelle preparation process of the present invention can effectively coat quercetin into the micelle core. In contrast, Comparative Examples 1 and 2 could hardly form stable micelle structures, resulting in extremely low coating rates, with quercetin mostly existing in a precipitated or free state.

[0028] 1.3 Transdermal permeability test Ex vivo pig scalp was purchased from Beijing Yuansenkaide Biotechnology Co., Ltd.; Franz diffusion cell (effective diffusion area approximately 2.8 cm²) 2 (The receiving chamber has a volume of approximately 15 mL) was purchased from Yuyan Instruments Company.

[0029] The experimental procedure included: Soaking pig scalp in a saline solution specifically for ex vivo skin for equilibration for 30 minutes, then fixing it between the supply and receiving chambers of a Franz diffusion cell, with the stratum corneum facing upwards (supply chamber) and the dermis facing downwards (receiving chamber). The seal was checked to ensure no air bubbles remained on the skin-receiving fluid contact surface. Degassed saline solution was added to the receiving chamber, and a constant-temperature water bath was turned on to maintain the receiving fluid temperature at 32°C. Magnetic stirring was started at 300 r / min. 0.5 mL of the sample to be tested was precisely added to the supply chamber of each diffusion cell. The top of the supply chamber was sealed to prevent moisture evaporation. Timing began (T0). At time points of 1 h, 2 h, 4 h, 6 h, 8 h, 10 h, and 12 h, 0.5 mL of receiving fluid was precisely drawn from the sampling port of the receiving chamber. Immediately, isothermal and equal-volume fresh receiving fluid was added to maintain the leakage state. The extracted samples were filtered through a 0.22 μm microporous membrane for testing. Three replicates were performed for each group.

[0030] Referring to 1.2, quercetin, a marker component in Platycladus orientalis leaf extract, was selected as the detection target. Its concentration at each time point was determined using HPLC, and the cumulative permeation (Qn) was calculated. ; Where V0: total volume of the receiving chamber (mL), Cn: measured concentration at the nth sampling point (μg / mL), Vi: volume taken from the i-th sampling point, Ci: measured concentration at the i-th sampling point (μg / mL); A: effective diffusion area (cm²). 2 The results are shown in Table 3-4.

[0031] Table 3. Concentration of total quercetin in the receiving solution (μg / mL) 1 5.20±0.62 0.45±0.12 1.15±0.25 2 14.35±1.45 1.20±0.35 3.80±0.78 4 32.80±3.10 3.55±0.90 9.65±1.45 6 58.12±5.24 6.80±1.25 17.40±2.80 8 84.55±6.80 10.45±1.85 26.12±3.55 10 112.40±9.15 14.12±2.10 35.90±4.20 12 138.65±12.40 18.55±2.85 45.30±5.60 Table 4. Permeation enhancement efficiency of nanomicelles for total quercetin 12-hour cumulative permeation <![CDATA[145.2μg / cm 2 ·h]]> <![CDATA[32.8μg / cm 2 ·h]]> <![CDATA[51.4μg / cm 2 ·h]]> 12-hour cumulative permeability ratio 7.47 times 1.00 times 2.44 times The results showed that the total quercetin cumulative penetration of Example 1 was 7.47 times that of Comparative Example 1. This indicates that the nanomicelle structure successfully solved the problem of quercetin's difficulty in penetrating the stratum corneum. Although Comparative Example 2 underwent high-pressure homogenization, the lack of saponins from the yucca extract as a "nanomicel framework" resulted in its deep penetration being far inferior to that of Example 1, indicating that the three components—Platycladus orientalis leaf, yucca, and Sargassum fusiforme—have a synergistic effect in self-assembly.

[0032] Example 2: Cellular experiments promoting hair follicle growth (detection of human dermal papilla cells (HFDPC) proliferation and growth factors) Raw material preparation: The formulation of each component is shown in Table 5 below. Table 5, Component Formulation

[0033] The test samples with the above-mentioned proportions were prepared into nanomicelles according to the preparation steps in Example 1. 100 μL of the original sample was added to 900 μL of PBS to prepare a 10 mg / μL stock solution, which was then further diluted to 50 μg / μL (the value after safety evaluation) to obtain the test solution. Cell experiments were then performed, specifically as follows: Human dermal papilla cells (HFDPC) were cultured at 5 × 10⁻⁶ cells / mL. 3 Cells were seeded per well in 96-well plates. After cell adhesion, the test solutions for each group were added, and the cells were cultured for 48 hours. Following the manufacturer's instructions, CCK-8 reagent was added, and absorbance was measured at 450 nm. Cell proliferation rate was calculated. Simultaneously, cell supernatant was collected, and ELISA was performed according to the manufacturer's instructions to detect whether cells secreted key germinal signaling molecules: VEGF and KGF. HFDPC was purchased from Mingzhou Biotechnology, and the CCK-8 reagent and ELISA kit were purchased from Shanghai Tongwei. Results are shown in Table 6.

[0034] Table 6 Blank control 100±4.2 150.2±12.5 85.4±7.2 110.5±9.8 Positive control 145.6±5.8** 285.6±18.4 165.2±11.5 215.3±15.2 Example 1 162.3±9.2** 286.5±13.3 173.1±10.8 203.2±13.6 Test Example 1 128.4±4.5* 260.4±15.1 130.8±10.3 180.2±12.4 Test Example 2 122.1±3.9* 210.5±14.2 125.6±9.7 165.8±11.0 Test Example 3 112.3±6.1* 257.9±16.5 158.4±12.1 208.7±14.8 Compared with the blank control group, *P < 0.05, **P < 0.01 (Graphpad, One-way ANOVA analysis) The results showed that Example 1 (25:15:15:10) exhibited the highest cell proliferation rate and secretion of key factors, indicating that at this ratio, the hydrogen bond self-assembly structure formed by yucca saponins and Sargassum fusiforme polysaccharides was the most stable and had the highest encapsulation efficiency, enabling more effective delivery of flavonoids from Platycladus orientalis leaves into the cells. The composition of this invention significantly upregulated the secretion of VEGF, KGF, and IGF-1. VEGF is crucial for maintaining the microvascular network around hair follicles, providing sufficient nutrients to the follicles and inducing them to transition from the resting phase to the growth phase, thus promoting hair follicle growth. This experiment demonstrates that this composition not only protects dermal papilla cells but also improves the hair follicle microenvironment and promotes hair follicle growth through the secretion of signaling molecules.

[0035] Example 3: Animal experiments promoting hair follicle growth The composite composition of nanomicelles prepared in Example 1 was compounded into a hair care product. The basic matrix composition is shown in Table 7 below. Then, 0.5% of the composite composition of nanomicelles was homogenized and added for later use.

[0036] Table 7 Matrix Components Penetration regulator ethanol 10.0 Penetration enhancer Polysorbate-20 0.2 Thickener Xanthan Gum 0.2 Moisturizer glycerin 5 Chelating agents Disodium EDTA 0.1 solvent Deionized water margin Animal experiment preparation: 1. Animal preparation: Purchase 24 C57BL / 6 mice, 6-8 weeks old, half female and half male (Guangdong Yaokang Biotechnology Co., Ltd.). Mice housing conditions: temperature controlled at 20℃~26℃, relative humidity controlled at 30%~70%, free access to water and food, and lighting using 12h / 12h day and night alternation.

[0037] 2. Experimental grouping: After passing quarantine, the participants were grouped as shown in Table 8.

[0038] Table 8 Grouping Table Blank control group Hair removal only, no medication administered. negative control group Apply matrix components Positive control group 5% Minoxidil experimental group Composite composition containing 0.5% nanomicelles 24 hours before administration, approximately 2×2 cm of the mouse's back was shaved using an electric clipper. 2 The hair was then treated with a chemical depilatory cream (commercially available, Veet) to thoroughly remove any remaining hair roots. 100 μL of the sample was applied to the treated area at a fixed time each morning for 28 consecutive days. After treatment, the animals were euthanized (CO2) and grossly dissected. Skin samples from the treatment site were fixed in 4% paraformaldehyde solution, stained with hematoxylin and eosin (HE), prepared as slides, and subjected to histopathological examination. The histopathological results are shown in [link to histopathological examination report]. Figure 1-2 .

[0039] The experimental results showed that, compared with the negative control group, the hair regeneration rate on the back skin of mice in the treatment group was significantly faster. By day 21 of administration, the bald areas in the treatment group were almost completely covered by new hair, which was black, shiny, and densely distributed. Histological section analysis (HE staining) confirmed that the number of hair follicles per unit area was significantly increased in the treatment group, and the diameter of the hair follicles was thicker than that in the control group.

[0040] The various embodiments described in this specification are presented in a progressive manner, with each embodiment focusing on its differences from other embodiments. Similar or identical parts between embodiments can be referred to interchangeably. The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A composite composition with scalp care function, characterized in that, The method for preparing the composite composition includes the following steps: (1) Pretreatment: Prepare 15-35 parts of Platycladus orientalis leaf extract, 10-25 parts of Yucca extract, 10-20 parts of Luffa extract and 5-15 parts of Sargassum extract by weight, dissolve them in water respectively to prepare Platycladus orientalis leaf extract, Yucca extract, Luffa extract and Sargassum extract. (2) Compound enzymatic hydrolysis: Mix the loofah extract and the Sargassum extract, add the compound enzyme, and enzymatically hydrolyze at 45-55℃ for 3-6 h to inactivate the enzyme and obtain the first extract. (3) Ultrasonic extraction: The extracts of Platycladus orientalis leaves and Yucca extracts were combined and subjected to ultrasonic extraction at 35-45℃ and a frequency of 40-60 kHz to obtain a second extract. (4) Self-assembly construction: The first extract and the second extract are mixed and sheared at a speed of 5000-8000 r / min for 15-30 min. The polarity difference between yucca saponins and Sargassum polysaccharides induces self-assembly to form nano micelles. During the high-speed shearing process, a natural antioxidant with a mass fraction of 0.1%-0.5% is added dropwise. The antioxidant is rosemary extract. The compound enzyme is composed of cellulase, papain and alginate lyase in a mass ratio of 3:(1-1.5):2, and the amount of the compound enzyme added is 0.5%-2.0% of the total mass of the raw materials.

2. The composite composition according to claim 1, characterized in that, The composite composition contains a nanomicelle encapsulation structure formed by the self-assembly of yucca saponins and Sargassum fusiforme polysaccharides through hydrogen bonds, and the average particle size of the nanomicelles is 100-300 nm.

3. The composite composition according to claim 2, characterized in that, The mass fraction of quercetin in the Platycladus orientalis leaf extract is ≥1.5%.

4. The composite composition according to claim 3, characterized in that, After the high-speed shearing in step (4) is completed, a high-pressure homogenization process is also included. The pressure of the high-pressure homogenization is 40-80 MPa, and the number of cycles is 2-4 times, so that the particle size distribution index of the nanomicelles is less than 0.

2.

5. The use of the composite composition according to any one of claims 1-4 in the preparation of cosmetics that promote hair follicle growth.

6. The use of the composite composition according to any one of claims 1-4 in the preparation of personal care products that promote hair follicle growth.

7. The application as described in claim 6, characterized in that, The personal care products mentioned are selected from shampoos, conditioners, hair growth serums, or scalp serums.

8. A scalp care product with repairing function, characterized in that, The product comprises, by weight percentage, 0.5%-10.0% of the composite composition according to any one of claims 1-4, with the remainder being a base acceptable for scalp care products.

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