An oral skin care composition based on gut skin axis theory and a method of preparing the same
Patent Information
- Application Number
- CN202510428713.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-08
- Publication Date
- 2026-10-20
- Estimated Expiration
- 2045-04-08
AI Technical Summary
[0002]目前市面上诸多口服美容产品存在的共性问题是:原料堆砌、概念添加、口服美容逻辑不清晰、作用机制不明确
(1)本发明的口服美肤组合物,采用双重微囊化技术及pH响应型控释体系,显著提升成分的稳定性和靶向吸收效率。内层微囊包裹活性胶原三肽、针叶樱桃粉、雨生红球藻粉,能够减缓成分氧化、降解;外层微囊为壳聚糖-果胶-钙离子交联网络,通过碱性环境响应机制实现肠道靶向释放,在胃部酸性条件下,壳聚糖质子化形成致密凝胶屏障,阻隔胃蛋白酶渗透;进入肠道后,果胶脱质子化,与钙离子竞争性解离,触发外层微囊快速崩解,释放组分,实现活性成分的高效吸收;
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Abstract
Description
Technical Field
[0001] This invention relates to the field of oral cosmetic products, specifically to an oral skin care composition based on the gut-skin axis theory and its preparation method. Background Technology
[0002] The common problems of many oral beauty products on the market are: excessive use of raw materials, added concepts, unclear logic of oral beauty, and unclear mechanism of action.
[0003] When collagen-containing oral beauty products are formulated into liquid beverages, they often face the problem of collagen loss due to the Maillard reaction. The Maillard reaction refers to a series of complex non-enzymatic browning reactions between carbonyl compounds (such as reducing sugars) and amino compounds (such as amino acids and proteins). In liquid beverages, collagen, as a protein, contains a large number of amino groups; while common fruit juices often contain reducing sugars such as glucose and fructose, which contain free carbonyl groups. When these reducing sugars and collagen are present simultaneously in collagen-containing liquid beverages, the amino groups in the collagen will react with the carbonyl groups of the reducing sugars during storage. In the early stages of the Maillard reaction, the carbonyl groups of the reducing sugars condense with the free amino groups of collagen to form a Schiff base. The Schiff base undergoes cyclization to form an N-substituted glycosylamine, which then undergoes the Amderui rearrangement to generate a reactive 1-amino-1-deoxy-2-ketose. As the Maillard reaction progresses, various reactive intermediates are generated in the intermediate stage, including substances such as hydroxymethylfurfural. These reactions not only alter the structure and properties of collagen, causing collagen loss and reducing the content of effective collagen in the product, but also negatively affect the product's color and flavor, ultimately leading to a decrease in the product's effectiveness and preventing it from fully realizing its intended beauty benefits.
[0004] Furthermore, the low bioavailability of food-derived bioactive peptides has largely hindered their application in the development of health foods; among them, gastrointestinal digestion and degradation is the key factor restricting the bioavailability of bioactive peptides.
[0005] In conclusion, existing oral beauty products often only focus on collagen supplementation without considering the interactions between the various ingredients, resulting in unsatisfactory actual beauty effects and poor shelf life.
[0006] To address this, the applicant attempted two methods. The first method, based on the gut microbiota axis theory, involves adding ingredients that alter the gut microbiota to oral beauty products to enhance their effectiveness. However, for ease of storage and transportation, the oral beauty products need to be formulated as powder, requiring reconstitution before oral administration. This method, however, suffers from poor dispersibility in water due to the large number and complexity of ingredients. The second method involves microencapsulating some components of the oral skincare composition to prevent Maillard reactions between components. Microencapsulation primarily involves the electrostatic interaction between cationic chitosan and anionic polymers to generate microcapsules. Polymers with anionic charges mainly include pectin, gum arabic, and carrageenan. When performing coagulation, a common method is the compounding method. Specifically, some components of the oral skincare composition are mixed with anionicly charged polymers, which then emulsify these components. Next, the mixture is mixed with cationicly charged chitosan for coating, and then further mixed with anionicly charged polymers for coating. Finally, calcium ions are used for cross-linking. However, when emulsifying components with anionicly charged polymers, water-soluble components may be lost, leading to a decrease in the cosmetic effect. Summary of the Invention
[0007] To address the shortcomings of existing technologies, this invention provides an oral skin care composition based on the gut-skin axis theory and its preparation method. The prepared oral skin care composition has good cosmetic effects, good storage resistance, and good dispersibility in water.
[0008] To solve the above technical problems, the technical solution adopted by the present invention is as follows: A method for preparing an oral skin care composition based on the gut-skin axis theory includes: preparing active collagen tripeptide-acerculia cherry-Haematococcus pluvialis microcapsule powder, preparing a dispersant, preparing sodium hyaluronate with multiple molecular weights, and mixing them; The preparation of active collagen tripeptide-acerculia lanceolata-Haematococcus pluvialis microcapsule powder includes: preparing chitosan solution, preparing pectin solution, preparing cyclodextrin complex, preparing mixed gel, preparing active collagen tripeptide solution, preparing mixed solution, and microencapsulation. The chitosan solution is prepared by dissolving chitosan in an acetic acid solution. In the preparation of the chitosan solution, the ratio of chitosan to acetic acid solution is 20g:1000-1200mL; The chitosan has a molecular weight of 50 kDa and a degree of deacetylation of 90%. The acetic acid solution has a mass concentration of 1%; The preparation of the pectin solution involves dissolving pectin in purified water to obtain the pectin solution. In the preparation of the pectin solution, the ratio of pectin to purified water is 20g:1000-1200mL; To prepare the cyclodextrin complex, β-cyclodextrin was dissolved in purified water at 65°C, polyethylene glycol 2000 was added, the mixture was stirred for 1-1.5 hours, allowed to stand, filtered, the filter residue was collected, and the residue was dried under vacuum to obtain the cyclodextrin complex. In the preparation of the cyclodextrin complex, the ratio of β-cyclodextrin, purified water, and polyethylene glycol 2000 is 10-10.5g:110-130mL:17.5-20g. The preparation of the mixed adhesive involves mixing gum arabic and carrageenan evenly to obtain the mixed adhesive. In the preparation of the mixed gum, the mass ratio of gum arabic to carrageenan is 30:55-65; The preparation of the active collagen tripeptide solution involves taking tilapia skin, removing excess tissue, scales, and fat, washing and draining to obtain treated skin; pulverizing the treated skin to a particle size <5mm, then soaking it in acetic acid solution for 2-2.5 hours to obtain softened skin; mixing the softened skin with purified water, allowing it to stand for 8-9 hours, adding pepsin, adjusting the pH to 2, enzymatically hydrolyzing at 37℃ for 8-8.5 hours, raising the temperature to 85℃, and maintaining it at 85℃ for 10-15 minutes. Cool to 50℃, add alkaline protease, adjust pH to 8.5, and hydrolyze at 50℃ for 3.5-4 hours. Perform the first high-pressure homogenization treatment, then cool to 40℃, add trypsin, and hydrolyze at 40℃ for 1.5-2 hours. Perform the second high-pressure homogenization treatment, heat to 85℃, maintain at 85℃ for 10-15 minutes, adjust pH to 4.5, centrifuge at 8000 rpm for 15 minutes, collect the supernatant to obtain the active collagen tripeptide solution. In the preparation of the active collagen tripeptide solution, the concentration of the acetic acid solution is 0.1 mol / L; The mass ratio of softened fish skin to purified water is 1:12-15; The dosage of pepsin was 8000 U / g substrate; The amount of alkaline protease used was 120 U / g substrate; The dosage of trypsin was 60 U / g substrate; The pressure of the first high-pressure homogenization process is 40-50 MPa, and the homogenization is performed 2-3 times. The pressure of the second high-pressure homogenization process is 30-40 MPa, and the number of homogenization cycles is 2-3. To prepare the mixture, the active collagen tripeptide solution, acerola cherry powder, Haematococcus pluvialis powder, cyclodextrin complex, and mixed gel are mixed and stirred at room temperature for 30-40 minutes. Then, phosphate buffer, lecithin, and Tween 80 are added and stirred for 20-40 minutes. The mixture is then subjected to high-pressure homogenization to obtain the mixture. In the preparation of the mixture, the ratio of active collagen tripeptide solution, acerola cherry powder, Haematococcus pluvialis powder, cyclodextrin complex, mixed gel, phosphate buffer, lecithin, and Tween 80 is 2000mL:12-15g:9-10g:50-55g:115-130g:16000mL:6-7g:5-6g; The pH of the phosphate buffer solution is 7.4; The high-pressure homogenization process is performed at a pressure of 30-40 MPa, and the homogenization is repeated 2-3 times. The microencapsulation process involves mixing the mixture with a chitosan solution and then homogenizing it under high pressure to obtain a homogenate. The pectin solution is stirred at room temperature while the homogenate is added dropwise to the pectin solution. After the addition is complete, the mixture is stirred for 30-40 minutes, then calcium chloride solution is added, and the pH is adjusted to 5.5. The mixture is stirred for 50-60 minutes, then centrifuged at 5000 rpm for 15 minutes. The precipitate is collected, freeze-dried, and the active collagen tripeptide-acnifolia cherry-Haematococcus pluvialis microcapsule powder is obtained. In the microencapsulation process, the ratio of the mixture, chitosan solution, pectin solution, and calcium chloride solution is 1800mL:5400-5600mL:3700-3800mL:670-700mL. The calcium chloride solution has a mass concentration of 2%; The high-pressure homogenization process is performed at a pressure of 30-40 MPa, and the homogenization is repeated 3-4 times. The homogenizing solution is added dropwise over a period of 1-1.5 hours. The dispersant is prepared by stirring a calcium chloride solution at room temperature, adding a pectin solution dropwise, stirring for 40-50 minutes after the addition is complete, filtering, collecting the filter residue, washing with purified water, and vacuum drying to obtain cross-linked microspheres; adding the cross-linked microspheres to a sodium citrate solution, stirring at room temperature for 1.5-2 hours, filtering, collecting the filter residue, and vacuum drying to obtain the dispersant. In the preparation of the dispersant, the volume ratio of calcium chloride solution, pectin solution, and sodium citrate solution is 3000-3200:300-350:1400-1600. The calcium chloride solution has a mass concentration of 5%. The pectin solution has a mass concentration of 5%; The sodium citrate solution has a mass concentration of 5%; The pectin solution is added over a period of 50-60 minutes. The preparation of sodium hyaluronate with multiple molecular weights involves uniformly mixing high molecular weight sodium hyaluronate, medium molecular weight sodium hyaluronate, and low molecular weight sodium hyaluronate to obtain sodium hyaluronate with multiple molecular weights. In the preparation of sodium hyaluronate with multiple molecular weights, the mass ratio of high molecular weight sodium hyaluronate, medium molecular weight sodium hyaluronate, and low molecular weight sodium hyaluronate is 100-200:100:100-200. The high molecular weight sodium hyaluronate has a molecular weight of 1 million to 4 million Da; The molecular weight of the medium molecular weight sodium hyaluronate is 250,000-1,000,000 Da; The molecular weight of the small molecule sodium hyaluronate is 80,200-250,000 Da; The mixture, by mass parts, includes sodium hyaluronate of multiple molecular weight, epigallocatechin gallate, salmon nasal cartilage proteoglycan, chitosan oligosaccharide, dispersant, and bonito elastin peptide in a mixer and is mixed for 10-15 minutes. Then, active collagen tripeptide-acergot cherry-Haematococcus pluvialis microcapsule powder is added and mixed for 20-25 minutes to obtain an oral skin care composition based on the intestinal axis theory. In the mixture, the mass ratio of sodium hyaluronate with multiple molecular weights, epigallocatechin gallate, salmon nasal cartilage proteoglycan, chitosan oligosaccharide, dispersant, bonito elastin peptide, active collagen tripeptide-acetic cherry-Haematococcus pluvialis microcapsule powder is 1.5-2:2-3:1.5-2:2.5-3:10-12:3.8-4.2:114-146.
[0009] An oral skin care composition based on the gut-skin axis theory, prepared by the aforementioned method.
[0010] The gut-skin axis is a functional relationship between the gut and skin. During aging, alterations in the gut microbiota can negatively impact skin function. With age, decreased gut barrier integrity is thought to contribute to age-related functional impairments associated with the penetration of immunogenic molecules. These antigens can enter the bloodstream, preferentially accumulate in the skin, and disrupt skin homeostasis, leading to chronic skin inflammation and persistent immune responses. Short-chain fatty acids (SCFAs), products of the gut microbiota, promote the integrity of the intestinal epithelial barrier and exert anti-inflammatory effects. SCAs, particularly butyrate, control skin immune responses by increasing regulatory T cells. SCAs play a crucial role in influencing skin immune responses by modulating the skin microbiota. Given the close relationship between the gut microbiota and the skin, the gut microbiota holds significant potential for targeted therapy in treating skin aging.
[0011] The theory of the "gut-skin axis" is also recorded in traditional Chinese medicine classics. The "Treatise on the Spleen and Stomach" states: "The large intestine governs fluids, and the small intestine governs body fluids. The large and small intestines receive nourishment from the stomach, which enables them to transport body fluids to the upper burner, irrigating the skin and hair, and nourishing the interstices of the skin."
[0012] In the main pathways by which oral hyaluronic acid promotes skin health, the gut microbiota plays a crucial role as a bridge. After fermentation by gut microbiota, hyaluronic acid is utilized by them, resulting in changes in its molecular weight, a decrease in pH, and a promotion of short-chain fatty acids (SCFAs), particularly a significant increase in the content of acetic acid and propionic acid. Oral hyaluronic acid can promote the proliferation of beneficial bacteria and inhibit the growth of harmful bacteria. Bifidobacteria are positively correlated with skin hydration, elasticity, smoothness, luster, and L-value; hyaluronic acid fermentation can increase the abundance of Bifidobacteria, thereby increasing skin hydration, elasticity, luster, and smoothness. Bacteroides are significantly negatively correlated with sebum content; Bacteroides can utilize polysaccharides, dietary fiber, etc., to produce fatty acids in the gut, and hyaluronic acid fermentation can increase the abundance of Bacteroides, thereby reducing sebum content. Simultaneously, oral hyaluronic acid can also improve skin firmness and reduce dullness.
[0013] Epigallocatechin gallate (EGCG) can significantly increase the concentration of SCFAs, especially acetic acid, propionic acid, and butyric acid. SCFAs, as metabolites produced by beneficial intestinal bacteria from the metabolism of dietary fiber and other carbohydrates, have a variety of beneficial functions, such as preventing the invasion of harmful bacteria and pathogens, controlling appetite, providing energy for colon cells, and combating chronic inflammation.
[0014] Chitosan oligosaccharides can regulate gut microbiota, enhance skin barrier function, reduce the harm of harmful substances to the gut, prevent toxins and inflammatory factors in the gut from reaching the skin through blood circulation, thus avoiding skin inflammation or accelerated aging, and reduce skin moisture loss, maintaining skin hydration and elasticity. Chitosan oligosaccharides can also promote the production of SCFAs (superficial skin fatty acids), whose anti-inflammatory effects can reduce skin inflammation and alleviate inflammatory skin diseases such as acne and eczema. By improving the gut microbiota, chitosan oligosaccharides help maintain healthy skin and prevent and alleviate certain skin diseases.
[0015] Further research has shown that sodium hyaluronate, when administered orally, can be degraded by intestinal bacteria into very low molecular weight hyaluronic acid oligosaccharides, which are then transported to the skin via blood or lymphatic circulation. These oligosaccharides, acting as stimulants and raw materials, promote the synthesis of high molecular weight hyaluronic acid in skin fibroblasts. High molecular weight hyaluronic acid inhibits skin moisture loss by promoting fibroblast proliferation to fill intercellular spaces and by increasing the total amount of hyaluronic acid within skin cells. It also reduces UV-induced epidermal cell apoptosis, thus preventing increased epidermal thickness. Compared to high molecular weight hyaluronic acid, low molecular weight hyaluronic acid exhibits stronger free radical scavenging and antioxidant activity; therefore, oral administration of low molecular weight hyaluronic acid can significantly reduce oxidative stress on the skin caused by UV radiation. Under specific conditions, hyaluronic acid can react with oxidative free radicals, scavenging excess free radicals through its degradation. Therefore, both low and high molecular weight hyaluronic acid can be transferred to the skin, promoting fibroblast proliferation and hyaluronic acid resynthesis, ultimately improving skin condition and slowing down skin aging.
[0016] Simultaneously, oral hyaluronic acid can increase the moisture content of the skin after ultraviolet radiation, slow down wrinkle formation, and reduce the rate of skin aging. Oral hyaluronic acid can increase skin moisture and also has antioxidant effects in the body. Through digestion and absorption, oral hyaluronic acid increases the precursors for hyaluronic acid synthesis in the body, promoting the synthesis of hyaluronic acid in skin fibroblasts, thereby improving the skin's water retention capacity, making the skin more elastic, and reducing wrinkles.
[0017] The active collagen tripeptide of this invention utilizes bioengineering technology to extract small molecule structures from collagen molecules that are beneficial to the skin. Studies have confirmed that small molecule peptides can be directly absorbed by intestinal villi epithelial cells and exert different physiological functions in the human body, including antioxidant, free radical scavenging, and anti-aging effects.
[0018] This invention combines active collagen tripeptide, acerola cherry powder, and Haematococcus pluvialis powder, which has the following advantages: acerola cherry is rich in vitamin C, which can promote collagen synthesis; Haematococcus pluvialis contains astaxanthin, which is a strong antioxidant. Together with active collagen tripeptide, the three have a synergistic effect, enhancing the product's antioxidant and anti-aging functions, promoting skin cell regeneration, slowing down skin cell aging, replenishing and maintaining skin moisture, and reducing skin pigmentation and deposition.
[0019] This invention also incorporates salmon nasal cartilage proteoglycans, which can protect the skin barrier from damage by influencing factors that constitute the skin barrier, such as UVB-damaged keratinocytes and intercellular matrix, and maintaining ceramide and hyaluronic acid levels; and improve epidermal moisture loss by increasing ceramide levels and reducing skin free radicals that damage collagen, thus preventing skin dehydration and wrinkles caused by photoaging.
[0020] Studies show that after ultraviolet (UV) irradiation, the levels of collagenase and elastase increase sharply, while treatment with skipjack tuna elastin peptides significantly reduces their levels, with the most significant decrease in elastase. This indicates that skipjack tuna elastin peptides can reduce the increase in collagenase and elastase induced by UV radiation, thereby inhibiting their degradation of elastin and collagen. Skipjack tuna elastin peptides can also, to some extent, reduce UV-induced fibroblast apoptosis.
[0021] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) The oral skin care composition of the present invention adopts dual microencapsulation technology and pH-responsive controlled release system, which significantly improves the stability and targeted absorption efficiency of the ingredients. The inner microcapsule encapsulates active collagen tripeptide, acerola cherry powder and Haematococcus pluvialis powder, which can slow down the oxidation and degradation of the ingredients; the outer microcapsule is a chitosan-pectin-calcium ion cross-linking network, which achieves targeted release in the intestine through an alkaline environment response mechanism. Under the acidic conditions of the stomach, chitosan is protonated to form a dense gel barrier, which blocks the penetration of pepsin; after entering the intestine, pectin is deprotonated and competitively dissociates with calcium ions, triggering the rapid disintegration of the outer microcapsule, releasing the components, and achieving efficient absorption of active ingredients; (2) In the preparation method of the oral skin care composition of the present invention, a cyclodextrin complex is also used in the preparation of active collagen tripeptide-acerculia lychnophora-Haematococcus pluvialis microcapsule powder. The cyclodextrin complex is specifically a complex of β-cyclodextrin and polyethylene glycol. The β-cyclodextrin in the cyclodextrin complex is bound to the molecular chain of polyethylene glycol 2000 through hydrogen bonds, which reduces the solubility of the cyclodextrin complex. After the cyclodextrin complex is mixed with the active collagen tripeptide liquid, the water-soluble components in the active collagen tripeptide are bound to the surface of the β-cyclodextrin in the cyclodextrin complex, and the solubility is further reduced by the mutual entanglement of the molecular chains between polyethylene glycol 2000, which is more conducive to the encapsulation, thereby playing the role of fixing the water-soluble components. It can also be used to bind the cyclodextrin complex with the mixed collagen. The interaction between the components enhances the adhesion between the wall material and the core material of the microcapsule, thereby improving the storage resistance of the prepared oral skin care composition. In preparing the oral skin care composition, this invention also incorporates a dispersant. First, calcium chloride and pectin are used to prepare calcium ion-crosslinked pectin microspheres. Then, the calcium ion-crosslinked pectin microspheres are mixed with a sodium citrate solution. The calcium ion-crosslinked pectin microspheres adsorb sodium citrate from the sodium citrate solution, resulting in pectin microspheres adsorbed with sodium citrate, which serves as the dispersant. Sodium citrate improves the taste, and because it contains carboxyl groups that provide anionic charges, it generates a repulsive force with the anionic charges on the surface of the microcapsules after dispersion in water, thereby improving the dispersibility of the oral skin care composition in water. (3) The oral skin care composition of the present invention has good dispersibility in water. Take 5g of the oral skin care composition of the present invention and disperse it in 50mL of purified water, stir for 1min, and let it stand for 10min. There is no precipitation. (4) The oral skin care composition of the present invention has good storage resistance. Take 25g of the oral skin care composition of the present invention, disperse it in 50mL of purified water, add 2g of peach concentrate for flavoring, and after high temperature sterilization, the hydroxymethylfurfural (HMF) content is 97.5-119.1μg / mL; take 25g of the oral skin care composition of the present invention, let it stand for 30 days in an environment with a temperature of 40℃ and a relative humidity of 50%, disperse it in 50mL of purified water, add 2g of peach concentrate for flavoring, and after high temperature sterilization, the hydroxymethylfurfural (HMF) content is 102.7-125.5μg / mL; (5) The oral skin-beautifying composition of the present invention was subjected to a simulated gastrointestinal fluid release test. After 2 hours in simulated gastric fluid, the cumulative release rate was 12.9-15.1%, and after 8 hours in simulated intestinal fluid, the cumulative release rate was 93.5-96.8%. (6) The oral skin care composition of the present invention has good cosmetic effects and has excellent effects of moisturizing, improving skin luster, anti-wrinkle, firming and nourishing. Detailed Implementation
[0022] To provide a clearer understanding of the technical features, objectives, and effects of the present invention, specific embodiments are now described. The examples given are merely illustrative and are not intended to limit the scope of the invention.
[0023] Example 1 A method for preparing an oral skin-beautifying composition based on the gut-skin axis theory is as follows: 1. Preparation of active collagen tripeptide-acerculia lychnophora-Haematococcus pluvialis microcapsule powder: (1) Preparation of chitosan solution: Dissolve 20g of chitosan in 1000mL of acetic acid solution with a mass concentration of 1% to obtain chitosan solution; The chitosan has a molecular weight of 50 kDa and a degree of deacetylation of 90%. (2) Preparation of pectin solution: Dissolve 20g of pectin in 1000mL of purified water to obtain pectin solution; (3) Preparation of cyclodextrin complex: At 65℃, 10g of β-cyclodextrin was dissolved in 110mL of purified water, 17.5g of polyethylene glycol 2000 was added, stirred for 1h, allowed to stand, filtered, the filter residue was collected, and dried under vacuum to obtain cyclodextrin complex. (4) Preparation of mixed gum: Mix 30g of gum arabic and 55g of carrageenan evenly to obtain mixed gum; (5) Preparation of active collagen tripeptide solution: Take tilapia skin, remove excess tissue, scales, and fat, wash and drain to obtain treated fish skin; crush the treated fish skin to a particle size <5mm, then soak it in 0.1mol / L acetic acid solution for 2h to obtain softened fish skin; mix the softened fish skin with purified water at a mass ratio of 1:12, let it stand for 8h, add pepsin, control the amount of pepsin to 8000U / g substrate, adjust the pH to 2, enzymatically hydrolyze at 37℃ for 8h, raise the temperature to 85℃, maintain at 85℃ for 10min, cool to 50℃, add alkaline protease, and control the alkaline protease... The substrate concentration was 120 U / g. The pH was adjusted to 8.5, and the mixture was enzymatically hydrolyzed at 50°C for 3.5 h. High-pressure homogenization was then performed at 40 MPa for two cycles. The mixture was then cooled to 40°C, and trypsin was added at a concentration of 60 U / g. The mixture was hydrolyzed at 40°C for 1.5 h, and then homogenized at 30 MPa for two cycles. The mixture was then heated to 85°C and maintained at 85°C for 10 min. The pH was adjusted to 4.5, and the mixture was centrifuged at 8000 rpm for 15 min. The supernatant was collected to obtain the active collagen tripeptide solution. (6) Preparation of mixture: Mix 2000mL of active collagen tripeptide solution, 12g of acerola cherry powder, 9g of Haematococcus pluvialis powder, 50g of cyclodextrin complex and 115g of mixed gel, stir at room temperature for 30min, add 16000mL of phosphate buffer, 6g of lecithin and 5g of Tween 80, stir for 20min, and perform high pressure homogenization treatment. Control the pressure of high pressure homogenization treatment to be 30MPa, and homogenize twice to obtain the mixture; The pH of the phosphate buffer solution is 7.4; (7) Microencapsulation: 1800 mL of the mixture was mixed with 5400 mL of chitosan solution and then subjected to high pressure homogenization. The pressure of the high pressure homogenization was controlled at 30 MPa and the number of homogenizations was 3 times to obtain a homogenized solution. 3700 mL of pectin solution was stirred at room temperature, and the aforementioned homogenized solution was added dropwise to 3700 mL of pectin solution. The dropwise addition time was controlled at 1 h. After the dropwise addition was completed, the mixture was stirred for 30 min. 670 mL of calcium chloride solution with a mass concentration of 2% was added. Then the pH was adjusted to 5.5 and stirred for 50 min. The mixture was centrifuged at 5000 rpm for 15 min, the precipitate was collected, and the mixture was freeze-dried to obtain active collagen tripeptide-acine cherry-Haematococcus pluvialis microcapsule powder. 2. Preparation of dispersant: At room temperature, 3000 mL of 5% calcium chloride solution was stirred, and 300 mL of 5% pectin solution was added dropwise over a time of 50 min. After the addition was completed, the mixture was stirred for 40 min, filtered, and the residue was collected. The residue was washed with purified water and then dried under vacuum to obtain cross-linked microspheres. The cross-linked microspheres were then added to 1400 mL of 5% sodium citrate solution and stirred at room temperature for 1.5 h. The mixture was then filtered, and the residue was collected and dried under vacuum to obtain the dispersant. 3. Preparation of multiple molecular weight sodium hyaluronate: Mix 100g of high molecular weight sodium hyaluronate, 100g of medium molecular weight sodium hyaluronate and 100g of low molecular weight sodium hyaluronate evenly to obtain multiple molecular weight sodium hyaluronate. The high molecular weight sodium hyaluronate has a molecular weight of 1 million Da; The molecular weight of the medium molecular weight sodium hyaluronate is 250,000 Da; The molecular weight of the small molecule sodium hyaluronate is 80,200 Da; 4. Mixing: By weight, add 1.5 parts of sodium hyaluronate with multiple molecular weight, 2 parts of epigallocatechin gallate, 1.5 parts of salmon nasal cartilage proteoglycan, 2.5 parts of chitosan oligosaccharide, 10 parts of dispersant, and 3.8 parts of bonito elastin peptide to a mixer and mix for 10 minutes. Then add 114 parts of active collagen tripeptide-acericle cherry-Haematococcus pluvialis microcapsule powder and mix for 20 minutes to obtain an oral skin care composition based on the intestinal axis theory.
[0024] This embodiment also provides an oral skin care composition based on the gut-skin axis theory, prepared by the aforementioned method.
[0025] Example 2 A method for preparing an oral skin-beautifying composition based on the gut-skin axis theory is as follows: 1. Preparation of active collagen tripeptide-acerculia lychnophora-Haematococcus pluvialis microcapsule powder: (1) Preparation of chitosan solution: Dissolve 20g of chitosan in 1100mL of acetic acid solution with a mass concentration of 1% to obtain chitosan solution; The chitosan has a molecular weight of 50 kDa and a degree of deacetylation of 90%. (2) Preparation of pectin solution: Dissolve 20g of pectin in 1100mL of purified water to obtain pectin solution; (3) Preparation of cyclodextrin complex: At 65℃, 10.2g of β-cyclodextrin was dissolved in 115mL of purified water, 18g of polyethylene glycol 2000 was added, stirred for 1h, allowed to stand, filtered, the filter residue was collected, and dried under vacuum to obtain cyclodextrin complex. (4) Preparation of mixed gum: Mix 30g of gum arabic and 58g of carrageenan evenly to obtain mixed gum; (5) Preparation of active collagen tripeptide solution: Take tilapia skin, remove excess tissue, scales, and fat, wash and drain to obtain treated fish skin; crush the treated fish skin to a particle size <5mm, then soak it in 0.1mol / L acetic acid solution for 2h to obtain softened fish skin; mix the softened fish skin with purified water at a mass ratio of 1:12, let it stand for 8h, add pepsin, control the amount of pepsin to 8000U / g substrate, adjust the pH to 2, enzymatically hydrolyze at 37℃ for 8h, raise the temperature to 85℃, maintain at 85℃ for 10min, cool to 50℃, add alkaline protease, and control the alkaline protease... The substrate concentration was 120 U / g. The pH was adjusted to 8.5, and the mixture was enzymatically hydrolyzed at 50°C for 3.5 h. High-pressure homogenization was then performed at 45 MPa for two cycles. The mixture was then cooled to 40°C, and trypsin was added at a concentration of 60 U / g. The mixture was enzymatically hydrolyzed at 40°C for 1.5 h. High-pressure homogenization was then performed at 35 MPa for two cycles. The mixture was then heated to 85°C and maintained at 85°C for 10 min. The pH was adjusted to 4.5, and the mixture was centrifuged at 8000 rpm for 15 min. The supernatant was collected to obtain the active collagen tripeptide solution. (6) Preparation of mixture: 2000 mL of active collagen tripeptide solution, 13 g of acerola cherry powder, 9.2 g of Haematococcus pluvialis powder, 52 g of cyclodextrin complex and 120 g of mixed gel were mixed and stirred at room temperature for 35 min. 16000 mL of phosphate buffer, 6.5 g of lecithin and 5.2 g of Tween 80 were added and stirred for 25 min. High pressure homogenization was performed and the pressure of high pressure homogenization was controlled at 30 MPa. The homogenization was performed twice to obtain the mixture. The pH of the phosphate buffer solution is 7.4; (7) Microencapsulation: 1800 mL of the mixture was mixed with 5500 mL of chitosan solution and then subjected to high pressure homogenization. The pressure of the high pressure homogenization was controlled at 35 MPa and the number of homogenizations was 3 times to obtain a homogenized solution. 3750 mL of pectin solution was stirred at room temperature, and the aforementioned homogenized solution was added dropwise to 3750 mL of pectin solution. The dropwise addition time was controlled at 1 h. After the dropwise addition was completed, the mixture was stirred for 32 min. 680 mL of calcium chloride solution with a mass concentration of 2% was added. Then the pH was adjusted to 5.5 and stirred for 52 min. The mixture was centrifuged at 5000 rpm for 15 min, the precipitate was collected, and the mixture was freeze-dried to obtain active collagen tripeptide-acine cherry-Haematococcus pluvialis microcapsule powder. 2. Preparation of dispersant: 3100 mL of 5% calcium chloride solution was stirred at room temperature, and 320 mL of 5% pectin solution was added dropwise over a time of 52 min. After the addition was completed, the mixture was stirred for 45 min, filtered, and the residue was collected. The residue was washed with purified water and then dried under vacuum to obtain cross-linked microspheres. The cross-linked microspheres were then added to 1450 mL of 5% sodium citrate solution and stirred at room temperature for 1.5 h. The mixture was then filtered, and the residue was collected and dried under vacuum to obtain the dispersant. 3. Preparation of multiple molecular weight sodium hyaluronate: Mix 120g of high molecular weight sodium hyaluronate, 100g of medium molecular weight sodium hyaluronate and 120g of low molecular weight sodium hyaluronate evenly to obtain multiple molecular weight sodium hyaluronate. The high molecular weight sodium hyaluronate has a molecular weight of 2 million Da; The molecular weight of the medium molecular weight sodium hyaluronate is 500,000 Da; The molecular weight of the small molecule sodium hyaluronate is 100,000 Da; 4. Mixing: By weight, add 1.7 parts of sodium hyaluronate with multiple molecular weight, 2.5 parts of epigallocatechin gallate, 1.7 parts of salmon nasal cartilage proteoglycan, 2.8 parts of chitosan oligosaccharide, 11 parts of dispersant, and 4 parts of bonito elastin peptide to a mixer and mix for 12 minutes. Then add 120 parts of active collagen tripeptide-acericle cherry-Haematococcus pluvialis microcapsule powder and mix for 23 minutes to obtain an oral skin care composition based on the intestinal axis theory.
[0026] This embodiment also provides an oral skin care composition based on the gut-skin axis theory, prepared by the aforementioned method.
[0027] Example 3 A method for preparing an oral skin-beautifying composition based on the gut-skin axis theory is as follows: 1. Preparation of active collagen tripeptide-acerculia lychnophora-Haematococcus pluvialis microcapsule powder: (1) Preparation of chitosan solution: Dissolve 20g of chitosan in 1150mL of acetic acid solution with a mass concentration of 1% to obtain chitosan solution; The chitosan has a molecular weight of 50 kDa and a degree of deacetylation of 90%. (2) Preparation of pectin solution: Dissolve 20g of pectin in 1150mL of purified water to obtain pectin solution; (3) Preparation of cyclodextrin complex: At 65℃, 10.4g of β-cyclodextrin was dissolved in 125mL of purified water, 19g of polyethylene glycol 2000 was added, stirred for 1.5h, allowed to stand, filtered, the filter residue was collected, and vacuum dried to obtain cyclodextrin complex. (4) Preparation of mixed gum: Mix 30g of gum arabic and 62g of carrageenan evenly to obtain mixed gum; (5) Preparation of active collagen tripeptide solution: Take tilapia skin, remove excess tissue, scales and fat, wash and drain to obtain treated fish skin; crush the treated fish skin to a particle size <5mm, and then soak it in 0.1mol / L acetic acid solution for 2h to obtain softened fish skin; mix the softened fish skin with purified water at a mass ratio of 1:12, let it stand for 8.5h, add pepsin, control the amount of pepsin to 8000U / g substrate, adjust the pH to 2, enzymatically hydrolyze at 37℃ for 8.5h, raise the temperature to 85℃, maintain at 85℃ for 10min, cool down to 50℃, add alkaline protease, and control the alkalinity. The amount of protease used was 120 U / g substrate. The pH was adjusted to 8.5, and the enzyme was hydrolyzed at 50℃ for 4 h. After high-pressure homogenization, the pressure was controlled at 45 MPa and the number of homogenization cycles was 3. Then, the temperature was lowered to 40℃, and trypsin was added at a dosage of 60 U / g substrate. The enzyme was hydrolyzed at 40℃ for 2 h, and the enzyme was homogenized at 35 MPa and the number of homogenization cycles was 3. The temperature was raised to 85℃ and maintained at 85℃ for 10 min. The pH was adjusted to 4.5, and the enzyme was centrifuged at 8000 rpm for 15 min. The supernatant was collected to obtain the active collagen tripeptide solution. (6) Preparation of mixture: 2000mL of active collagen tripeptide solution, 14g of acerola cherry powder, 9.8g of Haematococcus pluvialis powder, 54g of cyclodextrin complex and 125g of mixed gel were mixed and stirred at room temperature for 35min. 16000mL of phosphate buffer, 6.8g of lecithin and 5.5g of Tween 80 were added and stirred for 35min. High pressure homogenization was performed, with the pressure controlled at 35MPa and the number of homogenizations being 3 times to obtain the mixture. The pH of the phosphate buffer solution is 7.4; (7) Microencapsulation: 1800 mL of the mixture was mixed with 5550 mL of chitosan solution and then subjected to high pressure homogenization. The pressure of the high pressure homogenization was controlled at 40 MPa and the number of homogenizations was 4 to obtain a homogenized solution. 3800 mL of pectin solution was stirred at room temperature, and the aforementioned homogenized solution was added dropwise to 3800 mL of pectin solution. The dropwise addition time was controlled at 1.5 h. After the dropwise addition was completed, the mixture was stirred for 40 min. 690 mL of calcium chloride solution with a mass concentration of 2% was added. Then the pH was adjusted to 5.5 and stirred for 55 min. The mixture was centrifuged at 5000 rpm for 15 min, the precipitate was collected, and the mixture was freeze-dried to obtain active collagen tripeptide-acine cherry-Haematococcus pluvialis microcapsule powder. 2. Preparation of dispersant: At room temperature, 3150 mL of 5% calcium chloride solution was stirred, and 340 mL of 5% pectin solution was added dropwise over a time of 55 min. After the addition was completed, the mixture was stirred for 50 min, filtered, and the residue was collected. The residue was washed with purified water and then dried under vacuum to obtain cross-linked microspheres. The cross-linked microspheres were then added to 1500 mL of 5% sodium citrate solution and stirred at room temperature for 2 h. The mixture was then filtered, and the residue was collected and dried under vacuum to obtain the dispersant. 3. Preparation of multiple molecular weight sodium hyaluronate: Mix 180g of high molecular weight sodium hyaluronate, 100g of medium molecular weight sodium hyaluronate and 180g of low molecular weight sodium hyaluronate evenly to obtain multiple molecular weight sodium hyaluronate. The high molecular weight sodium hyaluronate has a molecular weight of 3 million Da; The molecular weight of the medium molecular weight sodium hyaluronate is 800,000 Da; The molecular weight of the small molecule sodium hyaluronate is 200,000 Da; 4. Mixing: By weight, add 1.8 parts of sodium hyaluronate with multiple molecular weight, 2.7 parts of epigallocatechin gallate, 1.8 parts of salmon nasal cartilage proteoglycan, 2.8 parts of chitosan oligosaccharide, 12 parts of dispersant, and 4 parts of bonito elastin peptide to a mixer and mix for 14 minutes. Then add 140 parts of active collagen tripeptide-acericle cherry-Haematococcus pluvialis microcapsule powder and mix for 24 minutes to obtain an oral skin care composition based on the intestinal axis theory.
[0028] This embodiment also provides an oral skin care composition based on the gut-skin axis theory, prepared by the aforementioned method.
[0029] Example 4 A method for preparing an oral skin-beautifying composition based on the gut-skin axis theory is as follows: 1. Preparation of active collagen tripeptide-acerculia lychnophora-Haematococcus pluvialis microcapsule powder: (1) Preparation of chitosan solution: Dissolve 20g of chitosan in 1200mL of acetic acid solution with a mass concentration of 1% to obtain chitosan solution; The chitosan has a molecular weight of 50 kDa and a degree of deacetylation of 90%. (2) Preparation of pectin solution: Dissolve 20g of pectin in 1200mL of purified water to obtain pectin solution; (3) Preparation of cyclodextrin complex: At 65℃, 10.5g of β-cyclodextrin was dissolved in 130mL of purified water, 20g of polyethylene glycol 2000 was added, stirred for 1.5h, allowed to stand, filtered, the filter residue was collected, and vacuum dried to obtain cyclodextrin complex. (4) Preparation of mixed gum: Mix 30g of gum arabic and 65g of carrageenan evenly to obtain mixed gum; (5) Preparation of active collagen tripeptide solution: Take tilapia skin, remove excess tissue, scales and fat, wash and drain to obtain treated fish skin; crush the treated fish skin to a particle size <5mm, and then soak it in 0.1mol / L acetic acid solution for 2.5h to obtain softened fish skin; mix the softened fish skin with purified water at a mass ratio of 1:15, let it stand for 9h, add pepsin, control the amount of pepsin to 8000U / g substrate, adjust the pH to 2, enzymatically hydrolyze at 37℃ for 8.5h, raise the temperature to 85℃, maintain at 85℃ for 15min, cool down to 50℃, add alkaline protease, and control the alkalinity. The amount of protease used was 120 U / g substrate. The pH was adjusted to 8.5, and the enzyme was hydrolyzed at 50℃ for 4 h. After hydrolysis, the enzyme was subjected to high-pressure homogenization at 50 MPa for 3 times. Then, the temperature was lowered to 40℃, and trypsin was added at 60 U / g substrate. The enzyme was hydrolyzed at 40℃ for 2 h, and the enzyme was homogenized at 40 MPa for 3 times. The temperature was then raised to 85℃ and maintained at 85℃ for 15 min. The pH was adjusted to 4.5, and the enzyme was centrifuged at 8000 rpm for 15 min. The supernatant was collected to obtain the active collagen tripeptide solution. (6) Preparation of mixture: Mix 2000mL of active collagen tripeptide solution, 15g of acerola cherry powder, 10g of Haematococcus pluvialis powder, 55g of cyclodextrin complex and 130g of mixed gel, stir at room temperature for 30-40min, add 16000mL of phosphate buffer, 7g of lecithin and 6g of Tween 80, stir for 40min, and perform high pressure homogenization treatment. Control the pressure of high pressure homogenization treatment to be 40MPa, and homogenize 3 times to obtain the mixture; The pH of the phosphate buffer solution is 7.4; (7) Microencapsulation: 1800 mL of the mixture was mixed with 5600 mL of chitosan solution and then subjected to high pressure homogenization. The pressure of the high pressure homogenization was controlled at 40 MPa and the number of homogenizations was 4 to obtain a homogenized solution. 3800 mL of pectin solution was stirred at room temperature, and the aforementioned homogenized solution was added dropwise to 3800 mL of pectin solution. The dropwise addition time was controlled at 1.5 h. After the dropwise addition was completed, the mixture was stirred for 40 min. 700 mL of calcium chloride solution with a mass concentration of 2% was added. Then the pH was adjusted to 5.5 and stirred for 60 min. The mixture was centrifuged at 5000 rpm for 15 min, the precipitate was collected, and the mixture was freeze-dried to obtain active collagen tripeptide-acine cherry-Haematococcus pluvialis microcapsule powder. 2. Preparation of dispersant: At room temperature, 3200 mL of 5% calcium chloride solution was stirred, and 350 mL of 5% pectin solution was added dropwise over a period of 60 min. After the addition was completed, the mixture was stirred for 40 min, filtered, and the residue was collected. The residue was washed with purified water and then dried under vacuum to obtain cross-linked microspheres. The cross-linked microspheres were then added to 1600 mL of 5% sodium citrate solution and stirred at room temperature for 2 h. The mixture was then filtered, and the residue was collected and dried under vacuum to obtain the dispersant. 3. Preparation of multiple molecular weight sodium hyaluronate: Mix 200g of high molecular weight sodium hyaluronate, 100g of medium molecular weight sodium hyaluronate and 200g of low molecular weight sodium hyaluronate evenly to obtain multiple molecular weight sodium hyaluronate. The high molecular weight sodium hyaluronate has a molecular weight of 4 million Da; The molecular weight of the medium molecular weight sodium hyaluronate is 950,000 Da; The molecular weight of the small molecule sodium hyaluronate is 240,000 Da; 4. Mixing: By weight, add 2 parts of sodium hyaluronate with multiple molecular weight, 3 parts of epigallocatechin gallate, 2 parts of salmon nasal cartilage proteoglycan, 3 parts of chitosan oligosaccharide, 12 parts of dispersant, and 4.2 parts of bonito elastin peptide to a mixer and mix for 15 minutes. Then add 146 parts of active collagen tripeptide-acerculia lychnophora-Haematococcus pluvialis microcapsule powder and mix for 25 minutes to obtain an oral skin care composition based on the intestinal axis theory.
[0030] This embodiment also provides an oral skin care composition based on the gut-skin axis theory, prepared by the aforementioned method.
[0031] Comparative Example 1 Based on Example 1, this comparative example omits the step of preparing the cyclodextrin complex in step (3) of preparing the active collagen tripeptide-acrylic cherry-Haematococcus pluvialis microcapsule powder in step 1, and omits the addition of the cyclodextrin mixture in step (6) of preparing the mixture.
[0032] The rest is the same as in Example 1.
[0033] Comparative Example 2 Based on Example 1, in the preparation of active collagen tripeptide-acerculia lychnophora-Haematococcus pluvialis microcapsule powder in step 1, only alkaline protease was used for enzymatic hydrolysis in step (5) of preparing active collagen tripeptide solution. Specifically, step (5) of preparing active collagen tripeptide solution was changed to: (5) Preparation of active collagen tripeptide solution: Take tilapia skin, remove excess tissue, scales and fat, wash and drain to obtain treated fish skin; crush the treated fish skin to a particle size <5mm, and then soak it in acetic acid with a concentration of 0.1mol / L for 2h to obtain softened fish skin; mix the softened fish skin with purified water at a mass ratio of 1:12, let it stand for 8h, add alkaline protease, control the amount of alkaline protease to 120U / g substrate, adjust the pH to 8.5, enzymatically hydrolyze at 50℃ for 3.5h, perform high pressure homogenization treatment, control the pressure of high pressure homogenization treatment to 40MPa, homogenize twice, then raise the temperature to 85℃, maintain at 85℃ for 10min, adjust the pH to 4.5, centrifuge at 8000rpm for 15min, collect the supernatant to obtain active collagen tripeptide solution.
[0034] The rest is the same as in Example 1.
[0035] Comparative Example 3 This comparative example omits step 2 (preparation of the dispersant) and step 4 (addition of the dispersant) in the mixing process, based on Example 1.
[0036] The rest is the same as in Example 1.
[0037] Experimental Example 1 Take 5g of each of the oral skin care compositions prepared in Examples 1-4 and Comparative Examples 1-3, disperse them in 50mL of purified water, stir for 1min, let stand for 10min, and observe whether there is precipitation. The observation results are shown in Table 1.
[0038] Table 1. Sample precipitation status
[0039] The results above show that dispersants are beneficial for improving the dispersibility of oral skin care compositions in water.
[0040] Experimental Example 2 Take 25g each of the oral skin-beautifying compositions prepared in Examples 1-4 and Comparative Examples 1-3, disperse them in 50mL of purified water, add 2g of concentrated peach juice for flavoring, stir for 1min, fill and sterilize at 115℃ for 30min to obtain test samples. Let the test samples stand at 50℃ for 10 days, and then determine the hydroxymethylfurfural (HMF) content in the sterilized samples using spectrophotometry. The specific determination method is as follows: Standard curve preparation: Accurately weigh 0.1000 g of HMF standard into a 100 mL volumetric flask, and dilute to the mark with purified water to prepare a 1000 μg / mL HMF stock solution. Pipette 0.00 mL, 0.50 mL, 1.00 mL, 1.50 mL, 2.00 mL, 2.50 mL, and 3.00 mL of the HMF stock solution into 50 mL volumetric flasks, and dilute to the mark with purified water to obtain HMF standard solutions with concentrations of 0 μg / mL, 10 μg / mL, 20 μg / mL, 30 μg / mL, 40 μg / mL, 50 μg / mL, and 60 μg / mL, respectively. Preheat the spectrophotometer for 30 min, adjust the wavelength to 284 nm, and use purified water as a blank control to measure the absorbance of the HMF standard solutions at different concentrations. Plot a standard curve with HMF concentration (µg / mL) on the x-axis and absorbance on the y-axis, and calculate the linear regression equation.
[0041] Weigh 10.000g of sample into a 100mL centrifuge tube, add 30mL of acetonitrile, vortex for 10min to precipitate protein and extract HMF, centrifuge at 5000r / min for 15min, transfer the supernatant to another centrifuge tube, concentrate under reduced pressure at 40℃ to near dryness, reconstitute with 10mL of purified water, and filter through a 0.22μm microporous membrane to obtain the test solution. Take an appropriate amount of the pretreated sample solution in a cuvette, and measure the absorbance of the sample at 284nm wavelength, using purified water as a blank. Based on the measured absorbance, substitute it into the linear regression equation of the standard curve to calculate the HMF content in the sample. The calculation results are shown in Table 2.
[0042] Table 2. Hydroxymethylfurfural (HMF) content in samples
[0043] The results above show that the absence of cyclodextrin complex in Comparative Example 1 resulted in poor stability of the formed microcapsules. During sterilization and static treatment, the active collagen tripeptide was easily leaked, leading to an increase in the content of hydroxymethylfurfural.
[0044] Experimental Example 3 The oral skin care compositions prepared in Examples 1-4 and Comparative Examples 1-3 were sealed and left to stand for 30 days in an environment with a temperature of 40°C and a relative humidity of 50% to obtain treated samples. The treated samples were then tested according to the method of Experimental Example 2. The content of hydroxymethylfurfural (HMF) in the treated samples is shown in Table 3.
[0045] Table 3. Hydroxymethylfurfural (HMF) content in samples stored for 30 days
[0046] Comparing the above results with those of Experimental Example 2, it was found that the absence of cyclodextrin complex in Comparative Example 1 and the absence of dispersant in Comparative Example 2 both resulted in poor storage resistance of the prepared oral skin care composition.
[0047] Experimental Example 4: In vitro simulated gastrointestinal fluid release test Preparation of simulated gastric fluid: Measure 8.3 mL of concentrated hydrochloric acid and add it to 800 mL of purified water. Stir and mix thoroughly, then add purified water to bring the volume to 1 L. Mix thoroughly and adjust the pH to 1.2. Weigh 3.2 g of pepsin (porcine gastric extract, activity ≥800 U / mg) and add it to the hydrochloric acid solution. Stir until completely dissolved.
[0048] Preparation of simulated intestinal fluid: Weigh 6.8g potassium dihydrogen phosphate and 7.5g disodium hydrogen phosphate and add to 800mL purified water. Stir until completely dissolved, then add purified water to bring the volume to 1L. Mix well and adjust the pH to 6.8. Weigh 10g pancreatic enzyme (extracted from porcine pancreas, activity ≥8 USP units / mg) and add to phosphate buffer. Stir until completely dissolved.
[0049] The release media, simulating gastric and intestinal fluids, were preheated to 37±0.5℃. 5g of each of the oral skin-beautifying compositions prepared in Examples 1-4 and Comparative Examples 1-3 were added to 50mL of preheated simulated gastric fluid. The mixture was stirred at 100rpm at 37℃. 5mL of the solution was collected after 0.5h, 1h, and 2h (with an equal volume of fresh media added simultaneously) to test the release concentration of collagen tripeptide and calculate the cumulative release rate. After 2h, all gastric fluid was extracted and added to 50mL of preheated simulated intestinal fluid. The mixture was stirred at 100rpm at 37℃. 5mL of the solution was collected after 3h, 4h, 6h, and 8h (with an equal volume of fresh media added simultaneously) to test the release concentration of collagen tripeptide and calculate the cumulative release rate. The calculation results are shown in Table 4.
[0050] Table 4 Cumulative Release Rate in In Vitro Simulated Gastrointestinal Fluid Release Test
[0051] The results above show that Comparative Example 1 had a faster cumulative release rate in simulated gastric juice, indicating that the cyclodextrin complex can fix collagen tripeptide and improve the sustained-release effect.
[0052] Experimental Example 5 The oral skin-beautifying compositions prepared in Example 1 and Comparative Example 2 were mixed with purified water at a mass-volume ratio of 1g:10mL and stirred evenly to prepare an oral skin-beautifying beverage. Sixty healthy subjects aged 25-50 years were randomly divided into two groups and drank the oral skin-beautifying beverages prepared from the oral skin-beautifying compositions of Example 1 and Comparative Example 2, respectively, each drinking 200mL of the oral skin-beautifying beverage daily. The effects of the oral skin care composition were compared by a third-party testing agency by measuring the skin stratum corneum moisture content and skin luster of each group of healthy subjects before and after using the test sample. The test results are shown in Tables 5-8.
[0053] Table 5. Results of skin stratum corneum moisture content test after using the oral skin care composition of Example 1 (unit: cu).
[0054] Table 6. Results of skin stratum corneum moisture content test after using the oral skin care composition of Comparative Example 2 (unit: cu).
[0055] The results above show that the oral skin care composition prepared in Example 1 is superior to the oral skin care composition prepared in Comparative Example 2 in increasing the moisture content of the stratum corneum.
[0056] Table 7. Results of skin radiance test after using the oral skin-beautifying composition of Example 1.
[0057] Table 8. Results of skin gloss test after using the oral skin-beautifying composition of Comparative Example 2
[0058] The results above show that the oral skin care composition prepared in Example 1 is better than the oral skin care composition prepared in Comparative Example 2 in improving skin radiance.
[0059] Combining the results of Examples 1-5, it can be seen that the oral skin care composition prepared in Example 1 has better absorption than the oral skin care composition prepared in Comparative Example 2.
[0060] Experimental Example 6 To further investigate the cosmetic effects of the oral skin-beautifying compositions prepared in Examples 1-4, the oral skin-beautifying compositions prepared in Example 1 were mixed with purified water at a mass-volume ratio of 1g:10mL and stirred evenly to prepare an oral skin-beautifying beverage. Thirty healthy subjects aged 25-50 years were selected, and a third-party testing institution measured the skin elasticity of each group of healthy subjects before and after using the test sample, and analyzed skin firmness parameters, skin roughness, skin smoothness, number of wrinkles, wrinkle area, wrinkle volume, stratum corneum thickness, epidermal thickness, ECLOR, and SAAID to evaluate the cosmetic effects of the oral skin-beautifying compositions prepared in Example 1. The evaluation results are shown in Tables 9-19.
[0061] Table 9 Results of Skin Elasticity R2 Value Test
[0062] Compared to before use, after 7 days of use of the oral skin-beautifying composition of Example 1 in 30 subjects, the R2 value of skin elasticity showed a highly significant difference; after 14 days of use of the oral skin-beautifying composition of Example 1, the R2 value of skin elasticity showed a highly significant difference; after 28 days of use of the oral skin-beautifying composition of Example 1, the R2 value of skin elasticity showed a highly significant difference. This indicates that the oral skin-beautifying composition of Example 1 has a firming effect after 28 days of use.
[0063] Table 10 Results of the skin firmness parameter F4 value test
[0064] Compared to before use, after 7 days of use of the oral skin-beautifying composition of Example 1 in 30 subjects, the skin firming parameter F4 value showed a highly significant difference; after 14 days of use of the oral skin-beautifying composition of Example 1, the skin firming parameter F4 value showed a highly significant difference; after 28 days of use of the oral skin-beautifying composition of Example 1, the skin firming parameter F4 value showed a highly significant difference. This indicates that the oral skin-beautifying composition of Example 1 has a firming effect after 28 days of use.
[0065] Table 11 Results of Skin Roughness SEr Value Test
[0066] Compared to before use, after 7 days of use of the oral skin-beautifying composition of Example 1, there was no significant difference in skin roughness (SEr) values among the 30 subjects; after 14 days of use, there was a significant difference in skin roughness (SEr) values; and after 28 days of use, there was a highly significant difference in skin roughness (SEr) values. This indicates that the oral skin-beautifying composition of Example 1 has a nourishing effect after 28 days of use.
[0067] Table 12 Results of the SEsm value test for skin smoothness
[0068] Compared with before use, there was no significant difference in skin smoothness SEsm values among the 30 subjects after 7 days of using the oral skin care composition of Example 1; there was no significant difference in skin smoothness SEsm values after 14 days of using the oral skin care composition of Example 1; and there was no significant difference in skin smoothness SEsm values after 28 days of using the oral skin care composition of Example 1.
[0069] Table 13 Results of the Skin Wrinkle Count Test
[0070] Compared with before use, after 7 days of use of the oral skin care composition of Example 1, the number of skin wrinkles in 30 subjects was significantly different; after 14 days of use of the oral skin care composition of Example 1, the number of skin wrinkles was significantly different; indicating that the oral skin care composition of Example 1 has an anti-wrinkle effect after 14 days of use.
[0071] Table 14 Results of Skin Wrinkle Area Test (Unit: mm) 2 )
[0072] Compared with before use, after 7 days of use of the oral skin care composition of Example 1, the area of skin wrinkles in 30 subjects showed a significant difference; after 14 days of use of the oral skin care composition of Example 1, the area of skin wrinkles showed a highly significant difference; indicating that after 14 days of use of the oral skin care composition of Example 1, it has an anti-wrinkle effect.
[0073] Table 15 Results of Skin Wrinkle Volume Test (Unit: mm) 3 )
[0074] Compared with before use, after 7 days of use of the oral skin care composition of Example 1, there was no significant difference in skin wrinkle volume among the 30 subjects; after 14 days of use, there was a highly significant difference in skin wrinkle volume; indicating that the oral skin care composition of Example 1 has an anti-wrinkle effect after 14 days of use.
[0075] Table 16 Results of the stratum corneum thickness test
[0076] Compared with before use, after 7 days of using the oral skin care composition of Example 1, the thickness of the stratum corneum of the skin of 30 subjects improved by 18.38%; after 14 days of using the oral skin care composition of Example 1, the thickness of the stratum corneum of the skin improved by 18.38%; and after 28 days of using the oral skin care composition of Example 1, the thickness of the stratum corneum of the skin improved by 20.98%.
[0077] Table 17 Results of the skin thickness test
[0078] Compared with before use, after 7 days of using the oral skin care composition of Example 1, the epidermal thickness of the 30 subjects improved by 4.82%; after 14 days of using the oral skin care composition of Example 1, the epidermal thickness improved by 19.60%; and after 28 days of using the oral skin care composition of Example 1, the epidermal thickness improved by 25.23%.
[0079] Table 18 ELCOR Test Results
[0080] Compared with before use, after 7 days of use of the oral skin care composition of Example 1, the ELCOR of 30 subjects improved by 6.74%; after 14 days of use of the oral skin care composition of Example 1, the ELCOR improved by 17.98%; and after 28 days of use of the oral skin care composition of Example 1, the ELCOR improved by 25.84%.
[0081] Table 19 SAAID Test Results
[0082] Compared with before use, after 7 days of using the oral skin care composition of Example 1, the SAAID of 30 subjects improved by 36.36%; after 14 days of using the oral skin care composition of Example 1, the SAAID improved by 54.55%; and after 28 days of using the oral skin care composition of Example 1, the SAAID improved by 109.09%.
[0083] In summary, the oral skin care composition prepared in Example 1 not only has the effects of moisturizing and improving skin radiance, but also has anti-wrinkle, firming and nourishing effects.
Claims
1. A method for preparing an oral skin-beautifying composition based on the gut-skin axis theory, characterized in that, include: Prepare active collagen tripeptide-acerculia cherry-Haematococcus pluvialis microcapsule powder, prepare dispersant, prepare sodium hyaluronate with multiple molecular weights, and mix them; The preparation of active collagen tripeptide-acerculia lanceolata-Haematococcus pluvialis microcapsule powder includes: preparing chitosan solution, preparing pectin solution, preparing cyclodextrin complex, preparing mixed gel, preparing active collagen tripeptide solution, preparing mixed solution, and microencapsulation. To prepare the cyclodextrin complex, β-cyclodextrin was dissolved in purified water at 65°C, polyethylene glycol 2000 was added, the mixture was stirred, allowed to stand, filtered, the filter residue was collected, and the residue was dried under vacuum to obtain the cyclodextrin complex. The preparation of the active collagen tripeptide solution involves taking tilapia skin, removing excess tissue, scales, and fat, washing and draining to obtain treated skin; pulverizing the treated skin and then soaking it in acetic acid solution to obtain softened skin; mixing the softened skin with purified water, allowing it to stand, adding pepsin, adjusting the pH to 2, enzymatically hydrolyzing at 37°C, inactivating the enzyme, cooling to 50°C, adding alkaline protease, adjusting the pH to 8.5, enzymatically hydrolyzing at 50°C, performing a first high-pressure homogenization treatment, then cooling to 40°C, adding trypsin, enzymatically hydrolyzing at 40°C, performing a second high-pressure homogenization treatment, inactivating the enzyme, adjusting the pH to 4.5, centrifuging, collecting the supernatant to obtain the active collagen tripeptide solution. The preparation of the mixture involves mixing active collagen tripeptide solution, acerola cherry powder, Haematococcus pluvialis powder, cyclodextrin complex, and mixed gel, stirring at room temperature, adding phosphate buffer, lecithin, and Tween 80, stirring, and then performing high-pressure homogenization to obtain the mixture. The microencapsulation process involves mixing the mixture with a chitosan solution, followed by high-pressure homogenization to obtain a homogenized solution. The pectin solution is stirred at room temperature while the homogenized solution is added dropwise to the pectin solution. After the addition is complete, the mixture is stirred, calcium chloride solution is added, and the pH is adjusted to 5.
5. The mixture is then stirred, centrifuged, the precipitate is collected, and freeze-dried to obtain active collagen tripeptide-acnifolia cherry-Haematococcus pluvialis microcapsule powder. The dispersant was prepared by stirring a calcium chloride solution at room temperature, adding a pectin solution dropwise, stirring after the addition was complete, filtering, collecting the filter residue, washing with purified water, and drying under vacuum to obtain cross-linked microspheres; the cross-linked microspheres were then added to a sodium citrate solution, stirred at room temperature, filtered, collecting the filter residue, and drying under vacuum to obtain the dispersant. In the preparation of the dispersant, the volume ratio of calcium chloride solution, pectin solution, and sodium citrate solution is 3000-3200:300-350:1400-1600. The mixture, by mass parts, includes sodium hyaluronate of multiple molecular weight, epigallocatechin gallate, salmon nasal cartilage proteoglycan, chitosan oligosaccharide, dispersant, and bonito elastin peptide in a mixer and is mixed. Then, active collagen tripeptide-acetic cherry-Haematococcus pluvialis microcapsule powder is added and mixed to obtain an oral skin care composition based on the intestinal axis theory. In the mixture, the mass ratio of sodium hyaluronate with multiple molecular weights, epigallocatechin gallate, salmon nasal cartilage proteoglycan, chitosan oligosaccharide, dispersant, bonito elastin peptide, active collagen tripeptide-acetic cherry-Haematococcus pluvialis microcapsule powder is 1.5-2:2-3:1.5-2:2.5-3:10-12:3.8-4.2:114-146.
2. The method for preparing the oral skin-beautifying composition based on the gut-skin axis theory according to claim 1, characterized in that, The chitosan solution is prepared by dissolving chitosan in an acetic acid solution. In the preparation of the chitosan solution, the ratio of chitosan to acetic acid solution is 20g:1000-1200mL; The chitosan has a molecular weight of 50 kDa and a degree of deacetylation of 90%. The acetic acid solution has a mass concentration of 1%; The preparation of the pectin solution involves dissolving pectin in purified water to obtain the pectin solution. In the preparation of the pectin solution, the ratio of pectin to purified water is 20g:1000-1200mL.
3. The method for preparing the oral skin-beautifying composition based on the gut-skin axis theory according to claim 1, characterized in that, In the preparation of the cyclodextrin complex, the ratio of β-cyclodextrin, purified water, and polyethylene glycol 2000 is 10-10.5g:110-130mL:17.5-20g.
4. The method for preparing the oral skin-beautifying composition based on the gut-skin axis theory according to claim 1, characterized in that, The preparation of the mixed adhesive involves mixing gum arabic and carrageenan evenly to obtain the mixed adhesive. In the preparation of the mixed gum, the mass ratio of gum arabic to carrageenan is 30:55-65; In the preparation of the active collagen tripeptide solution, the concentration of the acetic acid solution is 0.1 mol / L; The mass ratio of softened fish skin to purified water is 1:12-15; The dosage of pepsin was 8000 U / g substrate; The amount of alkaline protease used was 120 U / g substrate; The dosage of trypsin was 60 U / g substrate; The pressure of the first high-pressure homogenization process is 40-50 MPa, and the homogenization is performed 2-3 times. The pressure of the second high-pressure homogenization process is 30-40 MPa, and the homogenization is performed 2-3 times.
5. The method for preparing the oral skin-beautifying composition based on the gut-skin axis theory according to claim 1, characterized in that, In the preparation of the mixture, the ratio of active collagen tripeptide solution, acerola cherry powder, Haematococcus pluvialis powder, cyclodextrin complex, mixed gel, phosphate buffer, lecithin, and Tween 80 is 2000mL:12-15g:9-10g:50-55g:115-130g:16000mL:6-7g:5-6g; The pH of the phosphate buffer solution is 7.4; The high-pressure homogenization process is carried out at a pressure of 30-40 MPa, and the homogenization is performed 2-3 times.
6. The method for preparing the oral skin-beautifying composition based on the gut-skin axis theory according to claim 1, characterized in that, In the microencapsulation process, the ratio of the mixture, chitosan solution, pectin solution, and calcium chloride solution is 1800mL:5400-5600mL:3700-3800mL:670-700mL. The calcium chloride solution has a mass concentration of 2%; The high-pressure homogenization process is performed at a pressure of 30-40 MPa, and the homogenization is repeated 3-4 times. The homogenizing solution is added over a period of 1-1.5 hours.
7. The method for preparing the oral skin-beautifying composition based on the gut-skin axis theory according to claim 1, characterized in that, In the preparation of the dispersant, the mass concentration of the calcium chloride solution is 5%; The pectin solution has a mass concentration of 5%; The sodium citrate solution has a mass concentration of 5%; The pectin solution is added over a period of 50-60 minutes.
8. The method for preparing the oral skin-beautifying composition based on the gut-skin axis theory according to claim 1, characterized in that, The preparation of sodium hyaluronate with multiple molecular weights involves uniformly mixing high molecular weight sodium hyaluronate, medium molecular weight sodium hyaluronate, and low molecular weight sodium hyaluronate to obtain sodium hyaluronate with multiple molecular weights. In the preparation of sodium hyaluronate with multiple molecular weights, the mass ratio of high molecular weight sodium hyaluronate, medium molecular weight sodium hyaluronate, and low molecular weight sodium hyaluronate is 100-200:100:100-200. The high molecular weight sodium hyaluronate has a molecular weight of 1 million to 4 million Da; The molecular weight of the medium molecular weight sodium hyaluronate is 250,000-1,000,000 Da; The molecular weight of the small molecule sodium hyaluronate is 80,200-250,000 Da.
9. An oral skin care composition based on the gut-skin axis theory, prepared by the method according to any one of claims 1-8.
Citation Information
Patent Citations
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