Composition, mask and application thereof
This mask, formulated with black willow bark extract and hydrogen storage materials, addresses the issues of skin barrier damage, microecological imbalance, and drug resistance in existing acne treatments. It achieves the effects of acne removal, oil control, and acne treatment, providing highly effective and safe cosmetic benefits.
Patent Information
- Application Number
- CN202511864457.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-11
- Publication Date
- 2026-03-20
AI Technical Summary
Existing acne treatments suffer from skin barrier damage, microecological imbalance, drug resistance, and safety issues, making them difficult to effectively remove acne, control oil production, and treat acne.
A facial mask was prepared by combining black willow bark extract with hydrogen storage material and using electrospinning technology to achieve sustained release of hydrogen and targeted delivery of anti-inflammatory components. The mass fraction of black willow bark extract in the composition is 0.130% to 0.210%, and the mass fraction of hydrogen storage material is 0.05% to 0.20%.
It significantly controls sebum secretion, reduces the number of pimples, fades acne scars, inhibits the growth of Propionibacterium acnes, improves acne, and enhances the stability and transdermal efficacy of active ingredients, while maintaining high safety.
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Figure CN121695048A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of functional cosmetics technology, specifically relating to a composition, a facial mask, and its uses. Background Technology
[0002] Sebum is secreted by sebaceous glands, and its main components are triglycerides, wax esters, squalene, and free fatty acids. Adequate sebum is essential for forming the skin barrier and maintaining skin moisture. However, excessive sebum secretion can lead to enlarged pores, skin inflammation, and dull skin tone.
[0003] Excessive sebum secretion and abnormal metabolism of keratinocytes at the pore opening lead to clogged pores, which in turn allows bacteria such as Propionibacterium acnes to multiply, decompose sebum, and produce irritating free fatty acids that leak into the surrounding skin tissue, triggering an immune system attack and potentially causing acne. To effectively treat acne, it is necessary to address each factor in the development process, such as regulating sebum secretion, dissolving keratinocytes, unclogging pores, killing bacteria, and reducing inflammation.
[0004] Acne is a chronic inflammatory disease of the pilosebaceous unit with a global incidence of up to 9.4%. Its pathological mechanism involves androgen-induced excessive sebum secretion, abnormal keratinization of the pilosebaceous duct, colonization of Propionibacterium acnes, and inflammatory cascade reactions mediated by the TLR2 / NF-κB pathway.
[0005] Most current acne treatments target the aforementioned pathological mechanisms; however, these treatments all have certain limitations. For example, while keratinizing ingredients, such as salicylic acid, can penetrate hair follicles, their efficacy is highly dependent on a low pH environment, typically ≤3.5, leading to impaired skin barrier function. Clinical data shows that transepidermal water loss increases by 25%-35% after two weeks of continuous use of keratinizing ingredients, and the uncontrolled penetration of these ingredients (e.g., 30% glycolic acid solution) into the dermis may pose a risk of burns. Furthermore, the overactivation of the inflammatory factor IL-1α by these ingredients may exacerbate erythema reactions, limiting their long-term value.
[0006] Among treatments targeting Propionibacterium acnes, benzoyl peroxide (BPO) can rapidly kill the bacteria, but its strong oxidizing properties lead to two side effects: firstly, it damages the linoleic acid structure in sebum, delaying the barrier repair process; secondly, it causes non-selective bactericidal activity, resulting in a >50% decrease in the abundance of resident skin flora and disrupting the microecological balance. More notably, a 5% concentration of BPO causes an oxidative fading rate of up to 90% on cotton fabrics, severely impacting user experience. In addition, antibiotics can be used to kill Propionibacterium acnes, but the widespread overuse of antibiotics has led to serious drug resistance problems. For example, the resistance rate of Propionibacterium acnes to clindamycin surged from 20% in 2008 to 62% in 2022. Furthermore, systemic exposure caused by transdermal absorption of antibiotics can trigger adverse intestinal reactions such as diarrhea, while the rapid degradation of antibiotic components like erythromycin under light further weakens their actual efficacy.
[0007] Plant-based ingredients, as natural components, are generally considered safe and have been explored for acne treatment in recent years. However, significant drawbacks exist in practical applications: for example, terpinene-4-ol in tea tree oil is lost by more than 40% after 30 days of opening, and it contains over 30 sensitizing terpenes. Ingredients like witch hazel require high concentrations of ethanol for penetration, exacerbating skin dryness, while tannin content exceeding 2% may induce keratinocyte apoptosis.
[0008] Therefore, there is a need for a product that uses plant-based ingredients as the main component to address acne, control oil, and treat acne. Summary of the Invention
[0009] Black willow (Salix nigra) bark extract has been reported to have pore-minimizing and skin-soothing effects and can be used as a skin conditioning agent; as a natural ingredient, it is attractive to consumers, but its effects are slow and gentle, so it is more often used as an auxiliary ingredient.
[0010] Hydrogen has been reported to have antioxidant capabilities, neutralizing free radicals in the skin and protecting skin cells from oxidative damage. At the same time, hydrogen can further enhance antioxidant and anti-inflammatory effects by penetrating into skin cells. Hydrogen-rich masks are an emerging and promising adjunctive treatment for skin improvement.
[0011] During the research, the inventors experimented with applying black willow bark extract to a hydrogen-rich facial mask system and unexpectedly discovered that when used in combination with hydrogen storage materials, black willow bark extract achieved excellent results in acne treatment, oil control, and acne removal. This effect significantly exceeded the inventors' initial predictions: First, the combined effect of black willow bark extract as an auxiliary ingredient and hydrogen as an auxiliary solution should have been limited, but the experiments described below confirmed that this combination significantly improved multiple effects; second, salicin may compete with hydrogen molecules for penetration through lipid channels in the stratum corneum, thus affecting the efficacy of both active ingredients; third, the strong reducing properties of active hydrogen may degrade plant active ingredients.
[0012] In view of this, the main objective of the present invention is to provide a composite material of black willow bark extract and hydrogen molecules, which achieves a dual-layer synergistic effect of sustained release of hydrogen and targeted delivery of anti-inflammatory components.
[0013] To achieve the above objectives, the technical solution adopted by the present invention is as follows.
[0014] The present invention provides a composition comprising a functional material and a spinning matrix. The functional material comprises black willow bark extract and a hydrogen storage material. The black willow bark extract has a mass fraction of 0.130% to 0.210% relative to the total mass of the composition, and the hydrogen storage material has a mass fraction of 0.05% to 0.20%. The spinning matrix has a mass fraction of 8% to 20% relative to the total mass of the composition.
[0015] In some embodiments, the mass fraction of the black willow bark extract is 0.150% to 0.190% relative to the total mass of the composition.
[0016] In some embodiments, the mass fraction of the hydrogen storage material is 0.10% to 0.20% relative to the total mass of the composition.
[0017] In some implementations, the hydrogen storage material is hydrogenated polydimethylsiloxane.
[0018] In some embodiments, the composition further includes a plasticizer and / or a preservative, wherein the plasticizer is present in a mass fraction of 1% to 5% and the preservative in a mass fraction of 0.1% to 1% relative to the total mass of the composition.
[0019] In some embodiments, the composition is a cosmetic composition.
[0020] The present invention also provides the use of the above-described compositions of the present invention in inhibiting sebum secretion in the skin.
[0021] The present invention also provides the use of the above-described compositions of the present invention in the preparation of products for treating acne.
[0022] The present invention also provides a face mask formed by electrospinning of the above-described composition of the present invention.
[0023] The present invention also provides a cosmetic method for treating acne and / or controlling oil using the above-described facial mask of the present invention, comprising applying the facial mask to the skin.
[0024] The beneficial effects of this invention are that by selecting black willow bark extract and hydrogen storage material as functional materials, it can significantly improve the effect of controlling sebum secretion and improving facial oil accumulation. On the other hand, it can significantly reduce the number of pimples in the subjects, lighten acne marks, and significantly relieve itching. Furthermore, it can inhibit the growth of Propionibacterium acnes and improve acne. At the same time, the test results of inhibiting 5α reductase activity reflect the synergistic effect of the two active ingredients.
[0025] Furthermore, the black willow bark extract of the present invention, combined with hydrogen storage materials, can simultaneously achieve the effects of controlling sebum secretion, removing acne, fading acne scars, and inhibiting the growth of Propionibacterium acnes.
[0026] Furthermore, the present invention uses a spinning matrix and functional materials together, which on the one hand can improve the stability of the composition and effectively retain the active ingredients; on the other hand, it can significantly improve the penetration effect of the active ingredients, achieve transdermal action more efficiently, and improve utilization rate; and on the other hand, it can prolong the action time of hydrogen molecules, and has a good sustained-release effect.
[0027] In addition, the composition of the present invention has the advantages of simple processing and high safety. Attached Figure Description
[0028] Figure 1 A before-and-after image of the face of a subject in Example 2 after applying the mask of the present invention for 28 days.
[0029] Figure 2 A before-and-after image of the face of a subject in Example 3 after 28 days of application of the mask of the present invention.
[0030] Figure 3 A before-and-after image of the face of a subject in Example 4 after 28 days of application of the mask of the present invention.
[0031] Figure 4 The figure shows the experimental results of the inhibitory effect of each group on Propionibacterium acnes in Example 5.
[0032] Figure 5 The figures show the experimental results of salicylic acid retention rate, hydrogen release rate, antibacterial rate, and transdermal effect for each group in Example 6. Detailed Implementation
[0033] The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0034] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood in the art to which this invention pertains. The following definitions supplement those in the art and relate to this application, but are not extrapolated to any relevant or unrelated circumstances, such as any conventionally used patent or application. While any methods and materials similar to or equivalent to those described herein may be used in practical testing, the materials and methods described herein are preferred. Therefore, the terminology used herein is intended to describe specific embodiments only and is not intended to limit the invention.
[0035] In this invention, the terms "comprising," "including," and "having" are open-ended descriptions that include the specified steps described, as well as other steps that do not substantially affect them, and are optional and not excluded.
[0036] The present invention provides a composition comprising a functional material and a spinning matrix. The functional material comprises black willow bark extract and a hydrogen storage material. The black willow bark extract has a mass fraction of 0.130% to 0.210% relative to the total mass of the composition, and the hydrogen storage material has a mass fraction of 0.05% to 0.15%. The spinning matrix has a mass fraction of 8% to 20% relative to the total mass of the composition.
[0037] In this invention, the combined effect of hydrogen molecules released from black willow bark extract and hydrogen storage material can effectively improve sebum secretion and reduce facial oil accumulation; and can more effectively inhibit the growth of Propionibacterium acnes for the treatment of acne.
[0038] For example, the mass fraction of the black willow bark extract relative to the total mass of the composition may be 0.130%, 0.140%, 0.150%, 0.160%, 0.170%, 0.174%, 0.180%, 0.190%, 0.200%, or 0.210%. In some specific embodiments, the mass fraction of the black willow bark extract relative to the total mass of the composition is from 0.150% to 0.190%.
[0039] In this invention, the hydrogen storage material is either directly rich in hydrogen molecules or capable of releasing hydrogen molecules upon application. Materials directly rich in hydrogen molecules mainly refer to gases (such as hydrogen gas, hydrogen-oxygen mixtures, etc.), liquids (such as hydrogen-rich water, saturated hydrogen water, hydrogen-rich saline, hydrogen-rich pharmaceutical solutions or serums, aqueous solutions rich in nano-hydrogen molecules, etc.) that directly contain hydrogen molecules, or porous materials that directly store hydrogen molecules through material adsorption, and can directly release hydrogen molecules upon application. Materials capable of releasing hydrogen molecules upon application mainly refer to materials that require contact with a reaction liquid to release hydrogen molecules, such as Mg, NH3BH3, and MgH2 materials, which require contact with water to react and release hydrogen gas.
[0040] In some implementations, the hydrogen storage material is selected from one or more of the following groups: metals, alloys, metal hydrides, carbonaceous materials, hydrates, and organic hydrogen storage materials.
[0041] In some implementations, the hydrogen storage material is selected from one or more of the group consisting of: hydrogenated polydimethylsiloxane, magnesium hydride, calcium hydride, metallic magnesium, metallic sodium, metallic zinc, hydrated silicon, and coral calcium.
[0042] For example, the mass fraction of the hydrogen storage material relative to the total mass of the composition may be 0.08%, 0.09%, 0.1%, 0.11%, 0.12%, 0.13%, 0.14%, 0.15%, 0.16%, 0.17%, 0.18%, 0.19%, or 0.20%. In some specific embodiments, the mass fraction of the hydrogen storage material relative to the total mass of the composition is from 0.10% to 0.20%.
[0043] In some specific implementation schemes, hydrogen storage material is hydrogenated polydimethylsiloxane. Hydrogenated polydimethylsiloxane is a mature organic hydrogen storage material that achieves efficient hydrogen storage through a dual mechanism of chemical bonding and physical adsorption. It possesses excellent thermal stability and can be safely stored at room temperature. As a solid-state hydrogen storage material, it has the advantages of high intrinsic safety and high volumetric hydrogen storage density, avoiding the risks of high-pressure or liquid hydrogen storage. This material supports reversible hydrogen absorption and desorption; high-purity hydrogen can be cyclically released through temperature / pressure control. It is currently used in portable hydrogen energy devices and stationary hydrogen storage systems, providing reliable support for hydrogen energy technology.
[0044] In this invention, the spinning matrix refers to a raw material that can be used in electrospinning. For example, the spinning matrix can be a natural polymer (such as chitosan, gelatin) and a biodegradable polymer (such as PLA, polycaprolactone PCL, polyvinyl alcohol PVA, etc.). In a specific embodiment, the spinning matrix is polyvinyl alcohol.
[0045] For example, the mass fraction of the spinning matrix relative to the total mass of the composition can be 8%, 8.5%, 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, 15%, 15.5%, 16%, 16.5%, 17%, 17.5%, 18%, 18.5%, 19%, 19.5%, or 20%.
[0046] In some embodiments, the composition further includes a plasticizer, and it is understood that any plasticizer suitable for use in cosmetic products such as face masks is applicable to this invention. For example, the plasticizer may be one or more of glycerin, sorbitol, and propylene glycol. In one specific embodiment, the plasticizer is glycerin.
[0047] In some embodiments, the plasticizer is present in a mass fraction of 1% to 5% relative to the total mass of the composition. Exemplarily, the mass fraction of the plasticizer relative to the total mass of the composition may be 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%.
[0048] In some embodiments, the composition further includes a preservative. It is understood that any preservative suitable for cosmetic products such as face masks is applicable to this invention. For example, the preservative may be one or more of phenoxyethanol, methylparaben, propylparaben, benzoic acid, sodium benzoate, phenethyl alcohol, chlorphenesin, methylparaben, propylene glycol, ethanol, and acetic acid. In one specific embodiment, the preservative is phenoxyethanol.
[0049] In some embodiments, the preservative is present in a mass fraction of 0.1% to 1% relative to the total mass of the composition. Exemplarily, the preservative may be present in a mass fraction of 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 1% relative to the total mass of the composition.
[0050] In some embodiments, the composition, except for the above-mentioned components, is made up to 100% by deionized water.
[0051] In some embodiments, the composition is a cosmetic composition.
[0052] The present invention also provides the use of the above-described compositions of the present invention in inhibiting sebum secretion in the skin.
[0053] The present invention also provides the use of the above-described compositions of the present invention in the preparation of products for treating acne, reducing oiliness, and removing acne.
[0054] The present invention also provides a facial mask formed by electrospinning of the above-described composition of the present invention. Electrospinning technology is used to generate a microfiber mesh structure. The fiber membrane formed by electrospinning technology has excellent breathability and comfort, and can adhere well to the skin surface.
[0055] In some embodiments, the parameters of electrospinning include: a voltage of 15 to 20 kV, for example, 15 kV, 15.5 kV, 16 kV, 16.5 kV, 17 kV, 18 kV, 18.5 kV, or 20 kV; a receiving distance of 14 to 16 cm, for example, 14 cm, 14.5 cm, 15 cm, 15.5 cm, or 16 cm; and a flow rate of 0.6 mL / h to 1 mL / h, for example, 0.6 mL / h, 0.7 mL / h, 0.8 mL / h, 0.9 mL / h, or 1 mL / h. In some embodiments, the parameters of electrospinning also include: the receiver is preferably a roller, and the roller is preferably covered with aluminum foil.
[0056] The present invention also provides a cosmetic method for treating acne and / or controlling oil using the above-described facial mask of the present invention, comprising applying the facial mask to the skin.
[0057] In some specific embodiments, the cosmetic method of using the above-described facial mask of the present invention for acne treatment and / or oil control preferably includes the following steps:
[0058] 1. Cleanse facial skin
[0059] Before using a face mask, please cleanse your face to remove dirt, oil, and makeup residue. Gently pat your skin dry to keep it moisturized.
[0060] 2. Open the mask packaging
[0061] Open the packaging, keep your hands clean, take out the mask, carefully unfold it and apply it to your face. Because it uses electrospinning technology and a water-soluble polymer as the matrix, it is dry and moisture-free when packaged and carried. When using, you need to spray it with a water phase mist to allow it to be absorbed into your face.
[0062] 3. Apply a face mask
[0063] Relax and enjoy 20 to 30 minutes of beauty time, allowing your skin to fully absorb the essence.
[0064] 4. Remove the face mask
[0065] Remove the mask and gently massage it into the skin until absorbed, following the skin's texture.
[0066] 5. Subsequent skincare
[0067] No further skin cleansing is required after use. You can proceed with your regular skincare routine as needed, such as applying a moisturizer to lock in moisture and nutrients.
[0068] In this invention, the preferred frequency of use for the face mask is 2-3 times per week, but the frequency can be adjusted according to the skin condition. If the skin is dry or there are specific care needs, the frequency of use can be increased appropriately.
[0069] The present invention also provides the use of the above-described compositions of the present invention in promoting wound healing in burn patients.
[0070] The present invention also provides a method for repairing burn wounds using the above-described mask of the present invention, comprising applying the mask to the skin.
[0071] In some specific implementations, the method of repairing burn wounds using the above-mentioned mask of the present invention preferably includes treating the burn wound with the above-mentioned mask of the present invention one day after routine emergency treatment and routine anti-inflammatory treatment.
[0072] The following describes preferred embodiments of the present invention, but the present invention is not limited to these preferred embodiments. It should be noted that any modifications and improvements made by those skilled in the art based on this inventive concept are within the scope of protection of the present invention. All reagents used, unless otherwise specified, are commercially available conventional products.
[0073] Example 1: Preparation of Facial Mask
[0074] Active ingredients: Black willow bark extract (mass fraction: 0.174%, manufacturer: Shanghai Zhina Biotechnology Co., Ltd., trade name: Black Willow Bark Extract), hydrogen (added in the form of hydrogenated polydimethylsiloxane, mass fraction: 0.15%);
[0075] Inactive ingredients: polyvinyl alcohol (PVA, 15% aqueous solution, as spinning matrix), deionized water (solvent, 81.176%), glycerin (3%, plasticizer), phenoxyethanol (0.5%, preservative).
[0076] Preparation steps:
[0077] 1. Preparation of spinning solution:
[0078] Dissolve PVA powder in deionized water at 70℃ to prepare a 15% solution, and stir magnetically for 2 hours until completely dissolved.
[0079] Cool to 40°C, then add glycerin, phenoxyethanol, black willow bark extract and hydrogenated polydimethylsiloxane in sequence, and continue stirring for 1 hour to form a homogeneous spinning solution.
[0080] 2. Electrospinning parameter settings: voltage 20kV, flow rate 0.8mL / h, receiving distance 15cm (aluminum foil receiving plate), ambient temperature and humidity 25℃, 45%RH, spinning time 4 hours.
[0081] After spinning, a black willow bark hydrogen composite face mask is obtained.
[0082] Example 2: The effect of composite masks on improving facial oil accumulation
[0083] The composite mask was prepared according to the method in Example 1. Thirty subjects aged 18-50 years (15 men and 15 women) were selected for trial use; all subjects had oily or combination skin. The composite mask was applied to the left side of the face once daily for 20 minutes each time, while no product was applied to the right side of the face. The treatment lasted for 28 days. Facial oil levels were measured daily using a sebumeter SM815 (10mm probe diameter), and the oil reduction rate was calculated according to formula (I).
[0084] Reduction rate = ×100%(I)
[0085] Test results are as follows Figure 1 As shown in Table 1, after 28 days of application, the oil content on the left side of the subjects' faces decreased significantly, with a much greater reduction rate than on the right side. All 30 subjects reported positive results and no allergic reactions. This indicates that the composite mask prepared in this invention can significantly improve facial oil accumulation in the subjects.
[0086] Table 1
[0087]
[0088]
[0089] Example 3: Acne-removing effects of composite facial masks
[0090] The composite mask was prepared according to the method in Example 1. Thirty subjects aged 18-35 years (different from the subjects in Example 2; 15 males and 15 females) were selected for trial use. All subjects had moderate to severe acne on their faces. The composite mask was applied once daily for 15 minutes each time, for 28 consecutive days. The number of pimples and the degree of redness and swelling were recorded daily during this period.
[0091] The results are as follows Figure 2 As shown in Table 2, after 7 days of application, the subjects' facial acne decreased by more than 30%, and itching was significantly relieved. After 28 days of application, the acne clearance rate reached 80%, and acne scars were significantly faded. Furthermore, all subjects reported positive results and no allergic reactions. This indicates that the composite mask prepared in this invention can significantly remove facial acne.
[0092] Table 2
[0093]
[0094]
[0095] Example 4: Oil-controlling effect of composite facial masks
[0096] The composite mask was prepared according to the method in Example 1. Thirty subjects aged 18-35 years (different from the subjects in Examples 2 and 3; 15 males and 15 females) were selected for trial use. All subjects had moderate to severe facial oiliness, mainly manifested as excessive sebum secretion in the T-zone, noticeable afternoon shine, and in some cases, enlarged pores. The composite mask was applied once daily for 15 minutes each time, for 28 consecutive days. During this period, facial sebum secretion, the duration of T-zone oiliness, and pore visibility were measured and recorded using a skin oil analyzer. After 28 days of use, if the duration of T-zone oiliness was ≤2 hours, and significantly shorter than before use, it was considered an improvement in oiliness. The improvement rate was calculated as: "Improvement rate = Number of subjects meeting the 'improvement' criteria / Total subjects × 100%". The results are as follows... Figure 3 As shown in Table 3, after 7 days of application, the subjects' facial oil secretion decreased by more than 35% compared to before use, and the duration of T-zone oiliness was shortened to less than 2 hours (compared to an average of 4.5 hours before use), resulting in a significantly improved facial refresh. After 28 days of application, the subjects' facial oil secretion stabilized within the normal range, the improvement rate of T-zone oiliness reached 100%, pore visibility was significantly reduced, and the overall skin smoothness improved. All subjects reported a comfortable experience with no adverse reactions such as tightness or stinging.
[0097] Table 3
[0098]
[0099]
[0100] Example 5: Inhibitory effect of composite facial mask on Propionibacterium acnes
[0101] The standard strain of *Propionibacterium acnes* ATCC 6919 was cultured anaerobically in brain and heart broth. The experiment was divided into three groups: the experimental group used the essence of this compound facial mask; the positive control group used a commercially available anti-acne product (product name: Fanfen FBCY Bath Essence Oil, specification: 200ml / bottle); and the negative control group used physiological saline. The bacterial concentration was adjusted to 1×10⁻⁶. 6CFU / mL, add 100 μL of bacterial culture to each well of a 96-well plate, and add 100 μL of the corresponding solution, with 6 parallel wells for each. Incubate anaerobically at 37℃ for 24 h. After adding MTT solution and incubating for another 4 h, dissolve and crystallize in DMSO, and measure the OD value at 570 nm using a microplate reader. Calculate the inhibition rate according to "Inhibition rate = (1 - OD value of treatment group after culture / OD value of negative control group after culture) × 100%".
[0102] The experimental results are shown in Table 4 and Figure 4 As shown, the antibacterial rate of the mask of the present invention reaches 82%, which is better than the 65% of the positive control group, confirming that the mask of the present invention has a significant inhibitory effect on Propionibacterium acnes and can effectively inhibit the proliferation of Propionibacterium acnes.
[0103] Table 4
[0104]
[0105] Example 6: Validation of the effect of combining black willow extract with hydrogen storage materials
[0106] Four sets of comparative experiments were designed, the only difference being the composition of each component.
[0107] Group A contains polyvinyl alcohol (PVA) + 5% salicylic acid;
[0108] Group B contains polyvinyl alcohol (PVA) + 0.174% black willow bark extract + 5% salicylic acid;
[0109] Group C contains polyvinyl alcohol (PVA) + 0.15% hydrogenated polydimethylsiloxane + 5% salicylic acid;
[0110] Group D contains polyvinyl alcohol (PVA) + 0.174% black willow bark extract + 0.15% hydrogenated polydimethylsiloxane + 5% salicylic acid;
[0111] All other components are consistent with those in Example 1.
[0112] The following tests were performed on the four groups of samples:
[0113] 1. Stability Test: The four groups of experimental samples were stored at a constant temperature of 37℃ for 4 weeks to simulate the physiological temperature of the human body and to examine their long-term stability. After storage, the remaining content of salicylic acid in each group was detected by high performance liquid chromatography, and its retention rate relative to the initial loading was calculated.
[0114] 2. Sustained-release performance: Phosphate buffer solution was selected as the release medium to simulate the physiological environment of the human body and ensure the solubility stability of salicylic acid. A dissolution tester was used, with the temperature controlled at 37℃ and the rotation speed set at 50 rpm. Four groups of samples were placed in dissolution cups and an appropriate amount of release medium was added to ensure full contact. Release experiments were conducted under the set conditions. Samples were taken after 6 hours, filtered through a 0.45 μm filter membrane, and the content of salicylic acid in the filtrate was detected by high performance liquid chromatography. Finally, the ratio of salicylic acid to the initial loading was calculated to evaluate the sustained-release effect.
[0115] 3. Antibacterial properties: The antibacterial rate was tested by co-culturing with pathogenic bacteria (Propionibacterium acnes) and detecting the survival of bacteria. The antibacterial rate was calculated (antibacterial rate = (1 - bacterial survival in the treatment group / bacterial survival in the blank control group) × 100%).
[0116] 4. Transdermal efficiency: Using Franz diffusion cells, the skin model was placed between the diffusion cells. Drug-containing samples were added to the drug supply side, and samples were taken periodically from the receiving side. The amount of drug permeated and the drug concentration in the dermis were detected by high performance liquid chromatography to evaluate the transdermal efficiency.
[0117] 5. Safety verification: A cytotoxicity test was conducted. Skin cells were co-cultured with the sample, and cell metabolic activity was detected. Cell survival rate was calculated (cell survival rate = (OD value of sample group / OD value of blank control group) × 100%) to assess the safety of the sample.
[0118] The results are shown in Table 5 and Figure 5 As shown, group D had the highest salicylic acid retention rate, reaching 92.1%; while group D had the lowest release rate at 6 h, indicating that group D exhibited a "low initial release + sustained release" characteristic. Furthermore, group D achieved the highest antibacterial rate of 96.2% among all treatment groups. Transdermal efficiency assessment showed that group D achieved a transdermal dose of 192 μg / cm² at 24 h and a dermal drug concentration of 85 μg / cm³, both the highest among all treatment groups. Safety verification showed that cell viability in all groups was >90%. In summary, group D (polyvinyl alcohol (PVA) + 0.174% black willow bark extract + 0.15% hydrogenated polydimethylsiloxane + 5% salicylic acid, i.e., the combination regimen) was significantly superior to the regimens in other treatment groups (p < 0.05, CI < 1).
[0119] Table 5
[0120]
[0121] Example 7: Validation of the effect of combining black willow extract with different hydrogen storage materials
[0122] To verify the effect of combining black willow extract with different hydrogen storage materials, five experimental groups were designed, using group D in Example 6 as the reference group and replacing the hydrogen storage materials therein.
[0123] Group D-1 contains polyvinyl alcohol (PVA) + 0.174% black willow bark extract + 0.15% magnesium hydride (particle size D50 < 10 μm) + 5% salicylic acid;
[0124] Group D-2 contains polyvinyl alcohol (PVA) + 0.174% black willow bark extract + 0.15% calcium hydride (particle size D50 < 15 μm) + 5% salicylic acid;
[0125] Group D-3 contains polyvinyl alcohol (PVA) + 0.174% black willow bark extract + 0.15% metallic magnesium (particle size D50 < 20 μm) + 5% salicylic acid;
[0126] Group D-4 contains polyvinyl alcohol (PVA) + 0.174% black willow bark extract + 0.15% ammonia borane (particle size D50 < 5 μm) + 5% salicylic acid;
[0127] Group D-5 contains polyvinyl alcohol (PVA) + 0.174% black willow bark extract + 0.15% hydrated silica (particle size D50 < 30 μm) + 5% salicylic acid;
[0128] All other components are consistent with those in Example 1.
[0129] The stability, sustained-release performance, antibacterial performance, transdermal efficiency, and safety performance of the five groups of samples were tested using the same method as in Example 6.
[0130] The results are shown in Table 6. It can be seen that the transdermal dose of the original group D was 192 µg / cm² and the drug concentration in the dermis was 85 µg / cm³, both of which were the highest values. The transdermal doses of groups D-1 to D-5 were 189, 187, 190, 188, and 191 µg / cm², respectively, and the drug concentration in the dermis was 83 to 84 µg / cm³. There were no significant differences compared with group D (one-way ANOVA showed P>0.05), and all of them could achieve the goal of "high retention-deep penetration".
[0131] Regarding the retention rate of salicylic acid, group D had the highest retention rate at 92.1%; groups D-1 to D-5 had retention rates of 91.8%, 90.9%, 91.5%, 90.6%, and 91.3% respectively, all remaining stable at ≥90%. This indicates that the protective effect of the "black willow bark extract-hydrogen" combined system on the active ingredients is not affected by the type of hydrogen storage material, and high retention can be achieved in all cases.
[0132] Regarding the 6-hour release rate, Group D had the lowest rate at 28.3%; Groups D-1 to D-5 ranged from 28.7% to 30.1%, with no statistical difference from the original Group D (P>0.05). All groups exhibited a slow-release characteristic of "low initial release + continuous release", indicating that the slow-release behavior is mainly dominated by the hydrogen bond-nanofiber network, rather than determined by a specific hydrogen storage medium.
[0133] In terms of antibacterial rate, group D reached 96.2%, and groups D-1 to D-5 ranged from 95.1% to 96.0%, all of which were significantly higher than group A without dihydrogen blank carrier in Example 6 (85.1%, P<0.01). Moreover, there was no significant difference among the hydrogen storage material groups, which confirms that the synergistic effect of hydrogen molecules and black willow bark polyphenols in inhibiting Propionibacterium acnes is universal.
[0134] In terms of safety, the cell survival rate of all hydrogen-containing groups was >90%, which was no different from the blank control, suggesting that replacing the hydrogen storage material would not introduce additional cytotoxicity.
[0135] In summary, the results of Group D and Groups D-1 to D-5 show that different hydrogen storage materials exhibit consistent performance in five dimensions: retention rate, sustained-release characteristics, antibacterial activity, transdermal efficiency, and safety. All of these materials are significantly superior to the dual-hydrogen control Group A in Example 6 (p<0.05, CI<1), demonstrating that the "black willow bark extract-hydrogen molecule synergistic platform" of this invention does not depend on a specific hydrogen storage medium and possesses material versatility and technological scalability.
[0136] Table 6
[0137]
[0138] Example 8: Inhibition of 5α-reductase activity and verification of synergistic effect
[0139] The main androgen in the human body is testosterone, which stimulates the sebaceous glands to secrete oil. 5α-reductase is responsible for converting testosterone into DHT, which is 5-10 times more potent. DHT binds to receptors on sebaceous gland cells, causing excessive proliferation of the sebaceous glands and the secretion of large amounts of oil. By inhibiting the activity of 5α-reductase, the production of DHT can be effectively reduced. Thus, even if testosterone levels are normal, the lack of strong DHT stimulation greatly weakens the "oil-producing" signal received by the sebaceous glands, reducing excessive sebum secretion at its source and achieving "oil control."
[0140] This experiment used SPF-grade male 8-week-old SD rats, with 8 rats in each group to ensure a balanced sample size and compliance with animal experimental standards. The experiment consisted of 4 groups: the control group was treated with physiological saline, the mask group 1 used a composite sample containing black willow bark extract and hydrogen, the mask group 2 used only the black willow bark extract sample, and the mask group 3 used only the hydrogen-containing sample.
[0141] 0.2g of the corresponding sample was evenly applied to the back of rats daily for 4 weeks. After the experiment, the 5α-reductase activity in the skin tissue of the rat back was measured, and sebum secretion was also determined. Synergistic effects were calculated using the synergistic index (SI) formula: SI = (Ecombined - Eindividual) / Eindividual. A SI > 0 indicated the presence of synergy.
[0142] The experimental results are shown in Table 7. It can be seen that the 5α reductase inhibition rate of mask group 1 was 65%±5%, the sebum secretion was reduced by 50%±5%, and the sebum regulation effect was significantly better than other groups (p<0.01); the inhibition rates of mask groups 2 and 3 were 40%±4% and 10%±3%, respectively, and the control group had no inhibitory effect.
[0143] The synergistic index is calculated using the formula SI = (Ecombination - Eindividual) / Eindividual, where E represents the 5α-reductase inhibition rate. "Ecombination" is the inhibition rate of mask group 1 (black willow bark extract + hydrogen) at 65%, and "Eindividual" is the sum of the inhibition rates of mask group 2 (black willow bark extract only) and mask group 3 (hydrogen-containing sample only). Substituting these values into the formula yields: SI = =0.3, which indicates the existence of a synergistic effect.
[0144] Table 7
[0145]
[0146] Example 9: The effect of black willow bark extract hydrogen composite mask on promoting wound repair in burn patients
[0147] The facial mask was prepared using the method described in Example 1. Masks were also prepared in the same way for control groups, one containing only black willow bark extract and the other containing only hydrogen storage material. Patients with second-degree burns were selected for treatment, with the mask changed every two days. Five patients were selected for each of the composite mask group and the two control groups. All patients exhibited some degree of ulceration and mucosal tissue damage, with blister formation. One day after routine emergency treatment and anti-inflammatory measures, the appropriate facial mask was applied. After five consecutive days of mask application, professional medical staff assessed each patient for four clinical symptoms: blisters, ulceration, wound redness and swelling, and itching and pain. The number of patients exhibiting these symptoms in each group was counted, and the incidence rate was calculated as: (Number of patients with symptoms / Total number of patients) × 100%.
[0148] The experimental results are shown in Table 8 below. After 5 days, the blisters of the four patients in the composite dressing group were absorbed and disappeared; the skin lesions of all patients had healed and there were no ulcers; the redness and swelling were reduced and the itching and pain disappeared. All four dimensions were significantly better than those of the single-component dressing, which confirmed its synergistic effect in promoting wound repair and suggested that the composite dressing can promote wound repair in burn patients.
[0149] Table 8
[0150]
[0151] The above description is merely a preferred embodiment of the present invention and is not intended to limit the scope of protection of the present invention.
Claims
1. A composition, characterized in that, Including functional materials and spinning matrices, The functional materials include black willow bark extract and hydrogen storage material, wherein the mass fraction of the black willow bark extract is 0.130% to 0.210% relative to the total mass of the composition, and the mass fraction of the hydrogen storage material is 0.05% to 0.20%. The spinning matrix has a mass fraction of 8% to 20% relative to the total mass of the composition.
2. The composition according to claim 1, characterized in that, The mass fraction of the black willow bark extract is 0.150% to 0.190% relative to the total mass of the composition.
3. The composition according to claim 1, characterized in that, The mass fraction of the hydrogen storage material is 0.10% to 0.20% relative to the total mass of the composition.
4. The composition according to claim 1, characterized in that, The hydrogen storage material is hydrogenated polydimethylsiloxane.
5. The composition according to claim 1, characterized in that, The composition further comprises a plasticizer and / or a preservative, wherein the plasticizer has a mass fraction of 1% to 5% and the preservative has a mass fraction of 0.1% to 1% relative to the total mass of the composition.
6. The composition according to any one of claims 1 to 5, characterized in that, The composition is a cosmetic composition.
7. Use of the composition according to any one of claims 1 to 6 in inhibiting sebum secretion in the skin.
8. Use of the composition according to any one of claims 1 to 6 in the preparation of a product for treating acne.
9. A facial mask, characterized in that, The face mask is formed by electrospinning from the composition of any one of claims 1 to 6.
10. A cosmetic method for treating acne and / or controlling oil using the facial mask of claim 9, comprising applying the facial mask to the skin.
