Preparation of gel mask liquid containing plant extract composition

Through ultrasonic assisted extraction technology and alcohol precipitation method, the problem of low efficiency of existing extraction technology was solved, and efficient hematoxylin and cat claw polysaccharide were successfully prepared to prepare gel mask liquid with antioxidant and antibacterial effects, meeting the safety needs of skin care.

CN119792167APending Publication Date: 2025-04-11NANJING FORESTRY UNIV
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Patent Information

Application Number
CN202510167573.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-14
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

The existing extraction technology is inefficient and it is difficult to effectively extract hemu extract and cat claw grass extract, which limits its application in skin care products.

Method used

Ultrasonic assisted extraction technology, combined with alcohol precipitation and lyophilization treatment, improve the stability and efficiency of the extract, and prepare a gel mask liquid containing 2%-10% hematoxylin polyphenol and 2%-10% cat claw grass polysaccharide.

Benefits of technology

It has achieved efficient extraction of hematoxylin polyphenols and cat claw grass polysaccharides, improved the antioxidant and antibacterial effects of the product, met the skin care safety needs, and provided new ideas for cosmetics development.

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Abstract

The invention relates to preparation of a gel mask liquid containing a plant extract composition, and particularly discloses a gel mask liquid containing a sappan wood extract, a radix ranunculi ternati extract, a mask liquid matrix and purified water. In addition, the invention further discloses a preparation method of the hematoxylon extract and the radix ranunculi ternati extract, and the hematoxylon extract and the radix ranunculi ternati extract are applied to skin care product gel masks needing to have the anti-oxidation or anti-corrosion effect. Experimental results show that the skin care product antioxidant and preservative provided by the invention can effectively inhibit the growth of microorganisms, and the oxidation resistance and corrosion resistance of the product are remarkably improved. Skin care product preservative challenge tests prove that the product added with the plant extract is obviously superior to the product without the plant extract in the aspects of antioxidant skin care effect and preservative property. The raw materials are natural in source, have excellent antioxidant and antibacterial properties, are safe and mild, are convenient to use, and are suitable for skin care application.
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Description

Technical Field

[0001] The present application relates to the technical field of skin care products, and in particular to a method for preparing plant extracts and their application in cosmetics. Background Art

[0002] With the continuous improvement of the quality of life, people's demand for high-end skin care solutions has gradually increased, which has led to the emergence of a wide variety of beauty and skin care products on the market. Among them, facial masks are popular due to their versatility and portability. In particular, gel masks, as a unique category among facial masks, have developed significantly in recent years. At present, the main functions of facial masks on the market include anti-oxidation, antibacterial, hydrating and anti-aging. It is worth noting that gel masks formulated with natural active ingredients are highly favored by consumers due to their green and environmentally friendly characteristics.

[0003] Sappanwood Extract (SE), derived from the heartwood of Caesalpinia sappan, is a natural substance rich in bioactive ingredients, mainly polyphenolic compounds. These compounds include brazilin and sappan yellow flavonoids, which exhibit a wide range of biological effects. Historically, sappanwood extract has been widely used in traditional medicine and dye industries, and has become a research hotspot in the pharmaceutical and cosmetic fields in recent years.

[0004] Cat's Claw (Radix Ranunculi Ternati, Rt), also known as three-leaf Bidens Needle Grass and Golden Claw Grass, is the dried root of Ranunculus ternatus Thunb., a plant of the Ranunculaceae family. It is commonly used in traditional Chinese medicine and skin care. Cat's Claw is rich in active ingredients such as alkaloids, saponins, flavonoids, polysaccharides, and has multiple pharmacological activities.

[0005] Traditional extraction technology has the disadvantages of low efficiency and low extraction rate. In order to maximize the application of extracts in skin care products, it is meaningful to use more natural and safe extraction methods to obtain plant raw materials.

[0006] At the same time, adding natural active ingredients to facial masks can not only reduce side effects and improve safety, but also promote smoother, more hydrated and elastic skin. In addition, these ingredients may have a certain therapeutic effect on skin problems such as acne and blackheads. As the main bioactive component of sappan wood, sappan wood polyphenols play an important role in antioxidant and antibacterial effects. Although existing research mainly focuses on the potential application of sappan wood polyphenols in medical fields such as cardiovascular disease and cancer, there is still little research on its application as a cosmetic raw material, especially in facial masks. Summary of the invention

[0007] In view of this, the purpose of the present invention is to provide a plant extract having excellent antioxidant and antibacterial effects, and to apply the plant extract in cosmetics to prepare an anti-aging gel mask liquid that is natural, safe, mild and skin-friendly.

[0008] The object of the present invention is achieved through the following technical solutions:

[0009] A gel facial mask liquid containing a plant extract composition comprises the following components: a sappan wood extract, a cat's claw extract, a facial mask liquid matrix, a moisturizer, and the balance is purified water.

[0010] Furthermore, the skin care raw materials include 2%-10% sappan wood extract, 2%-10% cat's claw extract, 0.01%-0.05% facial mask liquid matrix, 5%-10% moisturizer, 0.05%-0.15% citric acid (Citric Acid, CA), and the balance is water.

[0011] Furthermore, the facial mask liquid matrix is ​​one or two of sodium carboxymethyl cellulose, chitosan, sodium hyaluronate, and xanthan gum, and the moisturizing agent is one or two of caprylyl glycol, pentylene glycol, propylene glycol, and ethylene glycol.

[0012] Furthermore, the facial mask liquid matrix is ​​sodium carboxymethyl cellulose, and the moisturizing agent is propylene glycol.

[0013] There are usually stability issues with sappan wood polyphenols. Adding a certain amount of propylene glycol can solubilize and stabilize at low temperatures. It can maintain the stability of the ingredients in the formula, improve the stability of the formula system, and has a good moisturizing effect when added to skin care products.

[0014] The method for preparing hematoxylin polyphenols comprises the following steps:

[0015] (1) Wash the bark of Sappan wood with clean water, dry it at 60°C, crush it through a sieve with a pore size of 0.21 mm, and sterilize it by irradiation;

[0016] (2) Ultrasonic alcohol extraction, preferably with an intensity of 100W, an extraction temperature of 20°C-70°C, a liquid-to-solid ratio of 20-45mL / g, an ethanol volume fraction of 30%-80%, an extraction time of 10-60min, and centrifugation at 6000-12000rpm / min to obtain the supernatant, evaporate and concentrate in a vacuum rotary device to remove the organic solvent, combine the concentrates, place in a vacuum freeze dryer for 24h to obtain freeze-dried powder, and store at -20°C in the dark for later use.

[0017] The preparation method of cat's claw polysaccharide comprises the following preparation steps:

[0018] (1) Ultrasonic-assisted water extraction method: clean the cat's claw, dry it at 60°C, crush it and pass it through a 0.21 mm sieve for later use, use 8-10 times the amount of water (mass ratio), ultrasonically heat it at 30°C for 30 min, remove the filter residue, use a rotary evaporator to concentrate, collect the concentrate, perform the same operation twice, and combine the two concentrates;

[0019] (2) Alcohol precipitation method: Add an appropriate amount of organic solvent to the cat's claw water extract, stir evenly, and place in a refrigerator at 4°C overnight. After centrifugation, concentrate and freeze-dry for later use.

[0020] The second object of the present invention is to provide the use of the plant extract in skin care products. The skin care products include care products with antioxidant and / or antiseptic requirements, such as water, milk, cream, sunscreen and facial mask. The present invention uses it in gel facial mask liquid.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] (1) Green extraction technology: using ultrasound to assist extraction, improve extraction efficiency and maintain the stability of active ingredients;

[0023] (2) Targeted extraction: Targeting specific effects (antioxidant, anti-aging), accurately extracting polyphenols from sappan wood extracts to avoid ingredient waste;

[0024] (3) Optimization of ingredient combination: The present invention adds two plant extracts and studies the synergistic effect of the composite plant extracts to improve the product efficacy. The composite plant extracts not only have better antioxidant effects, but also have stronger antibacterial effects, meeting the public's growing demand for skin care safety;

[0025] (4) Multifunctional application: Develop extracts with multiple functions (such as anti-inflammatory, antioxidant and moisturizing functions) to reduce the complexity of the formula, improve product performance, and provide new ideas for cosmetic development. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The present invention will be further described below in conjunction with the accompanying drawings.

[0027] Figure 1 : Sample pictures of gel mask liquid and wetting angle effect pictures of several formulas

[0028] Figure 2 : Antioxidant effect of gel mask liquid

[0029] Figure 3 :Antibacterial effect of gel mask liquid

[0030] Figure 4 :Biocompatibility of gel mask solution DETAILED DESCRIPTION

[0031] In order to better understand the above-mentioned objects, features and advantages of the present invention, the specific implementation methods of the present invention are described in detail below in conjunction with specific embodiments.

[0032] The structures, proportions, sizes, etc. illustrated in the drawings of the specification are only used to match the contents disclosed in the specification for people familiar with this technology to understand and read, and are not used to limit the limiting conditions for the implementation of the present invention, so they have no substantial technical significance. Any modification of the structure, change of the proportion relationship or adjustment of the size, without affecting the effects and purposes that can be achieved by the present invention, should still fall within the scope of the technical contents disclosed by the present invention. At the same time, the terms such as "upper", "lower", "front", "back", "middle" and so on quoted in this specification are only for the convenience of description, and are not used to limit the scope of the implementation of the present invention. The change or adjustment of their relative relationship should also be regarded as the scope of the implementation of the present invention without substantially changing the technical contents.

[0033] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments.

[0034] Example 1

[0035] The preparation method of hematoxylin polyphenols comprises the following steps:

[0036] (1) Wash the bark of the sappan wood with clean water, dry it at 60°C, grind it through a sieve with a pore size of 0.21 mm, and sterilize it by irradiation.

[0037] (2) Ultrasonic alcohol extraction, intensity 100w, extraction temperature 20℃-70℃, liquid-to-solid ratio 20-45mL / g, ethanol volume fraction 30%-80%, extraction time 10-60min, centrifugation at 6000-12000rpm / min to obtain the supernatant, evaporate and concentrate in a vacuum rotary device to remove the organic solvent, combine the concentrates, place in a vacuum freeze dryer for 24h to obtain freeze-dried powder, and store at -20℃ in the dark for later use.

[0038] (3) After optimizing various influencing factors, ultrasonic alcohol extraction was performed, with an intensity of preferably 100w, an extraction temperature of 20°C-70°C, a liquid-to-solid ratio of 30-40mL / g, an ethanol volume fraction of 50%-70%, and extraction for 10-30min. The supernatant was centrifuged at 10,000rpm / min, evaporated and concentrated in a vacuum rotary device to remove the organic solvent, and the concentrated solution was combined and placed in a vacuum freeze dryer for 24h to obtain a freeze-dried powder, which was stored at -20°C in the dark for later use.

[0039] Example 2

[0040] The preparation method of cat's claw polysaccharide comprises the following steps:

[0041] (1) Ultrasonic-assisted water extraction method: clean the cat's claw, dry it at 60°C, crush it and pass it through a 0.21 mm sieve for later use, use 8-10 times the amount of water (mass ratio), ultrasonically heat it at 30°C for 30 min, remove the filter residue, use a rotary evaporator to concentrate, collect the concentrate, perform the same operation twice, and combine the two concentrates;

[0042] (2) Alcohol precipitation method: Add an appropriate amount of organic solvent to the cat's claw water extract, stir evenly, and place in a refrigerator at 4°C overnight. After centrifugation, concentrate and freeze-dry for later use.

[0043] The dried cat's claw is preferred, and the ultrasonic extraction intensity is preferably 100 W. The centrifugal speed is 6000-12000 rpm / min, preferably 10000 rpm / min.

[0044] Example 3

[0045] A preparation method of a gel facial mask liquid containing a plant extract composition comprises the following steps:

[0046] The plant extracts are added to the sodium carboxymethyl cellulose matrix according to a certain formula ratio, stirred and evenly dispersed by ultrasonic crusher, and then set aside after eliminating bubbles.

[0047] The formula is as follows: dissolve an appropriate amount of solid sodium carboxymethylcellulose (CMC-Na) in water, add 2%-10% cat's claw polysaccharide mucus and 5%-10% moisturizer at room temperature, add 0.05%-0.15% citric acid in the presence of 2%-10% sappan wood polyphenol extract (SE), and continue stirring to obtain a uniform gel mask liquid.

[0048] Among them, gel mask liquid A: CMC-Na, gel mask liquid B: CMC-Na / Rt, gel mask liquid C: CMC-Na / Rt / SE / CA (0.05%), gel mask liquid D: CMC-Na / Rt / SE / CA (0.1%), gel mask liquid E: CMC-Na / Rt / SE / CA (0.15%).

[0049] The parameters of the ultrasonic disruption were set as follows: ultrasonic power 200 W, frequency 20 kHz, pulse mode 3 s on / 2 s off, and time setting 20 min (detection every 10 min).

[0050] Test Example 1. Antioxidant Testing of Gel Mask Liquid

[0051] (1) ABTS free radical scavenging test

[0052] 7.4mmol / L ABTS solution and 2.6mmol / L potassium persulfate solution were mixed in a volume ratio of 1:1 and reacted for 12 hours in a dark environment to generate ABTS. + Then, take 0.2mL of the diluted gel mask solution and 0.8mL of ABTS + The free radical cation solution (absorbance value is 0.7±0.02) was mixed. Then, it was allowed to stand for 6 minutes under light-proof conditions, and the absorbance was measured at 734 nm using a spectrophotometer. The result was expressed as ABTS + The inhibition rate is expressed as a percentage and is calculated as follows:

[0053] ABTS + (%)=(Abscontrd-Abssample) / Abscontrd×100

[0054] (2) DPPH free radical scavenging test

[0055] Take 100 μL of sample and mix with 1 mL of DPPH solution and let stand at room temperature for 30 minutes in the dark. The result is expressed as DPPH% and calculated using the following formula:

[0056] DPPH(%)=[Absblank-(Abssample-Abscontrol)] / Absblank×100

[0057] The results showed that the UV-visible light absorption intensity decreased after the gel mask solution was added to the DPPH solution. In contrast, when CMC-Na was added to the DPPH solution, the solution color did not change significantly (purple to yellow), and no free radical scavenging effect was observed. The corresponding data showed that the gel mask solution containing 2%-10% SE was able to effectively scavenge 94.79±0.5% of DPPH free radicals. After the gel mask solution was added to the ABTS solution, the solution appeared pink and the free radical scavenging rate was an average of 90.26±0.4%. This result further emphasizes the strong scavenging ability of the gel mask solution containing 2%-10% SE on ABTS free radicals. These results confirm that the samples retain the antioxidant properties of SE to a large extent.

[0058] Test Example 2. Antiseptic and Antibacterial Test of Gel Mask Liquid

[0059] Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were inoculated in 4-5 mL LB medium and cultured overnight in a 37°C bacterial incubator. 100 μL of bacterial suspension (1×106 CFU / mL) was inoculated overnight and evenly spread on the surface of the solid culture medium. A sterile filter paper with a diameter of 6 mm (soaked in gel mask liquid A, B, C, D, E in advance and dried) was placed on a culture dish and cultured at 37°C for 24 hours. Subsequently, a vernier caliper was used to measure the diameter of the inhibition zone (DIZ). The appearance of a transparent ring around the filter paper indicates that bacterial growth is inhibited. This phenomenon is used to evaluate the antibacterial activity of the gel mask liquid of vegetation and whether it has the potential to be used in skin care products.

[0060] The results showed that the prepared gel mask liquid had a strong inhibitory effect on bacteria, and the diameters of the inhibition zones were 27.41±0.4 mm (for Staphylococcus aureus S.aureus) and 33.20±0.6 mm (for Escherichia coli E.coli). These results showed that Staphylococcus aureus (Gram-positive bacteria) was less sensitive to the gel mask liquid than Escherichia coli (Gram-negative bacteria).

[0061] Test Example 3. Biocompatibility test of gel mask liquid

[0062] The hemolytic activity of the prepared gel mask solution was evaluated by a sheep red blood cell experiment. Take 5 mL of fresh and healthy sheep blood, centrifuge at 1200 rpm for 5 minutes, and discard the supernatant. Subsequently, the red blood cells were washed and resuspended with PBS to prepare a 2% red blood cell suspension, which was dispensed into EP tubes. 1 mL of SE gel mask solution of different concentrations (100, 80, 60, 40, 20 mg / mL) was added to each test tube as an experimental group. 0.1% Triton X-100 solution was used as a positive control, and PBS was used as a negative control. After all the mixed solutions were thoroughly mixed, they were incubated at 37°C for 6 hours. After the incubation, the sample was centrifuged, the absorbance was measured at 540 nm, and the hemolysis rate was calculated according to the following formula:

[0063] Hemolysis rate % = (Abspositive-Absnegative) / (Abssample-Absnegative)×100

[0064] The results showed that all tested samples had no significant differences compared with the negative control group, indicating that they would not induce hemoglobin cleavage, thus confirming their good biocompatibility and safety.

[0065] Test Example 4. Cytotoxicity test of gel mask solution

[0066] The cell viability of the prepared gel mask liquid was evaluated by the colorimetric methyl tetrazolium salt (MTT) method to measure the cell metabolic activity. L929 fibroblasts were cultured in DMEM medium containing 10% fetal bovine serum, 50 IU / mL penicillin and 50 IU / mL streptomycin and placed in a 5% CO2 (37°C) environment. Fibroblasts were cultured at 2×10 4 The cells were seeded at a density of 10 cells / well in a 96-well culture plate, and samples with final concentrations of 6.25, 12.5, 25, 50, and 100 μg / mL were added for treatment for 24 hours.

[0067] Subsequently, MTT solution (0.5 mg / mL, prepared in PBS solution) was added to the cells and incubated at 37°C for 4 hours. After removing MTT, 100% dimethyl sulfoxide (DMSO) was added to dissolve the tetrazolium salt crystals, and the absorbance was measured at 570 nm. The experiment was repeated 3 times, and 3 replicate wells were set. Finally, the absorbance of the control group was normalized and calculated as 100% cell viability.

[0068] Cell viability(%)=Abssample / Abscontrol×100

[0069] The results showed that SE and gel mask liquid had a dose-dependent inhibitory effect on the growth of L929 cells. At a concentration of 100 μg / mL, both SE and gel mask liquid showed cytotoxicity, reducing cell viability by 40.06±0.32% and 95.26±1.2%, respectively. However, in the concentration range of 6.25 μg / mL to 50 μg / mL, the gel mask liquid did not inhibit the proliferation of L929 cells, but promoted cell viability. At concentrations of 6.25, 12.5, 25, and 50 μg / mL, its cell viability reached 121.2±2.4%, 109.5±0.5%, and 104.2±4%, respectively. At all tested concentrations, the gel mask liquid did not show significant cytotoxicity to the L929 cell line, further confirming its safety in cosmetic applications.

Claims

1. A plant extract composition, characterized in that Contains the following ingredients: hematoxylin polyphenols, cat's claw polysaccharides, sodium carboxymethyl cellulose, and moisturizer.

2. A plant extract composition according to claim 1, characterized in that: The mass ratio of the hematoxylin polyphenol is 2%-10%, the mass ratio of the cat's claw polysaccharide is 2%-10%, the mass ratio of the mask liquid matrix is ​​0.01%-0.05%, and the mass ratio of the moisturizer is 15%.

3. A plant extract composition according to claim 1, characterized in that: The ratio of the plant extract hematoxylin polyphenols to cat's claw polysaccharide is 1:1, 2:1, or 3:

1.

4. A plant extract composition according to claim 1, characterized in that: The method for preparing hematoxylin polyphenols comprises the following steps: (1) Wash the bark of the sappan wood with clean water, dry it at 60°C, grind it through a sieve with a pore size of 0.21 mm for later use, and sterilize it by irradiation. (2) Ultrasonic alcohol extraction, preferably with an intensity of 100w, 20°C-70°C, a liquid-to-solid ratio of 20-45mL / g, an ethanol volume fraction of 30%-80%, extraction for 10-60min, centrifugation at 6000-12000rpm / min to obtain the supernatant, evaporation and concentration in a vacuum rotary device to remove the organic solvent, the concentrated solutions are combined, and placed in a vacuum freeze dryer for 24h to obtain freeze-dried powder, which is stored at -20°C in the dark for later use.

5. A plant extract composition according to claim 4, characterized in that: The ultrasonic intensity is 100w, the extraction time is 10-30min, the liquid-solid ratio is 30-40mL / g, and the ethanol volume fraction is 50%-70%.

6. A plant extract composition according to claim 1, wherein the preparation method of the cat's claw polysaccharide comprises the following steps: (1) Ultrasonic-assisted water extraction method: clean the cat's claw, dry it at 60°C, crush it and pass it through a 0.21 mm sieve for later use, use 8-10 times the amount of water (mass ratio), ultrasonically heat it at 30°C for 30 min, remove the filter residue, use a rotary evaporator to concentrate, collect the concentrate, perform the same operation twice, and combine the two concentrates; (2) Alcohol precipitation method: Add an appropriate amount of organic solvent to the cat's claw water extract, stir evenly, and place in a refrigerator at 4°C overnight. After centrifugation, concentrate and freeze-dry for later use.

7. A plant extract composition according to any one of claims 1 to 6 and its use in a gel facial mask liquid, characterized in that: The preparation method of the gel mask liquid comprises the following steps: dissolving an appropriate amount of solid sodium carboxymethylcellulose (CMC-Na) in water, adding 2%-10% of cat's claw polysaccharide mucus and 5%-10% of moisturizer at room temperature, adding 0.05%-0.15% of citric acid in the presence of 2%-10% of sappan wood polyphenol extract (SE), and continuously stirring to obtain a uniform gel mask liquid.

8. A plant extract composition according to claim 7 and its use in a gel mask liquid, characterized in that: The facial mask liquid matrix is ​​one or two of sodium carboxymethyl cellulose, chitosan, sodium hyaluronate and xanthan gum.

9. The plant extract composition according to claim 7 and its use in gel mask liquid, characterized in that: The moisturizing agent is one or two of caprylyl glycol, pentylene glycol, propylene glycol and ethylene glycol.