Plant composition for resisting skin inflammatory aging as well as preparation method and application of plant composition
By using the specific mass ratio of alpine azalea and Yunnan Coptis chinensis, combined with microwave-ultrasound combined extraction and macroporous resin purification, plant compositions with anti-inflammatory, antioxidant stress and moisturizing effects were prepared, which solved the problem of skin aging caused by oxidative stress and inflammation, and achieved the effect of delaying skin aging.
Patent Information
- Application Number
- CN202510289189.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-12
- Publication Date
- 2025-06-06
AI Technical Summary
The prior art is difficult to effectively solve the problem of skin aging caused by oxidative stress and inflammation, especially skin aging caused by exogenous factors such as ultraviolet rays, tobacco and environmental pollutants.
Using the specific mass ratio of alpine azalea and Yunnan Coptis chinensis as preparation materials, plant compositions with anti-inflammatory, antioxidant stress, moisturizing and skin elasticity were prepared by microwave-ultrasound combined extraction, decolorization treatment, flocculation treatment and macroporous resin purification enrichment.
This plant composition can effectively inhibit the secretion of inflammatory factors, inhibit ROS generation, increase skin elasticity and improve skin barrier function, thereby delaying skin aging, and is suitable for skin care products and medical auxiliary products.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of plant extracts and relates to a plant composition for resisting skin inflammatory aging and a preparation method and application thereof. Background Art
[0002] Inflammatory aging is used to describe a chronic mild inflammatory state caused by an imbalance between pro-inflammatory and anti-inflammatory responses in the body. This chronic inflammatory state can lead to aging of tissues and organs including the skin. Chronic inflammation that leads to skin aging can also be divided into endogenous chronic inflammatory states of the entire body and exogenous (sun exposure, pollution) oxidative stress and inflammatory states. In a normal human body, there is a homeostasis of the "neuro-immune-endocrine system". Bad living habits, work pressure, negative emotions, etc. can lead to an imbalance in the homeostasis of the "neuro-immune-endocrine system", the direct result of which is an imbalance in the oxidation-antioxidant balance and anti-inflammatory-pro-inflammatory balance in the body, causing the body's tissues and organs (including the skin) to be in a state of chronic oxidation and chronic inflammation.
[0003] The oxidative-inflammatory state caused by ultraviolet rays, tobacco, and environmental pollutants plays a major role in skin aging, especially for those with premature skin aging. Skin inflammatory aging caused by exogenous factors can be indirectly mediated by reactive oxygen species (ROS) or directly induced by ultraviolet rays to induce proinflammatory cytokines, which in turn affect fibroblast function and lead to reduced collagen synthesis and increased degradation. The mechanism of skin aging shows that skin aging directly or indirectly mediated by oxidative stress is dominant. Studies have shown that oxidative stress is closely related to inflammation and is also a key factor leading to skin aging.
[0004] Oxidative damage to cells by ROS triggers the release of TNF-α, which binds to cell surface receptors to activate the NF-κB signaling pathway, leading to overexpression of other inflammatory factors, upregulation of vascular endothelial growth factor and proinflammatory cytokines (IL-1, IL-6, and TNF-α), and the occurrence of chronic inflammatory reactions. Chronic inflammation further accelerates the oxidative stress response, and more ROS stimulate cells to synthesize a large number of matrix metalloproteinases (MMPs), degrading collagen and elastin, the most important extracellular matrix (ECM) in the dermis, causing damage to the dermis connective tissue structure, leading to aging manifestations such as skin wrinkles, sagging, and sagging.
[0005] Rhododendron is one of the eight famous flowers in Yunnan and the flower of the Yi people. It is used as a Yi medicine to treat injuries from falls, neurasthenia, bites, and hemostasis. Rhododendron alpinum is an evergreen shrub of the genus Rhododendron in the family Ericaceae. In addition to its colorful ornamental value, it also has the medicinal effects of promoting blood circulation and removing rheumatism. Most of them grow at an altitude of 2,500 to 4,000 meters. The leaves, roots, and flowers of Rhododendron alpinum can be used as medicine, which has anesthetic and sedative effects and can treat symptoms such as chronic tracheitis, cough with sputum, and cough and asthma.
[0006] Yunnan Coptis chinensis is a perennial herbaceous plant of the Ranunculaceae family and the genus Coptis. It is distributed in northwest Yunnan and southeast Tibet in China. It grows in the shade of cold and humid mountains at an altitude of 1500-2300 meters. It is wild or sometimes cultivated. The "Southern Yunnan Materia Medica" of the Ming Dynasty states: "Yunnan Coptis chinensis, also known as Yunlian, is not well known. It grows in the mountains. It looks like Plantain, has small seeds, and yellow roots that are connected into strips. This Coptis chinensis is a hundred times more effective than Sichuan Coptis chinensis. It has a bitter and cold smell and is non-toxic.
[0007] At present, it is very meaningful to develop more functions of Rhododendron australis or Coptis chinensis Yunnanensis. Summary of the invention
[0008] In view of the deficiencies in the prior art, the object of the present invention is to provide a plant composition for resisting skin inflammatory aging, and a preparation method and application thereof.
[0009] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:
[0010] In a first aspect, the present invention provides a plant composition for resisting skin inflammatory aging, characterized in that the raw materials for preparing the plant composition include alpine rhododendron and Yunnan coptis chinensis, and the mass ratio thereof is 1:(25-250).
[0011] The present invention develops a brand-new plant-based product with anti-skin inflammatory aging efficacy. The product is prepared from two specific plants, namely, alpine azalea and Yunnan coptis chinensis, which are matched with each other in a specific mass ratio to achieve synergistic effects. The plant composition has excellent functions of inhibiting the secretion of inflammatory factors, inhibiting the generation of ROS, increasing skin elasticity, improving skin barrier and the like, thereby having the efficacy of delaying skin aging. The plant composition can be used as an active ingredient in skin care products and medical auxiliary products to play the roles of anti-inflammatory, anti-oxidative stress, moisturizing, increasing skin elasticity and anti-aging.
[0012] The mass ratio of the alpine rhododendron to Yunnan coptis is 1:(25-250), for example 1:25, 1:50, 1:80, 1:100, 1:120, 1:140, 1:160, 1:180, 1:200, 1:220, 1:230, 1:250, etc.
[0013] In a second aspect, the present invention provides a method for preparing the plant composition according to the first aspect, the preparation method comprising the following steps:
[0014] (1) mixing the raw materials for preparing the plant composition with an ethanol aqueous solution, performing microwave-ultrasonic combined extraction, and performing solid-liquid separation to obtain an extract;
[0015] (2) concentrating the extract and then decolorizing it to obtain a decolorized solution;
[0016] (3) flocculating the decolorized liquid, separating the solid from the liquid, and obtaining a filtrate;
[0017] (4) Purifying and eluting the filtrate with a macroporous resin, collecting the eluate, concentrating and drying it to obtain the plant composition.
[0018] The plant composition involved in the present invention uses alpine azalea and Yunnan coptis root as raw materials for preparation, adopts microwave-ultrasound combined assisted alcohol extraction, decolorization treatment, flocculation treatment, and combined with macroporous resin purification and enrichment, and the alpine azalea and Yunnan coptis root cooperate with each other to enhance synergy. The plant composition has excellent functions of inhibiting the secretion of inflammatory factors, inhibiting the generation of ROS, increasing skin elasticity, improving skin barrier, etc., and thus has the effect of delaying skin aging. It can be used as an active ingredient of skin care products and medical auxiliary products, and has the effects of anti-inflammatory, anti-oxidative stress, moisturizing, increasing skin elasticity, and anti-aging.
[0019] Preferably, the volume fraction of the ethanol aqueous solution is 60-80%, for example, 60%, 63%, 65%, 68%, 70%, 72%, 75%, 78%, 80% and the like.
[0020] Compared with ethanol aqueous solutions of other concentrations, 60-80% ethanol aqueous solution is selected as the hot extraction solvent, and the final product is better in inhibiting the secretion of inflammatory factors, inhibiting the generation of ROS, increasing skin elasticity, and improving skin barrier function.
[0021] Preferably, the solid-liquid ratio of the preparation raw material to the ethanol aqueous solution is 1:(6-10) g / mL, for example 1:6 g / mL, 1:7 g / mL, 1:8 g / mL, 1:9 g / mL, 1:10 g / mL, etc.
[0022] Preferably, the extraction is carried out at 55-75°C (e.g., 55°C, 58°C, 60°C, 63°C, 65°C, 68°C, 70°C, 75°C, etc.) for 1-3 times (e.g., 1 time, 2 times or 3 times), each time for 20-40 min (e.g., 20 min, 25 min, 30 min, 35 min, 40 min, etc.).
[0023] Preferably, in the microwave-ultrasonic combined extraction, the power of the microwave is 100-400 W, for example, 100 W, 150 W, 200 W, 250 W, 300 W, 350 W, 400 W, etc.; the power of the ultrasound is 80-120 W, for example, 80 W, 90 W, 100 W, 110 W, 120 W, etc.
[0024] The present invention creatively finds that when performing microwave-ultrasonic combined treatment, using a microwave power of 100-400W and an ultrasonic power of 80-120W can effectively improve the above-mentioned efficacy of the plant composition compared with other powers. Increasing the microwave power can increase the temperature inside the plant cells and accelerate the rupture of the cell walls, but too high a power will lead to too fast a heating speed, thereby causing thermal damage or side reactions, thereby affecting the effect of the extracted product; increasing the ultrasonic power will enhance the cavitation effect generated by ultrasound, but too high an ultrasonic power will produce a buffering effect, reduce the rate of energy transfer and cause the cavitation effect to weaken, and may also cause degradation or isomerization of the active ingredients, thereby affecting the effect of the extracted product.
[0025] Preferably, the extract is concentrated to 1-3 times the mass of the feed amount, for example, 1 time, 1.3 times, 1.5 times, 1.8 times, 2 times, 2.5 times, 3 times, etc.
[0026] Preferably, the decolorization treatment uses activated carbon in an amount of 1-5% of the mass of the concentrated liquid, such as 1%, 2%, 3%, 4%, 5%, etc.
[0027] Preferably, the flocculation treatment uses a flocculant, which includes any one or a combination of at least two of water-soluble polysaccharides, cationic chitosan, guar gum, protein colloid, gelatin, animal glue, cationic starch or tannin.
[0028] The flocculant is pretreated as follows before use: the flocculant is first mixed and stirred in a small amount of acetic acid aqueous solution to a paste, and then mixed with water to swell.
[0029] Preferably, the flocculant comprises a combination of cationic chitosan and gelatin.
[0030] The flocculant treatment with a specific composition in the preparation method of the present invention can remove inactive impurities, so that the composition of the treated product is significantly improved in terms of inhibiting the secretion of inflammatory factors, inhibiting the generation of ROS, increasing skin elasticity, and improving skin barrier function.
[0031] Preferably, the mass ratio of the cationic chitosan to gelatin is (2-4):1, for example, 2:1, 2.5:1, 2.8:1, 3:1, 3.2:1, 3.5:1, 4:1, etc.
[0032] Preferably, the macroporous resin is selected from any one of D101, HP20, X-5, AB-8, HPD100, DM301 or NKA-9, or a combination of at least two thereof.
[0033] Preferably, the macroporous resin is a mixture of D101 and DM301.
[0034] Furthermore, the present invention creatively discovered that a mixed resin of D101 and DM301 is used to purify the extracted product. Compared with other types of resin combinations or single resins, D101 and DM301 can work synergistically, and the separated and purified final product is better in inhibiting the secretion of inflammatory factors, inhibiting the generation of ROS, increasing skin elasticity, and improving skin barrier function.
[0035] Preferably, the mass ratio of D101 to DM301 is (3-5):1, for example, 3:1, 3.5:1, 3.8:1, 4:1, 4.3:1, 4.5:1, 5:1, etc.
[0036] Based on the synergistic relationship between D101 resin and DM301 resin, when the two satisfy the above-mentioned specific mass ratio relationship, the final product of separation and purification is better in the above-mentioned efficacy.
[0037] Preferably, the purification and elution process is: first eluting with pure water or 0-10% ethanol aqueous solution, then eluting with 50-65% ethanol aqueous solution, and collecting the alcohol washing liquid;
[0038] Preferably, the purification and elution process is: firstly eluting with 1-5BV of pure water or 0-10% ethanol aqueous solution at 1-3BV / h, then eluting with 1-5BV of 50-65% ethanol aqueous solution at 1-3BV / h, and collecting the alcohol washing liquid.
[0039] The specific point values in the 1-5BV can be selected as 1BV, 2BV, 3BV, 4BV, 5BV, etc.; the specific point values in the 0-10% can be selected as 1%, 3%, 4%, 5%, 8%, 10%, etc.; the specific point values in the 50-65% can be selected as 50%, 53%, 55%, 58%, 60%, 65%, etc.; the specific point values in the 1-3BV / h can be selected as 1BV / h, 1.5BV / h, 2BV / h, 2.5BV / h, 3BV / h, etc.
[0040] In a third aspect, the present invention provides an application of the plant composition according to the first aspect or the method for preparing the plant composition according to the second aspect in preparing a product having any one or a combination of at least two of the following effects:
[0041] 1) Anti-inflammatory; 2) Anti-oxidative stress; 3) Moisturizing; 4) Increase skin elasticity; 5) Anti-aging.
[0042] Preferably, the mass percentage of the plant composition in the product is 0.1-5%, for example 0.1%, 0.5%, 0.8%, 1%, 1.5%, 2%, 3%, 4%, 5% and the like.
[0043] Preferably, the product comprises a cosmetic or a medical auxiliary product.
[0044] Preferably, the cosmetics include essence, lotion, emulsion, cream, mask or cleanser.
[0045] Other specific point values within the above numerical ranges can be selected and are all within the protection scope of the present invention. Considering the length of the article and the brevity of the expression, they will not be described one by one here.
[0046] Compared with the prior art, the present invention has the following beneficial effects:
[0047] The present invention develops a new plant-based product with anti-skin inflammatory aging effect, which uses two specific plants, alpine azalea and Yunnan coptis, as raw materials, adopts microwave-ultrasound combined assisted alcohol extraction, decolorization treatment, flocculation treatment, and combined with macroporous resin purification and enrichment. Alpine azalea and Yunnan coptis cooperate with each other and can synergize. The prepared product has excellent functions of inhibiting the secretion of inflammatory factors, inhibiting the generation of ROS, increasing skin elasticity, improving skin barrier, etc., so as to delay skin aging. It can be used as an active ingredient of skin care products and medical auxiliary products, and plays the role of anti-inflammatory, anti-oxidative stress, moisturizing, increasing skin elasticity, and anti-aging. DETAILED DESCRIPTION
[0048] In order to further explain the technical means and effects adopted by the present invention, the technical solution of the present invention is further described below in conjunction with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.
[0049] The sources of some raw materials involved in the following examples are as follows:
[0050] Cationic chitosan was purchased from Shanghai Yuanye Biotechnology Co., Ltd. with model number S28548-100g;
[0051] Gelatin was purchased from Shanghai Yuanye Biotechnology Co., Ltd. with model number S30952-100g.
[0052] Example 1
[0053] This embodiment provides a plant composition, and the preparation method thereof is as follows:
[0054] (1) 1 kg of plant raw material was crushed and passed through an 80-mesh sieve, and then mixed with a 70% ethanol aqueous solution at a solid-liquid ratio of 1:8 g / mL, and subjected to microwave-ultrasonic combined extraction at 65° C. The extraction time was 30 min, the microwave power was 200 W, and the ultrasonic power was 90 W; solid-liquid separation was performed to obtain an extract; the above extraction operation was repeated once on the residue, and the two extracts were combined; the plant raw material was alpine azalea and Yunnan coptis root at a mass ratio of 1:25;
[0055] (2) the extract is concentrated to 1 times the amount of the feed, and then activated carbon is added at 5% by mass of the concentrate for decolorization to obtain a decolorized solution;
[0056] (3) The decolorized liquid was mixed with 1.5% flocculant (cationic chitosan and gelatin in a mass ratio of 3:1 were first mixed with 3 times the mass of 1% acetic acid aqueous solution and stirred to a paste, and then mixed with 70 times the mass of water and swollen for 24 hours) for flocculation treatment, centrifuged at 2000 rpm for 30 minutes, and filtered to obtain a filtrate;
[0057] (4) The filtrate is purified and eluted with a macroporous resin, wherein the macroporous resin is a mixture of D101 and DM301 in a mass ratio of 4:1; the purification and elution process is: first eluting with 2BV of pure water at 1.5BV / h, then eluting with 2BV of 65% ethanol aqueous solution at 1.5BV / h, collecting the alcohol washings, concentrating, and drying to obtain the plant composition.
[0058] Example 2
[0059] This embodiment provides a plant composition, and the preparation method thereof is as follows:
[0060] (1) 1 kg of plant raw material was crushed and passed through a 60-mesh sieve, and then mixed with 80% ethanol aqueous solution at a solid-liquid ratio of 1:10 g / mL, and subjected to microwave-ultrasonic combined extraction at 75° C. The extraction time was 20 min, the microwave power was 150 W, and the ultrasonic power was 110 W; solid-liquid separation was performed to obtain an extract; the above extraction operation was repeated once on the residue, and the two extracts were combined; the plant raw material was alpine azalea and Yunnan coptis root at a mass ratio of 1:50;
[0061] (2) the extract is concentrated to 1 times the amount of the feed, and then 3% of the weight of the concentrate is added with activated carbon for decolorization to obtain a decolorized solution;
[0062] (3) The decolorized liquid was mixed with 1.5% flocculant (cationic chitosan and gelatin in a mass ratio of 4:1 were first mixed with 3 times the mass of 1% acetic acid aqueous solution and stirred to a paste, and then mixed with 70 times the mass of water and swollen for 24 hours) for flocculation treatment, centrifuged at 2000 rpm for 30 minutes, and filtered to obtain a filtrate;
[0063] (4) The filtrate is purified and eluted with a macroporous resin, wherein the macroporous resin is a mixture of D101 and DM301 in a mass ratio of 5:1; the purification and elution process is: first eluting with 4BV of pure water at 3BV / h, then eluting with 4BV of 55% ethanol aqueous solution at 3BV / h, collecting the alcohol washings, concentrating, and drying to obtain the plant composition.
[0064] Example 3
[0065] This embodiment provides a plant composition, and the preparation method thereof is as follows:
[0066] (1) 1 kg of plant raw material was crushed and passed through a 60-mesh sieve, and then mixed with a 60% ethanol aqueous solution at a solid-liquid ratio of 1:6 g / mL, and subjected to microwave-ultrasonic combined extraction at 55° C. The extraction time was 40 min, the microwave power was 250 W, and the ultrasonic power was 80 W; solid-liquid separation was performed to obtain an extract; the above extraction operation was repeated once on the residue, and the two extracts were combined; the plant raw material was alpine azalea and Yunnan coptis root at a mass ratio of 1:200;
[0067] (2) the extract is concentrated to 1 times the amount of the feed, and then 4% of the weight of the concentrate is added with activated carbon for decolorization to obtain a decolorized solution;
[0068] (3) The decolorized liquid was mixed with 1.5% flocculant (cationic chitosan and gelatin in a mass ratio of 2:1 were first mixed with 3 times the mass of 1% acetic acid aqueous solution and stirred to a paste, and then mixed with 70 times the mass of water and swollen for 24 hours) for flocculation treatment, centrifuged at 2000 rpm for 30 minutes, and filtered to obtain a filtrate;
[0069] (4) The filtrate is purified and eluted with a macroporous resin, wherein the macroporous resin is a mixture of D101 and DM301 in a mass ratio of 3:1; the purification and elution process is: first eluting with 3BV of pure water at 2BV / h, then eluting with 3BV of 60% ethanol aqueous solution at 2BV / h, collecting the alcohol washing liquid, concentrating it, and drying it to obtain the plant composition.
[0070] Example 4
[0071] This embodiment provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that: the macroporous resin in step (4) is a mixture of AB-8 and DM301 in a mass ratio of 4:1; other operations and parameters are consistent with those of Example 1.
[0072] Example 5
[0073] This embodiment provides a plant composition, and the preparation method thereof is different from that of embodiment 1 only in that the macroporous resin in step (4) is a single D101 resin; other operations and parameters are consistent with those of embodiment 1.
[0074] Example 6
[0075] This embodiment provides a plant composition, and the preparation method thereof is different from that of Embodiment 1 only in that the macroporous resin in step (4) is a single DM301 resin; and other operations and parameters are consistent with those of Embodiment 1.
[0076] Example 7
[0077] This embodiment provides a plant composition, and the preparation method thereof is different from that of Embodiment 1 only in that: in step (3), the cationic chitosan and gelatin in a mass ratio of 3:1 are replaced with a single cationic chitosan; other operations and parameters are consistent with those of Embodiment 1.
[0078] Example 8
[0079] This embodiment provides a plant composition, and the preparation method thereof is different from that of Embodiment 1 only in that: in step (3), the cationic chitosan and gelatin in a mass ratio of 3:1 are replaced with single gelatin; other operations and parameters are consistent with those of Embodiment 1.
[0080] Comparative Example 1
[0081] This comparative example provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that the plant raw material in step (1) is 1 kg of alpine azalea; and the other operations and parameters are consistent with those of Example 1.
[0082] Comparative Example 2
[0083] This comparative example provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that the plant raw material in step (1) is 1 kg of Coptis chinensis; other operations and parameters are consistent with those of Example 1.
[0084] Comparative Example 3
[0085] This comparative example provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that the method of obtaining the extract in step (1) is different, and the operations of the other steps remain the same, as follows:
[0086] (S1) grinding the alpine azalea flowers through an 80-mesh sieve and mixing with a 70% ethanol aqueous solution at a solid-liquid ratio of 1:8 g / mL, performing microwave-ultrasonic combined extraction at 65° C., the extraction time is 30 min, the microwave power is 200 W, and the ultrasonic power is 90 W; solid-liquid separation is performed to obtain an extract; the above extraction operation is repeated once on the filter residue, and the two extracts are combined to obtain an alpine azalea flower extract;
[0087] (S2) crushing the Yunnan coptis root through an 80-mesh sieve and mixing it with a 70% ethanol aqueous solution at a solid-liquid ratio of 1:8 g / mL, performing microwave-ultrasonic combined extraction at 65° C., the extraction time is 30 min, the microwave power is 200 W, and the ultrasonic power is 90 W; solid-liquid separation is performed to obtain an extract; the above extraction operation is repeated once on the filter residue, and the two extracts are combined to obtain a Yunnan coptis root extract;
[0088] The mass ratio of alpine rhododendron and Yunnan coptis is 1:25, and the total amount is 1kg.
[0089] (S3) combining the alpine azalea extract and the Yunnan coptis extract to obtain.
[0090] Comparative Example 4
[0091] This comparative example provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that the extraction method of step (1) is different, and the operations of other steps remain the same, as follows:
[0092] 1 kg of plant raw materials was crushed and passed through an 80-mesh sieve, then mixed with a 70% ethanol aqueous solution at a solid-liquid ratio of 1:8 g / mL, and microwave extraction was performed at 65°C for 40 min with a microwave power of 300 W. Solid-liquid separation was performed to obtain an extract; the above extraction operation was repeated once on the residue, and the two extracts were combined; the plant raw materials were alpine azalea and coptis yunnanensis in a mass ratio of 1:25.
[0093] Comparative Example 5
[0094] This comparative example provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that the extraction method of step (1) is different, and the operations of other steps remain the same, as follows:
[0095] 1 kg of plant raw materials was crushed and passed through an 80-mesh sieve, then mixed with a 70% ethanol aqueous solution at a solid-liquid ratio of 1:8 g / mL, and ultrasonic extraction was performed at 65°C for 40 minutes with an ultrasonic power of 120 W. Solid-liquid separation was performed to obtain an extract; the above extraction operation was repeated once on the residue, and the two extracts were combined; the plant raw materials were alpine azalea and coptis yunnanensis in a mass ratio of 1:25.
[0096] Comparative Example 6
[0097] This comparative example provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that no flocculation treatment is performed in step (3), and the operations of other steps remain the same, specifically: the decolorized liquid of step (2) is directly subjected to step (4) treatment to obtain the plant composition.
[0098] Comparative Example 7
[0099] This comparative example provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that: the plant raw materials described in step (1) are Rhododendron azalea and Coptis yunnanensis in a mass ratio of 1:10; other operations and parameters are consistent with those of Example 1.
[0100] Comparative Example 8
[0101] This comparative example provides a plant composition, and the preparation method thereof is different from that of Example 1 only in that the plant raw materials described in step (1) are Rhododendron australis and Coptis chinensis in a mass ratio of 2:1; other operations and parameters are consistent with those of Example 1.
[0102] Test Example 1
[0103] ROS inhibition assay:
[0104] (1) Configuration of the sample to be tested:
[0105] The plant compositions prepared in Examples 1-8 and Comparative Examples 1-8 were prepared into sample solutions with a concentration of 5 mg / mL using distilled water as a solvent.
[0106] (2) Adjust the density of Hacat cell suspension to 1×10 5 Cells were inoculated into 24-well plates at a volume of 200 μL per well and placed back into the incubator for incubation (37°C, 5% CO 2 After 24 hours, the 24-well plate was removed, the old culture medium was discarded, and samples were added to each group. 1 mL of basal culture medium was added to each well of the blank control group and the model group, and 1 mL of the corresponding concentration sample was added to each well of the experimental group. Then the plates were returned to the incubator for culture (37°C, 5% CO 2 ). After 24 hours, the 24-well plate was taken out and the model group and the experimental group were treated with 50mJ / m 2 The blank control group was not irradiated and the incubator (37°C, 5% CO 2 , 95% relative humidity) for 30 min.
[0107] (3) After the cell culture supernatant was removed by aspiration, the cells were washed with PBS, and 200 μL of the probe DCFH-DA was added to each well, and the cells were incubated in a cell culture incubator at 37°C for 30 min. The DCFH-DA solution was discarded, and the cells were washed with PBS for 3 times. The cells were digested with trypsin and collected into a 2 ml centrifuge tube, and centrifuged at 2500 rpm for 10 min. The supernatant was discarded, and 300 μL of PBS was added to each well to resuspend the cells. The cell resuspension solution was added to a 96-well plate at a rate of 200 μL per well, and the fluorescence intensity was detected by a fluorescence microplate reader (incident light wavelength 525 nm, excitation light wavelength 488 nm). The results are shown in Table 1.
[0108] Test Example 2
[0109] Inflammatory factor inhibition test:
[0110] (1) Configuration of the sample to be tested:
[0111] The plant compositions prepared in Examples 1-8 and Comparative Examples 1-8 were prepared into sample solutions with a concentration of 5 mg / mL using distilled water as a solvent.
[0112] (2) LPS-induced mouse macrophage RAW264.7 was used as an inflammatory model, and a blank control group was set up. The specific operation was as follows: RAW264.7 cells were cultured normally in RPMI1640 medium containing 10% fetal bovine serum (FBS) under the conditions of 5% carbon dioxide and 37°C. RAW264.7 cells in the best growth state were taken, and the cell suspension density was adjusted to 8×10 4 100 μL of cell suspension was inoculated into each well of a 96-well plate and placed at 37°C and 5% CO 2 Incubator culture. Then each group was intervened, where the sample group: added 1μg / ml LPS and each group of test sample solutions; model group: added 1μg / ml LPS and an equal volume of cell culture medium; blank control group: added an equal volume of cell culture medium. After 24 hours of culture, the supernatant was taken and the level of interleukin 6 (IL-6) (pg / mL) was detected by ELISA. The results are shown in Table 1.
[0113] Table 1
[0114]
[0115]
[0116] It can be seen from the data results in Table 1 that, compared with the comparative example, the plant composition involved in the present invention uses alpine azalea and Yunnan coptis chinensis in a specific mass ratio as raw materials for preparation, and adopts microwave-ultrasound combined assisted alcohol extraction, decolorization treatment, macroporous resin purification and enrichment, and combined with flocculation treatment. It has excellent antioxidant stress and anti-inflammatory effects, and the formula of the flocculant and the formula of the macroporous resin also affect the antioxidant stress and anti-inflammatory effects of the product to a certain extent.
[0117] Test Example 3
[0118] Human efficacy evaluation test:
[0119] (1) Configuration of the sample to be tested:
[0120] Emulsion products containing 0.5% of the plant composition of Examples 1-8 and Comparative Examples 1-8 were prepared, and the formula consisted of the following components: 0.5% of the plant composition, 2% of dipropylene glycol, 2% of inositol, 4% of glycerol, 1% of potassium cetyl phosphate, 1% of polysorbate-20, 0.5% of squalane, 0.3% of white meadowfoam seed oil, 0.3% of avocado butter, and the balance was water.
[0121] The preparation method is as follows: water and an alcohol solvent are mixed in an aqueous phase pot, heated to 70°C, kept warm for 25 minutes, cooled to 35°C, and then mixed with the plant composition to obtain an aqueous phase mixture; an emulsifier and an emollient are mixed in an emulsifying pot, homogenized at 2000 rpm for 5 minutes, and then mixed with the aqueous phase mixture, and homogenized at 2000 rpm for 5 minutes to obtain a test emulsion, and a blank product of the same formula without the plant composition is used as a blank control emulsion.
[0122] (2) 160 women were selected as subjects and divided into 16 groups, with 10 people in each group. A half-face control test was conducted at the same time. The test lotion was used on the entire half of the face according to the usage requirements, and the blank control lotion was used on the other half of the face. The lotion was applied once a day for 28 consecutive days, including data collection on both sides of the face on the 0th day (before use), 14 consecutive days, and 28 consecutive days. The degree of improvement of each skin condition was analyzed.
[0123] (3) Skin elasticity test:
[0124] Before the test, the subjects cleaned their faces, air-dried them, and marked the measurement areas. Before the test, they sat quietly in a standard room for at least 30 minutes, could not drink water, and kept relaxed. The skin elasticity instrument Cutometer MPA580 was used to collect data when not in use, at the 0th, 2nd week, and 4th week. The test site was the zygomatic region. During the measurement, the probe repeated the measurement 3 times in the same test area and took the average value. The test parameter is R2 (the ratio of the skin's rebound amount Ua when there is no negative pressure to the maximum stretch amount Uf when there is negative pressure). The closer R2 is to 1, the better the skin's elasticity. The test results are shown in Table 2.
[0125] Table 2
[0126]
[0127]
[0128] It can be seen from the data results in Table 2 that, compared with the comparative example, the plant composition involved in the present invention uses alpine azalea and Yunnan coptis chinensis in a specific mass ratio as raw materials for preparation, and adopts microwave-ultrasound combined assisted alcohol extraction, decolorization treatment, macroporous resin purification and enrichment, and combined with flocculation treatment. It has an excellent effect of increasing skin elasticity, and the formula of the flocculant and the formula of the macroporous resin also affect the above-mentioned effects of the product to a certain extent.
[0129] (4) Moisturizing effect test:
[0130] Before the test, the subject cleans the face, air-dries it, and marks the measurement area. Before the test, sit quietly in a standard room for at least 30 minutes, do not drink water, and stay relaxed. Use the probe Corneometer CM825 to measure the skin moisture content of the test area and the control area. Each area is measured three times in parallel and the average value is taken. First measure the blank value M of each test area 0 , used for 28 consecutive days, and tested the skin's moisture content on the 14th and 28th days 1 , the test of the same subject was completed by the same measurement personnel. The increase in skin moisture content in each time period was calculated. The test results are shown in Table 3.
[0131] Table 3
[0132]
[0133]
[0134] It can be seen from the data results in Table 3 that, compared with the comparative example, the plant composition involved in the present invention is prepared by using alpine azalea and Yunnan coptis chinensis in a specific mass ratio as raw materials, and adopts microwave-ultrasonic combined assisted alcohol extraction, decolorization treatment, flocculation treatment, and combined with macroporous resin purification and enrichment. It has excellent skin moisturizing effect, and the formula of the flocculant and the formula of the macroporous resin also affect the above-mentioned effects of the product to a certain extent.
[0135] The applicant declares that the present invention illustrates the technical solution of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.
[0136] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.
[0137] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.
Claims
1. A plant composition for resisting skin inflammatory aging, characterized in that: The raw materials for preparing the plant composition include alpine azalea and Yunnan coptis root, and the mass ratio thereof is 1:(25-250).
2. A method for preparing the plant composition according to claim 1, characterized in that: The preparation method comprises the following steps: (1) mixing the raw materials for preparing the plant composition with an ethanol aqueous solution, performing microwave-ultrasonic combined extraction, and performing solid-liquid separation to obtain an extract; (2) concentrating the extract and then decolorizing it to obtain a decolorized solution; (3) flocculating the decolorized liquid, separating the solid from the liquid, and obtaining a filtrate; (4) Purifying and eluting the filtrate with a macroporous resin, collecting the eluate, concentrating and drying it to obtain the plant composition.
3. The preparation method according to claim 2, characterized in that: The volume fraction of the ethanol aqueous solution is 60-80%; Preferably, the solid-liquid ratio of the preparation raw material to the ethanol aqueous solution is 1:(6-10) g / mL.
4. The preparation method according to claim 2, characterized in that: The extraction is performed at 55-75° C. for 1-3 times, each time for 20-40 minutes; Preferably, in the microwave-ultrasonic combined extraction, the power of the microwave is 100-400W, and the power of the ultrasound is 80-120W.
5. The preparation method according to claim 2, characterized in that: The extract is concentrated to 1-3 times the mass of the feed amount; Preferably, the decolorization treatment uses activated carbon in an amount of 1-5% of the mass of the concentrated liquid.
6. The preparation method according to claim 2, characterized in that: The flocculation treatment uses a flocculant, which includes any one or a combination of at least two of water-soluble polysaccharides, cationic chitosan, guar gum, protein colloid, gelatin, animal glue, cationic starch or tannin; Preferably, the flocculant comprises a combination of cationic chitosan and gelatin; Preferably, the mass ratio of the cationic chitosan to gelatin is (2-4):
1.
7. The preparation method according to claim 2, characterized in that: The macroporous resin is selected from any one of D101, HP20, X-5, AB-8, HPD100, DM301 or NKA-9, or a combination of at least two thereof; Preferably, the macroporous resin is a mixture of D101 and DM301; Preferably, the mass ratio of D101 to DM301 is (3-5):
1.
8. The preparation method according to claim 2, characterized in that: The purification and elution process is: first eluting with pure water or 0-10% ethanol aqueous solution, then eluting with 50-65% ethanol aqueous solution, and collecting the alcohol washing liquid; Preferably, the purification and elution process is: firstly eluting with 1-5BV of pure water or 0-10% ethanol aqueous solution at 1-3BV / h, then eluting with 1-5BV of 50-65% ethanol aqueous solution at 1-3BV / h, and collecting the alcohol washing liquid.
9. Use of the plant composition according to claim 1 or the preparation method according to any one of claims 2 to 8 in preparing a product having any one or at least two of the following effects; 1) Anti-inflammatory; 2) Anti-oxidative stress; 3) Moisturizing; 4) Increase skin elasticity; 5) Anti-aging.
10. The use according to claim 9, characterized in that: The mass percentage of the plant composition in the product is 0.1-5%; Preferably, the product includes cosmetics or medical auxiliary products; Preferably, the cosmetics include essence, lotion, emulsion, cream, mask or cleanser.