Composition with effects of shrinking pores and tightening skin as well as preparation method and application of composition

Abstract

The invention relates to a composition with effects of shrinking pores and tightening skin as well as a preparation method and application of the composition. The composition is prepared from the following components in parts by weight: 1 to 4 parts of camellia flower extract, 1 to 4 parts of camellia leaf extract and 0.2 to 2 parts of lotus corniculatus seed extract. The invention accidentally finds that the camellia leaf extract can control inflammation and grease secretion by inhibiting an inflammation signal factor NF-kappa B and down-regulating sterol regulatory element binding protein SREBP-1, so that the camellia leaf extract is combined with the camellia flower extract and the lotus corniculatus seed extract to synergistically shrink pores and tighten skin through a plurality of pathways, and the effects of diminishing inflammation, diminishing inflammation and diminishing inflammation can be achieved through the combination of the camellia leaf extract, the camellia flower extract and the lotus corniculatus seed extract. The problem of coarse facial pores is improved. Meanwhile, by optimizing the extraction process of the camellia flower extract and the lotus corniculatus seed extract, the content and activity of various active ingredients are improved, and therefore the pore shrinking effect is further improved.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, and relates to a composition with the effects of shrinking pores and tightening skin, its preparation method and application. Background Technology

[0002] Pores are tiny openings on the skin's surface that allow gas or liquid to pass through. These openings are formed by the tiny openings of sweat glands or hair follicle sebaceous glands. Visible pores are commonly seen on the nose, cheeks, and forehead. While enlarged pores may seem like a harmless skin condition, this problem not only affects global perceptions of skin aesthetics and quality but also serves as a clear sign of skin aging. Therefore, numerous effective ingredients, skincare products, and beauty methods targeting the shrinking of pores or the improvement of enlarged facial pores have emerged on the market.

[0003] Enlarged pores are caused by a variety of factors. Current research indicates that factors such as sebum secretion, abnormal keratinization, genetic predisposition, UV exposure, acne, and aging are all related to changes in pores. Among these, excessive sebum secretion is one of the common causes of enlarged pores. Excessive sebum accumulation at the hair follicle opening can easily stretch the pores. Abnormal keratinization can cause keratinocytes to accumulate at the pore opening, forming keratin plugs that block the pores and enlarge them. Genetic predisposition means that some people are born with larger pores. UV exposure can damage skin collagen and elastin fibers, leading to skin laxity and enlarged pores. When acne occurs, Propionibacterium acnes proliferates in large numbers within the hair follicles, causing inflammation. After the inflammation subsides, enlarged pores may remain. Inflammatory factors are also one of the causes of excessive sebum secretion, creating a vicious cycle of inflammation and excessive sebum secretion. Aging slows down skin metabolism, causing pores to gradually lose elasticity and enlarge.

[0004] Currently, common methods for improving enlarged pores on the market mainly include using skincare products such as astringents and serums. These products often contain ingredients like alcohol and menthol, which utilize their volatility to remove heat from the skin's surface, thus temporarily shrinking pores. However, this effect is often short-lived and cannot fundamentally improve the problem of enlarged pores. Additionally, some methods use chemical exfoliation or physical scrubs to remove dead skin cells and promote cell renewal, aiming to shrink pores. However, these methods may irritate the skin, even causing sensitivity or inflammation, and long-term use is not beneficial to skin health. Regarding active ingredients, some existing technologies use natural plant extracts or bioactive components to improve enlarged pores. However, these ingredients and compositions often target pores caused by excessive sebum secretion, offering only a single effect and failing to comprehensively address the root cause of enlarged pores. Therefore, analyzing the multiple factors causing enlarged pores and developing a multi-effect composition for shrinking and improving facial pores has become a technical problem to be solved in this field. Summary of the Invention

[0005] To solve the above-mentioned technical problems, the present invention provides a composition with the effect of shrinking pores and tightening skin, as well as its preparation method and application.

[0006] Firstly, this invention provides a plant-based composition that can synergistically target multiple points to shrink pores and tighten skin, improving the problem of enlarged facial pores. This composition is suitable for people with enlarged facial pores, addressing the technical problem of existing technologies that do not simultaneously target the following: loss of dermal collagen and elastin leading to collapsed skin around hair follicles and prominent pores; abnormal proliferation of epidermal keratinocytes easily forming keratin plugs that block and enlarge pores; and inflammation and skin's water-oil imbalance leading to excessive sebum secretion that passively dilates the opening of the hair follicle duct (dry skin leads to compensatory excessive sebum secretion, which passively dilates the opening of the hair follicle duct, forming enlarged pores; inflammatory factors can make sebaceous gland cells more active and secrete more sebum). This invention provides a multi-effect composition suitable for skincare of people with enlarged facial pores.

[0007] Secondly, the present invention provides a method for preparing a plant composition, which, through a reasonable ratio of plant extracts, synergistically and effectively improves the problem of enlarged pores on the face.

[0008] Thirdly, the present invention provides an application of a composition with the effect of shrinking pores and tightening skin, which is applied to toners, lotions, serums, and creams. The skin care product uses a composition containing multiple effects to improve the problem of enlarged pores as the core component, and effectively shrinks pores and tightens skin, targeting the skin characteristics of enlarged pores on the face.

[0009] The objective of this invention can be achieved through the following methods:

[0010] In a first aspect, the present invention provides a composition having the effect of shrinking pores and tightening skin, comprising: 1-4 parts by weight of camellia flower extract, 1-4 parts by weight of camellia leaf extract, and 0.2-2 parts by weight of spider lily seed extract.

[0011] As one embodiment of the present invention, the weight ratio of the camellia flower extract, the camellia leaf extract and the spider vine seed extract is 1:1:0.3-0.4.

[0012] As one embodiment of the present invention, the camellia extract is prepared by the following steps: A1. Pretreatment: Take fresh red camellia flowers, dry them to obtain dried flowers, crush the dried flowers, add pure water to soak them, and obtain the liquid. A2. Distillation and concentration: The feed liquid is subjected to ultrasonic vacuum distillation, and the collected distillate is concentrated under reduced pressure to obtain concentrated distillate for later use. A3. Water extraction: Heat the remaining liquid from step A2 to extract the extract. A4. Concentration: The extract is concentrated under reduced pressure to obtain concentrate 1; A5. Alcohol precipitation for impurity removal: Add ethanol to concentrate 1, stir and let stand, then separate the supernatant; add more ethanol to the supernatant, stir and let stand, then separate the supernatant; then concentrate the supernatant under reduced pressure to obtain concentrate 2. A6. Water precipitation to remove impurities: Add pure water to concentrate 2, stir and let stand, separate the supernatant, and concentrate to obtain concentrate 3. A7. Drying: Combine the concentrated distillate from step A2 and the concentrated liquid 3 from step A6 and dry under reduced pressure to obtain camellia extract.

[0013] Furthermore, in step A1, the mass of pure water added is 12 to 15 times the mass of the red camellia flowers, and the soaking time is 1 to 2 hours.

[0014] Further, in step A2, the ultrasonic vacuum distillation is performed with an ultrasonic frequency of 22-28 kHz, a vacuum distillation pressure of 30-50 kPa, and a temperature of 70±5℃; the ultrasonic vacuum distillation time is 1-1.5 h.

[0015] Further, in step A2, the volume is concentrated under reduced pressure to 1 / 10 to 1 / 5 of its original weight.

[0016] Further, in step A3, the heating extraction temperature is 90~100℃, and the time is 1.5~2h. In some embodiments, the heating extraction further includes a secondary extraction, wherein the residue is added to 8~10 times the amount of water, and a second extraction is performed for 1~1.5h, the extract is collected, and the two extracts are combined.

[0017] Further, in step A4, the concentration is reduced by pressure to 3 to 5 times the weight of the red camellia flowers.

[0018] Further, in step A5, the mass of ethanol added is 1.5 to 3 times the mass of the concentrate, until the ethanol concentration in the concentrate is 35 to 40%; the mass of ethanol replenished is 4 to 7 times the mass of the concentrate, until the ethanol concentration in the supernatant is 65 to 70%; and the concentration is carried out under reduced pressure until it is 3 to 5 times the weight of the red camellia flower.

[0019] Furthermore, in step A6, the mass of pure water added is 2 to 3 times the mass of concentrate 2; and the concentration is increased to 1 to 2 times the weight of the red camellia flowers.

[0020] As one embodiment of the present invention, the total flavonoid content in the camellia extract is ≥2%, and the total phenol content is ≥1%.

[0021] As one embodiment of the present invention, the preparation method of the camellia tea extract includes the following steps: B1. Take fresh Hongshan tea leaves, dry them to obtain dried leaves, and then crush the dried leaves into powder; B2. Add ethanol to the crushed dried leaves, perform ultrasonic extraction, and filter to obtain the filtrate; B3. Concentrate the filtrate under reduced pressure to obtain a concentrated solution; B4. The concentrate is refrigerated and filtered to obtain a clear filtrate; after being concentrated under reduced pressure, anhydrous ethanol is added, and the filtrate is refrigerated and filtered to remove the ethanol, thus obtaining the extract of red tea leaves. B5. Dry the extract of Hongshan tea leaves under reduced pressure to obtain the final product.

[0022] In one embodiment of the present invention, in step B1, the drying temperature is 55-65°C and the time is 8-10 hours.

[0023] In one embodiment of the present invention, in step B2, the mass of ethanol added is 8-12 times the mass of the dried leaves; the ultrasonic extraction power is 400-450W, the temperature is 45-55℃, and the time is 1-2h.

[0024] In one embodiment of the present invention, in step B4, the refrigeration temperature is 3-5°C and the time is 15-48h; the material is concentrated under reduced pressure to 1-3 times the mass of the dried leaves.

[0025] As one embodiment of the present invention, the Paeonia lactiflora seed extract is prepared by the following steps: C1. Impurity removal, drying and pulverization: Select the seeds of the bird's foot and remove impurities, wash, dry and pulverize them to obtain bird's foot seed powder; C2. Degreasing: The powder of *Spiraea japonica* seeds is degreased by supercritical CO2 extraction to obtain defatted *Spiraea japonica* seed powder. C3. Enzymatic hydrolysis: Take defatted Lobelia chinensis seed powder, add pure water to soak, adjust the pH, add hemicellulase, cellulase and pectinase respectively, stir and hydrolyze, and then inactivate the enzymes in a water bath. C4. Ultrasonic extraction: Add ethanol to the filter residue after enzymatic hydrolysis, sonicate, filter and collect the filtrate; C5. Reflux extraction: Add ethanol to the remaining residue after enzymatic hydrolysis in step C3, heat under reflux, repeat 1-2 times, filter and collect the filtrate. C6. Purification: Combine the filtrates from steps C4 and C5, filter through a microfiltration membrane, and then purify by adsorption with macroporous resin. C7. Concentration and Drying: The purified filtrate is concentrated under reduced pressure to obtain a concentrated extract; the concentrated extract is then dried under reduced pressure to obtain the Lobelia chinensis seed extract.

[0026] Furthermore, in step C1, the drying temperature is 45-55℃ and the drying time is 6-8 hours.

[0027] Furthermore, in step C2, during the supercritical CO2 extraction and defatting, the flow rate of the CO2 fluid is 15~30 mL / min, the extraction pressure is 20~30 MPa, the temperature is 35~50℃, and the time is 1~1.5 h.

[0028] Further, in step C3, the mass of pure water added is 8-12 times the mass of the Lobelia chinensis seed powder; the soaking temperature is 40-50℃, and the time is 1-2 h; the pH is adjusted to 4.5-5.0; the mass percentage of hemicellulase added is 0.1-0.2%, the mass percentage of cellulase added is 0.5-0.7%, and the mass percentage of pectinase added is 0.2-0.4%.

[0029] Furthermore, in step C4, the mass of ethanol added is 8-12 times the mass of the filter residue; the ultrasonic power is 150-200W, and the time is 25-35min.

[0030] Furthermore, in step C5, the mass of ethanol added is 5-10 times the mass of the remaining enzymatically hydrolyzed filter residue from step C3; the heating and reflux time is 1-1.5 hours.

[0031] As one embodiment of the present invention, the total alkaloid content in the *Polygonum multiflorum* seed extract is ≥4%.

[0032] As one embodiment of the present invention, the composition further includes a polar polyol and water, wherein the content of the polyol is ≥40%, and the pH of the composition is controlled at 4.0-5.0.

[0033] Secondly, the present invention provides a method for preparing the composition having the effect of shrinking pores and tightening skin, comprising the following steps: S1. Lobelia root extract, water, and polyol were selected as phase A, and camellia flower extract, camellia leaf extract, water, and polyol were selected as phase B. S2. Mix the water and polyol in phase A and stir. After heating, slowly add the Lobelia chinensis extract powder and stir until completely dissolved. Adjust the pH. S3. Mix water and polyol in phase B, stir, and slowly add camellia flower extract and camellia leaf extract after heating. S4. Combine phase A and phase B, stir evenly, and filter the liquid to obtain the composition.

[0034] In one embodiment of the present invention, in step S2 or S3, the temperature is raised to 45-50°C; the polyol content ratio in phase A or phase B is 1:0.9-1.2.

[0035] In one embodiment of the present invention, in step S2, the pH is adjusted to 4.0-5.0.

[0036] Thirdly, the present invention provides the use of the composition in the preparation of cosmetics that improve large facial pores.

[0037] As one embodiment of the present invention, the composition is added to cosmetics at an amount of 0.2-10%.

[0038] The composition of this invention has the effect of shrinking pores and tightening skin. It works by synergistically shrinking pores and tightening skin through multiple pathways, improving the problem of enlarged facial pores. The camellia flower extract contained in the composition can promote the secretion of aquaporin 3, hyaluronic acid, and filaggrin, enhancing the skin's water retention capacity. Furthermore, the camellia flower extract can inhibit the abnormal proliferation of keratinocytes by upregulating p21 protein, preventing the formation of keratin plugs that enlarge pores. The tea leaf extract contained in the composition can control inflammation and sebum secretion by inhibiting the inflammatory signaling factor NF-κB and downregulating sterol regulatory element-binding protein SREBP-1. The combination of camellia flower extract and tea leaf extract can synergistically improve the problem of enlarged pores caused by excessive sebum secretion due to dehydration by regulating the water-oil balance. In addition, the coix seed extract contained in the composition can improve the problem of enlarged pores caused by the loss of collagen and elastin in the dermis by upregulating microfibrillary-associated glycoprotein-1 (MAGP-1) and promoting the secretion of collagen and elastin in the dermis, resulting in the collapse and protrusion of the skin around the hair follicles.

[0039] Compared with the prior art, the present invention has the following beneficial effects: 1. This invention unexpectedly discovered that camellia tea extract can control inflammation and sebum secretion by inhibiting the inflammatory signaling factor NF-κB and downregulating the sterol regulatory element-binding protein SREBP-1. Therefore, combining camellia tea extract with camellia flower extract and spider plant seed extract can synergistically shrink pores and tighten skin through multiple pathways, improving the problem of enlarged facial pores. Simultaneously, this invention further enhances the pore-shrinking effect by optimizing the extraction process of camellia flower extract and spider plant seed extract, thereby increasing the content and activity of various active ingredients.

[0040] 2. This invention employs a distillation + water extraction process to prepare camellia extract, utilizing stepwise alcohol removal (first removing polysaccharides with a low-alcohol solution, then removing proteins with a higher-alcohol solution). This reduces polyphenol oxidation at high temperatures, effectively enriching the active ingredients such as polyphenols and flavonoids in camellia and enhancing their activity. Compared to traditional vinegar extraction, the camellia extract prepared using this optimized extraction method significantly increases the relative expression levels of the AQP3 gene, HA content, and FLG gene, exhibiting significant moisturizing effects. This helps maintain the skin's water-oil balance, preventing excessive sebum secretion and enlarged pores caused by water-oil imbalance. It also significantly increases p21 protein content, inhibiting excessive keratinocyte proliferation. Furthermore, this extraction method shortens distillation time and is more energy-efficient.

[0041] 3. This invention uses an enzymatic hydrolysis-ethanol extraction method to prepare *Cassia tora* seed extract, enriching the total alkaloids in the seeds. This results in a multi-active ingredient in the extract, which promotes the secretion of collagen and elastin in the dermis, improving the problem of sunken, protruding, and enlarged pores around hair follicles caused by the loss of collagen and elastin in the dermis. Compared to traditional extraction methods that use high-purity rhamnosyluridine for extraction, with the goal of oil control, this invention uses an optimized extraction method to prepare *Cassia tora* seed extract. Unexpectedly, it was found that this extract can significantly increase the secretion of type I collagen, type III collagen, and elastin by upregulating microfibrillary-associated glycoprotein-1 (MAGP-1), increasing the relative expression level of the MAGP-1 gene, improving the problem of sunken, protruding, and enlarged pores around hair follicles caused by the loss of collagen and elastin in the dermis, and enhancing the pore-shrinking effect.

[0042] 4. The composition provided by this invention includes camellia flower extract, tea leaf extract, and spider lily seed extract. These three plant extracts are compounded with polyols and water. In addition to the clear target effects of each component on the problem of enlarged facial pores, they also have a synergistic effect. The composition can enhance the skin's water-retention capacity, inhibit excessive proliferation of keratinocytes, suppress inflammation and sebum secretion, and promote the secretion of collagen and elastin in the dermis. This achieves skin water-oil balance, prevents keratin plugs, prevents the vicious cycle of inflammation and excessive sebum secretion, and prevents sagging skin around hair follicles. It can comprehensively solve the problem of enlarged facial pores through multiple pathways. Furthermore, the raw materials are natural and safe, showing good application prospects.

[0043] 5. The composition provided by the present invention, by combining camellia flower extract and tea leaf extract, can synergistically regulate the skin's water-oil balance, thereby improving the problem of enlarged pores caused by excessive oil secretion due to skin dehydration by maintaining the skin's water-oil balance; at the same time, by limiting the ratio of camellia flower extract, tea leaf extract, and spider lily seed extract, it can achieve the comprehensive effect of shrinking pores, tightening skin, and improving the enlarged facial pores.

[0044] 6. The composition provided by this invention is controlled to be weakly acidic, with a pH value of 4.0-5.0. Maintaining a weakly acidic composition helps maintain a healthy physiological environment for the skin, preventing pore blockage. Furthermore, limiting the proportion of polyols in phases A and B ensures symmetry between phases A and B in both polarity and density dimensions, resulting in better stability after mixing phases A and B. Attached Figure Description

[0045] Other features, objects, and advantages of the present invention will become more apparent from the following detailed description of non-limiting embodiments with reference to the accompanying drawings: Figure 1This is a comparison of the effect of the product on improving enlarged facial pores before (day 0, left image) and after (day 28, right image) in the base group; Figure 2 This is a comparison chart showing the improvement in enlarged facial pores in Group A before (0 days, left image) and after (28 days, right image); Figure 3 The comparison chart shows the improvement in enlarged facial pores in Group B before (0 days, left image) and after (28 days, right image). Figure 4 The comparison chart shows the improvement in enlarged facial pores in Group C before (0 days, left image) and after (28 days, right image); Figure 5 This is a comparison chart showing the improvement in enlarged facial pores in Group D before (0 days, left image) and after (28 days, right image). Detailed Implementation

[0046] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments. The following examples are implemented under the premise of the technical solution of the present invention, providing detailed implementation methods and specific operating procedures, which will help those skilled in the art to further understand the present invention. It should be noted that the scope of protection of the present invention is not limited to the following embodiments; any adjustments and improvements made under the concept of the present invention are all within the scope of protection of the present invention.

[0047] Example 1 This embodiment provides a method for preparing camellia flower extract, which specifically includes the following steps: Step (1) Pretreatment: Take fresh red camellia flowers, dry them to obtain dried camellia flowers, crush them and soak them in 15 times the amount of pure water for 1 hour; Step (2) Distillation and concentration: The liquid in step (1) is subjected to ultrasonic vacuum distillation for 1.5 hours. The ultrasonic parameters are: frequency of 25 kHz, pulse mode (5 seconds on, 5 seconds off). The vacuum distillation parameters are: pressure control of 40 kPa, temperature control of 70 ℃, so that the liquid is kept at a slight boil. The distillate is collected and concentrated under vacuum to 1 / 5 of the weight of the raw liquid to obtain concentrated distillate, which is stored at 4 ℃ for later use. Step (3) Water extraction: Heat the liquid to 90~100℃ and extract for 2 hours under a slight boiling state. Collect the liquid and pass it through a 100-mesh sieve for later use. Add 9 times the amount of water to the residue and perform a second extraction for 1 hour. Collect the liquid and pass it through a 100-mesh sieve for later use. Step (4) Concentration: Combine the two extraction liquids and concentrate under reduced pressure until the concentration is 4 times the weight of dried red camellia flowers to obtain concentrated liquid; Step (5) Alcohol precipitation to remove impurities: Add 2 times anhydrous ethanol to the concentrate, stir for 10 min, let stand at low temperature for 4 h, and centrifuge with a refrigerated centrifuge to collect the supernatant; add 5.4 times ethanol to the supernatant, stir for 10 min, let stand at low temperature for 10 h, centrifuge again to collect the supernatant and concentrate under reduced pressure to recover ethanol. Step (6) Water precipitation to remove impurities: Add 2 times the amount of pure water to the concentrate, stir and let stand for 8 hours, centrifuge to take the supernatant, and concentrate the supernatant to 2 times the weight of dried red camellia flowers; Step (7) Drying: Combine the concentrate from step (6) with the concentrated distillate from step (2), and dry under reduced pressure to obtain camellia extract.

[0048] The camellia extract powder obtained in Example 1 was tested for its active ingredient content. The total flavonoid content was 2.3%, and the total phenol content was 1.6%. The test method for total flavonoid content was in accordance with DB43 / T 476-2009; the test method for total phenol content was in accordance with T / AHFIA005-2018.

[0049] Comparative Example 1 This comparative example refers to patent application CN104027265A, which provides a method for preparing camellia vinegar extract, specifically including the following steps: Step (1) Preparation of distiller's grains: Wash 2 kg of brown rice and soak it in 3 kg of mineral water for 5 hours, then drain and set aside. Wash and cut red camellia flowers and drain them. Mix the soaked brown rice with 0.9 kg of camellia flowers and steam at 90-110℃ for 25-35 minutes, then cool to 60℃. Add 0.2 kg of malt powder to the cooled brown rice and saccharify for 12 hours. Then add 0.6 kg of koji and saccharify at 30℃ for 48 hours to activate the Aspergillus. Put the obtained rice into a vat, add 4 kg of mineral water, and maintain the temperature at 25℃ for 72 hours, blocking air from the outside and only releasing carbon dioxide, thus obtaining distiller's grains.

[0050] Step (2) Ethanol fermentation: Wash 1.3 kg of brown rice, soak it in 2 kg of water for 1 hour, drain the water, and steam the remaining brown rice and 0.1 kg of camellia flowers at a temperature of 90~110℃ for 25~35 minutes to obtain steamed rice. Add the prepared steamed rice and 1 kg of camellia flowers to the lees prepared in step (1) above, and carry out ethanol fermentation at 25℃ for 10~15 days.

[0051] Step (3) Acetic acid fermentation: After diluting the fermentation product obtained in step (2) with 0.1 kg of water, carry out a one-time (aerobic) acetic acid fermentation at 27°C for 2 months. During this process, the mouth of the container is sealed with a cloth, but oxygen can enter the container. Occasionally, it needs to be stirred to provide oxygen. The acidity of the obtained fermentation product is measured (pH-230SD pH meter). After confirming that the pH is above 4, the supernatant is separated and subjected to a second ripening in a cool place at 5~20°C. The ripened liquid is then filtered to obtain camellia vinegar extract. The obtained camellia vinegar extract is sterilized, bottled, and stored in a cool, dark place.

[0052] Example 2 This embodiment refers to a method for preparing camellia tea extract provided by patent application CN113797261A, which specifically includes the following steps: Step (1) Pretreatment: Take fresh Hongshan tea leaves and dry them at 60℃ for 8~10h (at this time, the yield of dried Hongshan tea leaves is approximately 1:0.2 of fresh leaves to dried leaves). The dried Hongshan tea leaves are then crushed. Step (2) Ultrasonic extraction: Add 8 times the weight of 60% ethanol, sonicate for 1.5 h, filter and collect the filtrate, repeat twice; the ultrasonic parameters are: power 420W, temperature 50℃; Step (3) Concentration: Combine the two extracts from step (2) and concentrate under reduced pressure at 45°C to obtain a concentrated solution; Step (4) Impurity removal: The concentrate is placed at 4℃ for 15 hours and filtered to obtain a clear filtrate; the filtrate is then concentrated under reduced pressure to twice the weight of the original dry red tea powder, and anhydrous ethanol equal to the weight of the dry red tea powder is added. The concentrate is then placed at 4℃ for 48 hours and filtered to obtain a clear liquid; the clear liquid is then concentrated under reduced pressure to remove the ethanol, and red tea extract paste is obtained. Step (5) Drying: The red tea extract extract from step (4) is dried under reduced pressure to obtain red tea extract.

[0053] Example 3 This embodiment provides a method for preparing a root extract of *Polygonum multiflorum*, which specifically includes the following steps: Step (1) Removing impurities, drying, and pulverizing: Select the seeds of the Lobelia chinensis, remove impurities, wash, and dry at 50℃ for 6 hours; use a high-speed pulverizer to pulverize the Lobelia chinensis seeds to obtain powder; Step (2) Degreasing: Degrease the Paeonia lactiflora seed powder by supercritical CO2 extraction (extraction parameters: CO2 fluid flow rate 200mL / min, extraction pressure 20Mpa, temperature 40℃, time 1.5h) to obtain degreased Paeonia lactiflora seed powder, which is stored at 4℃ for later use. Step (3) Enzymatic hydrolysis: Take 30g of defatted Lophatherum gracile seed powder, add 10 times the weight of pure water, soak at 45℃ for 1h, adjust pH to 5.0, add 0.1% hemicellulase, 0.6% cellulase and 0.3% pectinase by weight of Lophatherum gracile seed powder respectively, stir at constant temperature for 1.5h, and inactivate enzymes in a 90℃ water bath for 10min; Step (4) Extraction: ① Ultrasonic extraction: Add 10 times the weight of 70% ethanol to the filter residue after enzymatic hydrolysis, and sonicate at 40℃ for 30 min (using intermittent ultrasound: ultrasound power 180W, ultrasound for 10s, stop for 5s, effective ultrasound time 30min), filter and collect the filtrate; ② Reflux extraction: Add 8 times the weight of 70% ethanol to the filter residue in step (4)-①, heat and reflux for 1h, repeat twice, filter and collect the filtrate; Step (5) Purification: Combine the filtrates from steps ① and ② in step (4), filter them through a microfiltration membrane, and then purify them by adsorption with macroporous resin; Step (6) Concentration and drying: The purified liquid is concentrated under reduced pressure to obtain concentrated extract; the extract is dried under reduced pressure to obtain Lobelia chinensis seed extract.

[0054] The active ingredient index of the extract of *Smilax china* obtained in Example 3 was detected, and the total alkaloid content was 5.6%. The detection method of total alkaloid content was ultraviolet spectrophotometry, specifically: (1) Preparation of standard: Weigh berberine hydrochloride, dissolve it in 30% ethanol solution and make up to 100 mL to prepare a standard stock solution with a mass concentration of 4 mg / mL; then dilute it to a series of standard solutions with mass fractions of 0.4, 0.8, 1.2, 1.6 and 2.0 mg / mL; plot the standard curve with the mass concentration of the series standard solutions as the abscissa and the absorbance as the ordinate. (2) Preparation of sample: Weigh 6 mg of sample, dissolve it in 30% ethanol solution and make up to 100 mL, shake well. (3) Analytical testing: The absorbance values ​​of the standard solution and the sample were measured at a wavelength of 347 nm and calculated according to the following formula: ω = (c × V) / m × 100; where: ω is the total alkaloid content, %; c is the concentration of berberine hydrochloride calculated according to the standard curve, mg / mL; V is the final volume of the sample, mL; m is the mass of the sample, mg.

[0055] Comparative Example 2 This comparative example refers to patent application CN114437158B, which provides a method for extracting rhamnosides from the seeds of *Spiraea japonica*, specifically including the following steps: (1) Take 500g of *Spiraea japonica* seeds, remove oil by pressing with an oil press, and recover the filter cake; (2) Add water at 10 times the weight of the filter cake, extract at 80℃ for 2h, and filter the obtained extract through 10um and 5um polypropylene membranes in sequence, and collect the filtrate; (3) Adsorb the filtrate with a D101 macroporous resin column, wash with pure water until the effluent is basically colorless, and then wash with 30% ethanol until the effluent is basically colorless, collect the 30% ethanol eluent, and concentrate it to an ethanol content of 4% (measured by an ethanol alcohol meter); (4) Adsorb the concentrate in step (3) with an MCI CHP20P resin column, and wash the column in sequence with water, 10% ethanol, 20% ethanol, and 30% ethanol; (5) Remove the solvent from the 20% ethanol eluent in step (4) by rotary evaporation to obtain *Spiraea japonica* seed extract.

[0056] Example 4 This embodiment provides a composition with the effect of shrinking pores and tightening skin. The composition consists of: 2.5 parts of camellia flower extract (Example 1), 2.5 parts of camellia leaf extract (Example 2), 0.75 parts of spider lily seed extract (Example 3), 48.75 parts of 1,3-propanediol, and 45.5 parts of water.

[0057] The preparation method of the above composition is as follows: (1) Phase separation: Phase A consists of 0.75 parts of Lobelia chinensis extract, 25.5 parts of water, and 23.75 parts of polyol; Phase B consists of 2.5 parts of Camellia japonica extract, 2.5 parts of Camellia oleifera extract, 20 parts of water, and 25 parts of polyol; (2) Mix and stir the water and polyol in Phase A, heat to 45°C, slowly add Lobelia chinensis extract, stir until completely dissolved, cool to room temperature, and adjust the pH to 4.50; (3) Mix and stir the water and polyol in Phase B, heat to 45°C, and slowly add Camellia japonica extract and Camellia oleifera extract; (4) Combine Phase A and Phase B, stir evenly, and filter the liquid through a 0.22μm membrane to obtain the composition.

[0058] Comparative Example 3 The composition and preparation method of this comparative example are basically the same as those in Example 4, except that the tea leaf extract is omitted from the composition.

[0059] Comparative Example 4 The composition and preparation method of this comparative example are basically the same as those of Example 4, except that the camellia extract is replaced with the camellia extract prepared in Comparative Example 1.

[0060] Comparative Example 5 The composition and preparation method of this comparative example are basically the same as those of Example 4, except that the root extract of *Polygonum multiflorum* is replaced with the root extract of *Polygonum multiflorum* prepared in Comparative Example 2.

[0061] Example 5 This embodiment provides a composition with the effect of shrinking pores and tightening skin. The composition consists of: 1 part camellia flower extract, 1 part camellia leaf extract, 0.4 parts coix seed extract, 42 parts 1,3-propanediol, and 55.6 parts water.

[0062] The preparation method of the above composition is as follows: (1) Phase separation: Phase A consists of 0.4 parts of Lobelia chinensis extract, 25.6 parts of water, and 20 parts of polyol; Phase B consists of 1 part of Camellia japonica extract, 1 part of Camellia oleifera extract, 30 parts of water, and 22 parts of polyol; (2) Mix and stir the water and polyol in Phase A, heat to 45°C, slowly add Lobelia chinensis extract, stir until completely dissolved, cool to room temperature, and adjust the pH to 5.00; (3) Mix and stir the water and polyol in Phase B, heat to 45°C, and slowly add Camellia japonica extract and Camellia oleifera extract; (4) Combine Phase A and Phase B, stir evenly, and filter the liquid through a 0.22μm membrane to obtain the composition.

[0063] Example 6 This embodiment provides a composition with the effect of shrinking pores and tightening skin. The composition consists of: 4 parts camellia flower extract, 4 parts tea leaf extract, 1.4 parts coix seed extract, 50 parts 1,3-propanediol, and 40.6 parts water.

[0064] The preparation method of the above composition is as follows: (1) Phase separation: Phase A consists of 1.4 parts of Lobelia chinensis extract, 22.6 parts of water, and 25 parts of polyol; Phase B consists of 4 parts of Camellia japonica extract, 4 parts of Camellia oleifera extract, 18 parts of water, and 25 parts of polyol; (2) Mix and stir the water and polyol in Phase A, heat to 45°C, slowly add Lobelia chinensis extract, stir until completely dissolved, cool to room temperature, and adjust the pH to 4.50; (3) Mix and stir the water and polyol in Phase B, heat to 45°C, and slowly add Camellia japonica extract and Camellia oleifera extract; (4) Combine Phase A and Phase B, stir evenly, and filter the liquid through a 0.22μm membrane to obtain the composition.

[0065] Verification Example 1 This embodiment demonstrates the efficacy of the camellia extract in enhancing skin's moisture retention capacity and inhibiting abnormal proliferation of keratinocytes. The samples used in this verification example are the products obtained in Example 1 and Comparative Example 1, respectively.

[0066] The relative expression levels of aquaporin-3 (AQP3) gene, hyaluronic acid (HA) content, filaggrin (FLG) gene, and p21 protein content were measured using a Hacat cell model. The experimental groups included a blank control group (BC group, no sample added, no cell induction), a model control group (NC group, no sample added, model induced by H2O2), and a sample group (sample added after H2O2 induction). The AQP3 content, hyaluronic acid content, and relative expression levels of filaggrin (FLG) gene were measured using a double-antibody sandwich assay kit; the p21 protein content was detected using immunofluorescence. The results are shown in Table 1 below. The increase rate was calculated as: Increase rate = (sample group index value - NC group index value) / NC group index value 100%.

[0067] Table 1

[0068] Note: Compared with the model control group: This indicates that p < 0.05; This indicates that p < 0.01; This indicates that p < 0.001; This indicates that p < 0.0001. The p value is a core parameter used in hypothesis testing in statistics. p < 0.05 indicates that the experimental result is statistically significant. The smaller the p value, the stronger the statistical significance.

[0069] Aquaporin-3 (AQP-3) is located on the membrane of epidermal keratinocytes and has the function of transmembrane transport of small molecules such as water, glycerol, and urea, maintaining skin hydration. Hyaluronic acid (HA) is a natural moisturizing factor in the skin and can effectively lock in moisture. Filamentin (FLG) is secreted by keratinocytes and has the function of maintaining epidermal hydration, forming a physical barrier, reducing epidermal water loss, and maintaining the moisture content of the stratum corneum. p21 protein is a small molecule CDK inhibitor protein that is closely related to the proliferation of keratinocytes. As shown in Table 1, when cells are damaged, the expression levels of AQP-3, HA, FLG, and p21 all decrease. The addition of the camellia extract provided in this invention can significantly increase the relative expression level of AQP3 gene, HA content, and FLG gene, showing significant moisturizing effects; and can significantly increase the p21 protein content, showing the effect of inhibiting excessive proliferation of keratinocytes. The camellia extract provided by this invention has significantly better moisturizing and anti-keratinocyte proliferation effects than the camellia vinegar extract in Comparative Example 1.

[0070] Verification Example 2 This embodiment provides efficacy verification of the tea leaf extract in inhibiting the inflammatory signaling factor NF-κB and downregulating the sterol regulatory element-binding protein SREBP-1. The sample used in this embodiment is the product obtained in Example 2.

[0071] The NF-κB assay was designed according to the research document "Anti-inflammatory and Anti-oxidative Effects of Korean Red Ginseng Extract in Human Keratinocytes". Real-time quantitative PCR (RT-qPCR) was used to detect the mRNA level of NF-κB in human keratinocytes (HaCaT cells). The experiment included a blank control group (normal HaCaT cells), a model control group (LPS-induced HaCaT cells), and a sample group (HaCaT cells induced by LPS followed by the addition of experimental samples). The results are shown in Table 2 below.

[0072] Table 2

[0073] Note: Comparison between the blank control group and the model control group: # This indicates that p < 0.05. ## This indicates that p < 0.01. ### This indicates p < 0.001; Comparison between the sample group and the model control group: This indicates that p < 0.05. This indicates that p < 0.01. This indicates that p < 0.001.

[0074] The SREBP-1 assay used a golden hamster sebaceous gland patch model, and immunohistochemistry was used to detect the expression of SREBP-1 in the sebaceous gland patches. The experiment included a blank control group (normal individuals treated without intervention) and a sample group (using the skin images of the experimental sample group). The results are shown in Table 3 below.

[0075] Table 3

[0076] Note: Compared with the blank group, A p-value < 0.05 indicates a significant difference; otherwise, there is no significant difference.

[0077] NF-κB plays a crucial role in inflammatory responses, participating in the regulation of various inflammatory factors. Activation of NF-κB can increase the production of pro-inflammatory cytokines, thereby triggering and regulating inflammatory responses, and in most cases leading to the activation of a pro-inflammatory cascade. Inflammatory factors can indirectly stimulate sebaceous gland cells to secrete more sebum, and can also cause abnormal keratinization of the hair follicle opening, providing physical blockage conditions for sebum accumulation. Sterol regulatory element-binding protein SREBP-1 is a major transcriptional regulator of lipid metabolism; its reduced activity can inhibit the expression levels of lipid synthesis-related enzymes such as fatty acids and triglycerides. Therefore, testing the expression level of SREBP-1 in sebaceous gland cells can reflect the effect and extent of the active ingredient on sebum metabolism. As shown in Tables 2-3, the camellia tea extract provided in this invention can significantly inhibit the expression of the inflammatory factor NF-κB and significantly downregulate the expression of SREBP-1.

[0078] Verification Example 3 This embodiment provides efficacy verification of the above-described *Spiraea japonica* seed extract in promoting fibroblast proliferation and upregulating microfibrillary-associated glycoprotein-1 (MAGP-1). The samples used in this verification example are the products obtained in Example 3 and Comparative Example 2, respectively.

[0079] The content of type I collagen was determined according to "T / SHRH 031-2020, Cosmetic Firming and Anti-wrinkle Efficacy Test - In Vitro Fibroblast Type Collagen Content Determination", using enzyme-linked immunosorbent assay (ELISA). The relative expression level of MAGP-1 gene was determined according to "Qiu W, Chen F, Feng X, Shang J, Luo X, Chen Y. Potential role of inflammation mediated by the complement system in enlarged facial pores. JCosmet Dermatol. 2024 Jan;23(1):27-32. doi:10.1111 / jocd.15956. Epub 2023 Aug9. PMID:37555304.". The experimental groups included a blank control group (normal fibroblasts, no sample added), a positive control group (normal fibroblasts, positive drug 50 ng / mL TGF-β added), and a sample group (normal fibroblasts, experimental sample added). The results are shown in Table 4 below.

[0080] Table 4

[0081] Note: Compared with the blank control group This indicates that P < 0.05. This indicates that P < 0.01. P < 0.0001 indicates a significant difference.

[0082] The method for determining type III collagen content followed the guidelines in "Type III Collagen Production in Human Skin Fibroblast Cultures and Its Decline with Age," while the method for determining elastin content followed the guidelines in "RUBY / MS-S0042-A00," employing immunofluorescence staining. Experimental groups included a blank control group (normally cultured fibroblasts without treatment), a model control group (fibroblasts treated with UVA), and a sample group (fibroblasts treated with UVA and supplemented with experimental samples). The results are shown in Table 5 below.

[0083] Table 5

[0084] Note: Comparison between the blank control group and the model control group: # This indicates that p < 0.05. ## This indicates that p < 0.01. ### This indicates p < 0.001; Comparison between the sample group and the model control group: This indicates that p < 0.05. This indicates that p < 0.01. This indicates that p < 0.001.

[0085] Type I collagen, type III collagen, and elastin are the main components of the extracellular matrix of human dermal cells. When type I and type III collagen decrease, the skin's supporting structure weakens, leading to fine lines and deep wrinkles. When elastin is lost, the skin loses elasticity and resilience, resulting in sagging. Microfibrils are nanoscale fibrous structures in the extracellular matrix, mainly composed of fibrillary proteins. Their core function is to provide a scaffold for elastin deposition and maintain skin structural integrity through interaction with collagen fibers. Microfibril-associated glycoprotein 1 (MAGP-1), as a low-molecular-weight glycoprotein, is a key regulator of microfibril homeostasis. In the area around hair follicles / pores, the loss of MAGP-1 leads to impaired microfibril assembly, thereby weakening the anchoring and function of elastic fibers, reducing the elasticity of the peripore structure, and ultimately manifesting as signs of aging such as enlarged pores. As shown in Tables 4-5, the extract of *Smilax china* seeds provided by this invention can significantly increase the secretion of type I collagen, type III collagen and elastin, and significantly increase the relative expression level of the MAGP-1 gene, indicating that it has a firming effect and can shrink pores, and the effect is significantly better than that of the comparative sample 2.

[0086] Verification Example 4 This embodiment provides verification of the efficacy of the composition in improving enlarged facial pores. At the level of human trials, the pore-shrinking effects of Comparative Example 4, Comparative Example 3, Comparative Example 4, and Comparative Example 5 are compared. Specific formulations for human use are shown in Table 6.

[0087] Table 6

[0088] Test method: Multiple subjects were recruited to use the test sample continuously for 28 days. A blinded, self-controlled, and pre- and post-test methods were used. Multifunctional 3D skin imaging analysis (Antera 3D, Miravex, Ireland) was used to test the total number of skin pores, total pore area, and number of pores to judge and compare the efficacy of the sample. The results are shown in Table 7.

[0089] As shown in Table 7, after 28 days of product use, the pore-related parameters of the subjects in Group A were significantly improved, and were superior to those of Groups B, C, and D.

[0090] Table 7

[0091] Note: Compared with before use (day 0): This indicates that p < 0.05. This indicates that p < 0.01.

[0092] Figure 1-5The images show a comparison of the improvement in enlarged facial pores before (day 0, left image) and after (day 28, right image) product use in the matrix group, group A (with sample from Example 4), group B (with sample from Comparative Example 3), group C (with sample from Comparative Example 4), and group D (with sample from Comparative Example 5). It is evident that group A showed a significant improvement in pore shrinkage, superior to groups B, C, and D.

[0093] The specific embodiments of the present invention have been described above. It should be understood that the present invention is not limited to the specific embodiments described above, and those skilled in the art can make various modifications or variations within the scope of the claims, which do not affect the essence of the present invention.

Claims

1. A composition having the effect of shrinking pores and tightening skin, characterized in that, include: By weight, 1-4 parts camellia flower extract, 1-4 parts camellia leaf extract, and 0.2-2 parts spider lily seed extract.

2. The composition according to claim 1, characterized in that, The camellia flower extract was prepared by the following steps: A1. Pretreatment: Take fresh red camellia flowers, dry them to obtain dried flowers, crush the dried flowers, add pure water to soak them, and obtain the liquid. A2. Distillation and concentration: The feed liquid is subjected to ultrasonic vacuum distillation, and the collected distillate is concentrated under reduced pressure to obtain concentrated distillate for later use. A3. Water extraction: Heat the remaining liquid from step A2 to extract the extract. A4. Concentration: The extract is concentrated under reduced pressure to obtain concentrate 1; A5. Alcohol precipitation for impurity removal: Add ethanol to concentrate 1, stir and let stand, then separate the supernatant; add more ethanol to the supernatant, stir and let stand, then separate the supernatant; then concentrate the supernatant under reduced pressure to obtain concentrate 2. A6. Water precipitation to remove impurities: Add pure water to concentrate 2, stir and let stand, separate the supernatant, and concentrate to obtain concentrate 3. A7. Drying: Combine the concentrated distillate from step A2 and the concentrated liquid 3 from step A6 and dry under reduced pressure to obtain camellia extract.

3. The composition according to claim 2, characterized in that, In step A1, the mass of pure water added is 12 to 15 times the mass of the red camellia flowers, and the soaking time is 1 to 2 hours; And / or, in step A2, the ultrasonic vacuum distillation is carried out at a frequency of 22-28 kHz, a pressure of 30-50 kPa, and a temperature of 70±5℃; the ultrasonic vacuum distillation time is 1-1.5 h; and the concentration is reduced to 1 / 10-1 / 5 of the original weight. And / or, in step A3, the heating extraction temperature is 90~100℃, and the time is 1.5~2h; And / or, in step A4, concentrate under reduced pressure to 3 to 5 times the weight of the red camellia flower; And / or, in step A5, the mass of ethanol added is 1.5 to 3 times the mass of the concentrate, until the ethanol concentration in the concentrate is 35 to 40%; the mass of ethanol replenished is 4 to 7 times the mass of the concentrate, until the ethanol concentration in the supernatant is 65 to 70%; and the concentration is carried out under reduced pressure until it is 3 to 5 times the weight of the red camellia flower. And / or, in step A6, the mass of pure water added is 2 to 3 times the mass of concentrate 2; concentrate to 1 to 2 times the weight of red camellia flowers.

4. The composition according to claim 1, characterized in that, The preparation method of the camellia tea extract includes the following steps: B1. Take fresh Hongshan tea leaves, dry them to obtain dried leaves, and then crush the dried leaves into powder; B2. Add ethanol to the crushed dried leaves, perform ultrasonic extraction, and filter to obtain the filtrate; B3. Concentrate the filtrate under reduced pressure to obtain a concentrated solution; B4. Refrigerate and filter the concentrate to obtain a clear filtrate; After concentration under reduced pressure, anhydrous ethanol is added, and the mixture is refrigerated, filtered, and the ethanol is removed to obtain a Hongshan tea extract paste. B5. Dry the extract of Hongshan tea leaves under reduced pressure to obtain the final product.

5. The composition according to claim 4, characterized in that, In step B1, the drying temperature is 55-65℃ and the time is 8-10 hours; And / or, in step B2, the mass of ethanol added is 8-12 times the mass of the dry leaves; the ultrasonic extraction power is 400-450W, the temperature is 45-55℃, and the time is 1-2h; And / or, in step B4, the refrigeration temperature is 3-5°C, and the time is 15-48 hours; the material is concentrated under reduced pressure to 1-3 times the mass of the dried leaves.

6. The composition according to claim 1, characterized in that, The *Polygonum multiflorum* seed extract was prepared by the following steps: C1. Impurity removal, drying and pulverization: Select the seeds of the bird's foot and remove impurities, wash, dry and pulverize them to obtain bird's foot seed powder; C2. Degreasing: The powder of *Spiraea japonica* seeds is degreased by supercritical CO2 extraction to obtain defatted *Spiraea japonica* seed powder. C3. Enzymatic hydrolysis: Take defatted Lobelia chinensis seed powder, add pure water to soak, adjust the pH, add hemicellulase, cellulase and pectinase respectively, stir and hydrolyze, and then inactivate the enzymes in a water bath. C4. Ultrasonic extraction: Add ethanol to the filter residue after enzymatic hydrolysis, sonicate, filter and collect the filtrate; C5. Reflux extraction: Add ethanol to the remaining residue after enzymatic hydrolysis in step C3, heat under reflux, repeat 1-2 times, filter and collect the filtrate. C6. Purification: Combine the filtrates from steps C4 and C5, filter through a microfiltration membrane, and then purify by adsorption with macroporous resin. C7. Concentration and Drying: The purified filtrate is concentrated under reduced pressure to obtain a concentrated extract; the concentrated extract is then dried under reduced pressure to obtain the Lobelia chinensis seed extract.

7. The composition according to claim 6, characterized in that, In step C1, the drying temperature is 45-55℃ and the drying time is 6-8 hours; And / or, in step C2, during the supercritical CO2 extraction defatting, the flow rate of the CO2 fluid is 15~30 mL / min, the extraction pressure is 20~30 MPa, the temperature is 35~50℃, and the time is 1~1.5 h; And / or, in step C3, the mass of pure water added is 8-12 times the mass of the Lobelia chinensis seed powder; the soaking temperature is 40-50℃, and the time is 1-2 h; the pH is adjusted to 4.5-5.0; the mass percentage of hemicellulase added is 0.1-0.2%, the mass percentage of cellulase added is 0.5-0.7%, and the mass percentage of pectinase added is 0.2-0.4%; And / or, in step C4, the mass of ethanol added is 8-12 times the mass of the filter residue; the ultrasonic power is 150-200W and the time is 25-35min; And / or, in step C5, the mass of ethanol added is 5-10 times the mass of the remaining enzymatically hydrolyzed filter residue from step C3; the heating and reflux time is 1-1.5 h.

8. A method for preparing a composition having the effect of shrinking pores and tightening skin as described in any one of claims 1-7, characterized in that, Includes the following steps: S1. Lobelia root extract, water, and polyol were selected as phase A, and camellia flower extract, camellia leaf extract, water, and polyol were selected as phase B. S2. Mix the water and polyol in phase A and stir. After heating, slowly add the Lobelia chinensis extract powder and stir until completely dissolved. Adjust the pH. S3. Mix water and polyol in phase B, stir, and slowly add camellia flower extract and camellia leaf extract after heating. S4. Combine phase A and phase B, stir evenly, and filter the liquid to obtain the composition.

9. The preparation method according to claim 8, characterized in that, In step S2 or S3, the temperature is raised to 45-50℃; the polyol content ratio in phase A or phase B is 1:0.9-1.

2. And / or, in step S2, adjust the pH to 4.0-5.

0.

10. The use of the composition according to any one of claims 1-7 in the preparation of cosmetics for improving enlarged facial pores, characterized in that, The composition is added to cosmetics at a rate of 0.2-10%.

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