Oral skin beautifying composition based on intestinal axis theory and preparation method thereof
Through the oral skin beauty composition based on the intestinal skin axis theory, dual microencapsulation technology and pH-responsive controlled release system are adopted to solve the instability problems caused by collagen loss and component reaction, and efficient intestinal targeted release and skin beauty effects are achieved.
Patent Information
- Application Number
- CN202510428713.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-08
- Publication Date
- 2025-07-11
AI Technical Summary
Existing oral beauty products have problems such as collagen loss, poor effect caused by Maillard reaction, instability caused by reaction of ingredients and low bioavailability, and poor storage and dispersion.
Using oral skin beautification composition based on intestinal axes theory, the intestinal tripeptide-caused cherry-Redococcus Chrysan Radix Radix Radix microcapsules powder, multi-molecular weight sodium hyaluronate and dispersant were prepared, combined with dual microencapsulation technology and pH-responsive controlled release system, the chitosan-pectin-calcium ion crosslinking network is used to achieve targeted intestinal release, improving component stability and targeted absorption.
It improves the beauty effect, storage resistance and water dispersion of oral skin beautification compositions, ensures efficient release and absorption of active ingredients in the intestines, and significantly improves skin health and beauty effects.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of oral beauty products, and particularly relates to an oral skin-beautifying composition based on the gut-skin axis theory and a preparation method thereof. Background Art
[0002] The common problems of many oral beauty products on the market at present are: ingredient piling, concept addition, unclear oral beauty logic, and unclear action mechanism.
[0003] When collagen-containing oral beauty products are made into liquid beverages, they often face the problem of collagen loss caused by 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, proteins, etc.). In liquid beverages, collagen, as a protein, contains a large number of amino groups; while common ingredients such as fruit juices often contain reducing sugars such as glucose and fructose, and these reducing sugar molecules contain free carbonyl groups. When these reducing sugars and collagen coexist in a collagen-containing liquid beverage, during storage, the amino groups in the collagen will react with the carbonyl groups of the reducing sugars. In the initial stage of the Maillard reaction, the carbonyl group of the reducing sugar condenses with the free amino group of the collagen to form a Schiff base, and the Schiff base cyclizes to form an N-substituted glycosylamine, which then undergoes an Amadori rearrangement reaction to generate a reactive 1-amino-1-deoxy-2-ketose. As the Maillard reaction progresses, various reactive intermediates are generated in the middle stage, including hydroxymethylfurfural and other substances. These reactions will not only cause changes in the structure and properties of collagen, resulting in collagen loss and a decrease in the content of effective collagen in the product, but also have an adverse impact on the color and flavor of the product, ultimately leading to a poor use effect of the product and an inability to fully exert its due beauty effects.
[0004] In addition, the low bioavailability of food-derived bioactive peptides largely hinders their application in the development of health foods; among them, gastrointestinal digestion and degradation are the key factors restricting the bioavailability of bioactive peptides.
[0005] In summary, existing oral beauty products often only focus on collagen supplementation and do not consider the reactions between various ingredients, resulting in unsatisfactory actual beauty effects and poor storage stability of existing oral beauty products.
[0006] In view of this, the applicant has tried two methods. The first method is based on the gut-skin axis theory, adding ingredients that can change the gut microbiota to oral beauty products to improve the beauty effect. At the same time, for the convenience of storage and transportation, the oral beauty products need to be made into powders and redissolved before oral administration. However, due to the large number and complexity of the ingredients, it is easy to result in poor dispersibility in water. The second method is to microencapsulate some of the ingredients in the oral skin-beautifying composition to avoid the Maillard reaction between the ingredients. When performing microencapsulation, complex coacervation mainly occurs through the electrostatic interaction between chitosan with a cationic charge and a polymer with an anionic charge to obtain microcapsules. The polymers with anionic charges used mainly include pectin, gum arabic, carrageenan, etc. When performing complex coacervation, the commonly used method is the composite method. Specifically, some of the ingredients in the oral skin-beautifying composition are mixed with a polymer with an anionic charge, emulsified by the polymer with an anionic charge, then mixed with chitosan with a cationic charge, coated by chitosan with a cationic charge, then mixed with a polymer with an anionic charge again, coated by the polymer with an anionic charge, and finally crosslinked with calcium ions. However, when emulsifying the ingredients with a polymer with an anionic charge, for water-soluble ingredients, there is a problem of ingredient loss, resulting in a decline in the beauty effect. Summary of the Invention
[0007] In view of the deficiencies of the prior art, the present invention provides an oral skin-beautifying composition based on the gut-skin axis theory and its preparation method. The prepared oral skin-beautifying composition has good beauty effect, good storage resistance, and good dispersibility in water.
[0008] To solve the above technical problems, the technical solutions adopted by the present invention are as follows: A preparation method of an oral skin-beautifying composition based on the gut-skin axis theory, comprising: preparing active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder, preparing a dispersant, preparing sodium hyaluronate with multiple molecular weights, and mixing; The preparation of the active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder includes: preparing a chitosan solution, preparing a pectin solution, preparing a cyclodextrin complex, preparing a mixed gum, preparing an active collagen tripeptide solution, preparing a mixed solution, and microencapsulation; For the preparation of the chitosan solution, chitosan is dissolved in an acetic acid solution to obtain a chitosan solution; In the preparation of the chitosan solution, the dosage ratio of chitosan to the acetic acid solution is 20 g: 1000 - 1200 mL; The molecular weight of the chitosan is 50 KDa, and the degree of deacetylation is 90%; The mass concentration of the acetic acid solution is 1%; To prepare the pectin solution, dissolve pectin in purified water to obtain the pectin solution; In the preparation of the pectin solution, the dosage ratio of pectin to purified water is 20 g: 1000 - 1200 mL; To prepare the cyclodextrin complex, dissolve β-cyclodextrin in purified water at 65°C, add polyethylene glycol 2000 thereto, stir for 1 - 1.5 h, let stand, filter by suction, collect the filter residue, and dry it under vacuum to obtain the cyclodextrin complex; In the preparation of the cyclodextrin complex, the dosage ratio of β-cyclodextrin, purified water, and polyethylene glycol 2000 is 10 - 10.5 g: 110 - 130 mL: 17.5 - 20 g; To prepare the mixed gum, mix gum arabic and carrageenan evenly to obtain the mixed gum; In the preparation of the mixed gum, the mass ratio of gum arabic to carrageenan is 30: 55 - 65; To prepare the active collagen tripeptide solution, take tilapia fish skin, remove excess tissues, scales, and fat, wash and drain to obtain the treated fish skin; crush the treated fish skin to a particle size of <5 mm, then soak it in an acetic acid solution for 2 - 2.5 h to obtain the softened fish skin; mix the softened fish skin with purified water, let stand for 8 - 9 h, add pepsin, adjust the pH to 2, enzymatically hydrolyze at 37°C for 8 - 8.5 h, raise the temperature to 85°C, maintain at 85°C for 10 - 15 min, cool down to 50°C, add alkaline protease, adjust the pH to 8.5, enzymatically hydrolyze at 50°C for 3.5 - 4 h, perform the first high-pressure homogenization treatment, then cool down to 40°C, add trypsin, enzymatically hydrolyze at 40°C for 1.5 - 2 h, perform the second high-pressure homogenization treatment, raise the temperature to 85°C, maintain at 85°C for 10 - 15 min, adjust the pH to 4.5, centrifuge at a speed of 8000 rpm for 15 min, and 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 the softened fish skin to purified water is 1: 12 - 15; The dosage of pepsin is 8000 U / g substrate; The dosage of alkaline protease is 120 U / g substrate; The dosage of trypsin is 60 U / g substrate; The pressure of the first high-pressure homogenization treatment is 40 - 50 MPa, and the number of homogenization times is 2 - 3 times; The pressure of the second high-pressure homogenization treatment is 30 - 40 MPa, and the number of homogenization times is 2 - 3 times; To prepare the mixed solution, mix the active collagen tripeptide solution, acerola cherry powder, Haematococcus pluvialis powder, cyclodextrin complex, and mixed gum, and stir at room temperature for 30 - 40 min. Then add phosphate buffer solution, lecithin, and Tween 80, and stir for 20 - 40 min. Perform high-pressure homogenization treatment to obtain the mixed solution; In the preparation of the mixed solution, the dosage ratio of the active collagen tripeptide solution, acerola cherry powder, Haematococcus pluvialis powder, cyclodextrin complex, mixed gum, phosphate buffer solution, lecithin, and Tween 80 is 2000 mL: 12 - 15 g: 9 - 10 g: 50 - 55 g: 115 - 130 g: 16000 mL: 6 - 7 g: 5 - 6 g; The pH of the phosphate buffer solution is 7.4; For the high-pressure homogenization treatment, the pressure is 30 - 40 MPa, and the number of homogenization times is 2 - 3 times; For the microencapsulation, mix the mixed solution with the chitosan solution and perform high-pressure homogenization treatment to obtain the homogenized solution. Stir the pectin solution at room temperature, and at the same time, dropwise add the homogenized solution into the pectin solution. After the dropping is completed, stir for 30 - 40 min, add calcium chloride solution, then adjust the pH to 5.5, stir for 50 - 60 min, centrifuge at a centrifugal speed of 5000 rpm for 15 min, collect the precipitate, and freeze-dry to obtain the active collagen tripeptide-acerola cherry-Haematococcus pluvialis microcapsule powder; In the microencapsulation, the dosage ratio of the mixed solution, chitosan solution, pectin solution, and calcium chloride solution is 1800 mL: 5400 - 5600 mL: 3700 - 3800 mL: 670 - 700 mL; The mass concentration of the calcium chloride solution is 2%; For the high-pressure homogenization treatment, the pressure is 30 - 40 MPa, and the number of homogenization times is 3 - 4 times; The dropping time of the homogenized solution is 1 - 1.5 h; To prepare the dispersant, stir the calcium chloride solution at room temperature, dropwise add the pectin solution, and after the dropping is completed, stir for 40 - 50 min, then perform suction filtration, collect the filter residue, wash it with purified water, and vacuum dry it to obtain the cross-linked microspheres. Add the cross-linked microspheres into the sodium citrate solution, stir at room temperature for 1.5 - 2 h, perform suction filtration, collect the filter residue, and vacuum dry it to obtain the dispersant; In the preparation of the dispersant, the volume ratio of the calcium chloride solution, pectin solution, and sodium citrate solution is 3000 - 3200: 300 - 350: 1400 - 1600; The mass concentration of the calcium chloride solution is 5%; The mass concentration of the pectin solution is 5%; The mass concentration of the sodium citrate solution is 5%; The dropping time of the pectin solution is 50 - 60 min; To prepare sodium hyaluronate with multiple molecular weights, mix high-molecular-weight sodium hyaluronate, medium-molecular-weight sodium hyaluronate, and low-molecular-weight sodium hyaluronate evenly 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 molecular weight of the high-molecular-weight sodium hyaluronate is 1 million - 4 million Da. The molecular weight of the medium-molecular-weight sodium hyaluronate is 250,000 - 1 million Da. The molecular weight of the low-molecular-weight sodium hyaluronate is 80,200 - 250,000 Da. For the mixing, by mass parts, add sodium hyaluronate with multiple molecular weights, epigallocatechin gallate, salmon nasal cartilage proteoglycan, chitosan oligosaccharide, dispersant, and bonito elastin peptide into a mixer, mix for 10 - 15 min, then add active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder, and mix for 20 - 25 min to obtain an oral skin-beautifying composition based on the gut-skin axis theory. In the mixing, the mass ratio of sodium hyaluronate with multiple molecular weights, epigallocatechin gallate, salmon nasal cartilage proteoglycan, chitosan oligosaccharide, dispersant, bonito elastin peptide, and active collagen tripeptide - acerola 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-beautifying composition based on the gut-skin axis theory prepared by the aforementioned preparation method.
[0010] The gut-skin axis is a functional relationship between the intestine and the skin. During the aging process, changes in the gut microbiota may have a negative impact on skin function. With aging, a decrease in intestinal barrier integrity is thought to lead to aging dysfunctions related to the penetration of immunogenic molecules. These antigens can enter the bloodstream, preferentially accumulate in the skin, and disrupt skin homeostasis, resulting in chronic skin inflammation and a persistent immune response. Short-chain fatty acids (SCFAs) are products of the gut microbiota, which can promote the integrity of the intestinal epithelial barrier and exert an anti-inflammatory effect. Short-chain fatty acids, especially butyric acid, control skin immune responses by increasing regulatory T cells. Short-chain fatty acids play an important role in influencing skin immune responses by regulating the skin microbiota. The gut microbiota is closely related to the skin, and the gut microbiota has significant potential for targeted treatment of skin aging.
[0011] Regarding the "gut-skin axis" theory, there are also relevant records in traditional Chinese medical classics. "On the Theory of the Spleen and Stomach" states that the large intestine is responsible for the body fluid, and the small intestine is responsible for the liquid. The large and small intestines receive the nourishing qi from the stomach, and then they can transport body fluids to the upper jiao, irrigate the skin and hair, and fill the interstices.
[0012] Among the main ways of promoting skin health by oral administration of hyaluronic acid, the gut microbiota plays an important role as a bridge. After hyaluronic acid is fermented by the microbiota, it is utilized by the gut microbiota, with changes in molecular weight and a decrease in pH, promoting the production of short-chain fatty acids (SCFAs). In particular, the contents of acetic acid and propionic acid increase significantly. Oral administration of hyaluronic acid can promote the growth of beneficial bacteria and inhibit the proliferation of harmful bacteria. The genus Bifidobacterium is positively correlated with skin water content, elasticity, smoothness, gloss, and L value. Fermentation of hyaluronic acid can increase the abundance of the genus Bifidobacterium, and thus increase skin water content, skin elasticity, gloss, and smoothness; the genus Bacteroides is significantly negatively correlated with sebum content. The genus Bacteroides in the intestine can utilize polysaccharides, dietary fiber, etc. to produce fatty acids, etc. Fermentation of hyaluronic acid can increase the abundance of the genus Bacteroides, and thus reduce sebum content; at the same time, oral administration of hyaluronic acid can also improve skin firmness and reduce skin dullness.
[0013] Epigallocatechin gallate (EGCG) can significantly increase the concentration of SCFAs, especially the concentrations of acetic acid, propionic acid, and butyric acid. As metabolites produced by the metabolism of dietary fiber and other carbohydrates by beneficial gut bacteria, SCFAs have various 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 oligosaccharide can enhance the skin barrier function by regulating the gut microbiota, reduce the damage of harmful substances to the intestine, prevent toxins and inflammatory factors in the intestine from reaching the skin through blood circulation, thereby inducing skin inflammation or accelerating aging, reduce skin water loss, and maintain skin moisture and elasticity. Chitosan oligosaccharide can also promote the production of SCFAs, and the anti-inflammatory effect of SCFAs can reduce skin inflammatory responses and relieve skin inflammatory diseases such as acne and eczema. By improving the gut microecology, chitosan oligosaccharide helps to maintain the healthy state of the skin and prevent and relieve certain skin diseases.
[0015] Further studies have shown that sodium hyaluronate administered orally can be degraded by bacteria in the intestine into hyaluronic acid oligosaccharides with extremely low molecular weight, and then migrate to the skin through blood circulation or lymphatic circulation. As a stimulating factor and raw material, oligosaccharides can promote the synthesis of high-molecular-weight hyaluronic acid in skin fibroblasts. High-molecular-weight hyaluronic acid fills the cell gaps by promoting fibroblast proliferation and jointly inhibits the loss of skin moisture by increasing the total amount of hyaluronic acid in skin cells; high-molecular-weight hyaluronic acid can also reduce ultraviolet-induced epidermal cell apoptosis, thereby preventing the increase in epidermal thickness. Compared with high-molecular-weight hyaluronic acid, low-molecular-weight hyaluronic acid has stronger free radical scavenging and antioxidant activities. Therefore, oral administration of low-molecular-weight hyaluronic acid can significantly reduce the oxidative stress of ultraviolet irradiation on the skin. Under specific circumstances, hyaluronic acid can react with oxidative free radicals to scavenge excess free radicals through the degradation of hyaluronic acid. Therefore, both low-molecular-weight hyaluronic acid and high-molecular-weight hyaluronic acid can be transferred to the skin, promote fibroblast proliferation and hyaluronic acid resynthesis, and ultimately achieve the effect of improving skin condition and slowing down skin aging.
[0016] At the same time, oral administration of hyaluronic acid can also increase the water content in the skin after ultraviolet irradiation, slow down the formation of wrinkles and reduce the skin aging rate. Oral administration of hyaluronic acid can increase the water content of human skin and also has an antioxidant effect in vivo. Hyaluronic acid is digested and absorbed through oral administration, increasing the precursors for the synthesis of hyaluronic acid in the body, promoting the synthesis of hyaluronic acid in skin fibroblasts, thereby improving the water retention performance of the skin, making the skin elastic and reducing wrinkles.
[0017] The active collagen tripeptide of the present invention utilizes bioengineering technology to intercept the small molecular structure useful for the skin in collagen molecules; research has confirmed that small molecular peptides can be directly absorbed by small intestinal villus epithelial cells and play different physiological functions in the human body, having antioxidant, free radical scavenging and anti-aging effects.
[0018] The present invention combines active collagen tripeptide, acerola cherry powder and Haematococcus pluvialis powder, with the following advantages: Acerola cherries are rich in vitamin C, which can promote collagen synthesis. Haematococcus pluvialis contains astaxanthin, which is a strong antioxidant. The three of them, together with active collagen tripeptide, synergistically enhance the antioxidant and anti-aging functions of the product, promote skin cell regeneration, slow down skin cell aging, supplement and maintain skin moisture, and reduce skin pigment generation and precipitation.
[0019] The present invention also adds salmon nasal cartilage proteoglycan. Salmon nasal cartilage proteoglycan can protect the skin barrier from being damaged by affecting the factors constituting the skin barrier, such as UVB-damaged keratinocytes and the extracellular matrix, and maintaining the content of ceramides and hyaluronic acid; it improves epidermal water loss by increasing the ceramide level and reducing skin free radicals that damage collagen, and prevents skin water shortage and wrinkles caused by photoaging.
[0020] Research shows that after ultraviolet irradiation, the contents of collagenase and elastase increase sharply, while after treatment with skipjack elastin peptide, their contents decrease significantly, among which the decrease in elastase content is the most obvious. This indicates that skipjack elastin peptide can reduce the increase in collagenase and elastase caused by ultraviolet radiation, thereby inhibiting their degradation of elastin and collagen. Skipjack elastin peptide can, to a certain extent, reduce the apoptosis of fibroblasts induced by ultraviolet rays.
[0021] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) The oral beauty composition of the present invention adopts a double microencapsulation technology and a pH-responsive controlled release system, significantly improving the stability and targeted absorption efficiency of the components. The inner microcapsule encapsulates active collagen tripeptide, acerola cherry powder, and Haematococcus pluvialis powder, which can slow down the oxidation and degradation of the components; the outer microcapsule is a chitosan-pectin-calcium ion cross-linked network, which realizes intestinal targeted release through an alkaline environment response mechanism. Under the acidic conditions of the stomach, chitosan is protonated to form a dense gel barrier to block the penetration of pepsin; after entering the intestine, pectin is deprotonated, competitively dissociates with calcium ions, triggering the rapid disintegration of the outer microcapsule and releasing the components to achieve the efficient absorption of the active ingredients; (2) In the preparation method of the oral beauty composition of the present invention, a cyclodextrin complex is also used in the preparation of the active collagen tripeptide-acerola cherry-Haematococcus pluvialis microcapsule powder. The cyclodextrin complex is specifically a complex of β-cyclodextrin and polyethylene glycol. β-cyclodextrin in the cyclodextrin complex binds to the molecular chain of polyethylene glycol 2000 through hydrogen bonds, reducing the solubility of the cyclodextrin complex; after mixing with the cyclodextrin complex and the active collagen tripeptide solution, the water-soluble components in the active collagen tripeptide bind to the surface of β-cyclodextrin in the cyclodextrin complex, and the entanglement of the molecular chains between polyethylene glycol 2000 is utilized to further reduce the solubility, which is more conducive to encapsulation, thereby playing a role in fixing the water-soluble components. It can also improve the adhesion between the wall material and the core material of the microcapsule through the interaction between the cyclodextrin complex and the mixed gum, thereby improving the storage resistance of the prepared oral beauty composition; when preparing the oral beauty composition of the present invention, a dispersant is also added. When preparing the dispersant, calcium chloride and pectin are first used to prepare calcium ion-crosslinked pectin microspheres, and then the calcium ion-crosslinked pectin microspheres are mixed with a sodium citrate solution. The calcium ion-crosslinked pectin microspheres adsorb sodium citrate in the sodium citrate solution to obtain pectin microspheres adsorbed with sodium citrate, that is, the dispersant. Sodium citrate plays a role in improving the taste, and sodium citrate contains carboxyl groups, which can provide anionic charges. After being dispersed in water, it generates a repulsive force with the anionic charges on the surface of the microcapsule, thereby improving the dispersibility of the oral beauty composition in water; (3)The oral beauty composition of the present invention has good dispersibility in water. Take 5 g of the oral beauty composition of the present invention and disperse it in 50 mL of purified water, stir for 1 min, and let it stand for 10 min, and there is no precipitation. (4)The oral beauty composition of the present invention has good storage resistance. Take 25 g of the oral beauty composition of the present invention, disperse it in 50 mL of purified water, add 2 g of peach concentrate for flavoring, after high-temperature sterilization, the content of hydroxymethylfurfural (HMF) is 97.5 - 119.1 μg / mL; take 25 g of the oral beauty composition of the present invention, stand it in an environment with a temperature of 40 °C and a relative humidity of 50% for 30 d, disperse it in 50 mL of purified water, add 2 g of peach concentrate for flavoring, after high-temperature sterilization, the content of hydroxymethylfurfural (HMF) is 102.7 - 125.5 μg / mL. (5)Perform a simulated gastrointestinal fluid release test on the oral beauty composition of the present invention. After 2 h in simulated gastric fluid, the cumulative release rate is 12.9 - 15.1%, and after 8 h in simulated intestinal fluid, the cumulative release rate is 93.5 - 96.8%. (6)The oral beauty composition of the present invention has good beauty effects and has excellent effects of moisturizing, improving skin gloss, anti-wrinkle, firming, and nourishing. Specific Embodiments
[0022] For a clearer understanding of the technical features, objectives, and effects of the present invention, the specific embodiments of the present invention are now described. The examples given are only to explain the present invention and do not limit the scope of the present invention.
[0023] Example 1 A preparation method of an oral beauty composition based on the enterocutaneous axis theory is as follows: 1. Prepare active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder: (1)Prepare a chitosan solution: Dissolve 20 g of chitosan in 1000 mL of acetic acid solution with a mass concentration of 1% to obtain a chitosan solution. The molecular weight of the chitosan is 50 KDa, and the degree of deacetylation is 90%. (2)Prepare a pectin solution: Dissolve 20 g of pectin in 1000 mL of purified water to obtain a pectin solution. (3)Prepare a cyclodextrin complex: At 65 °C, dissolve 10 g of β-cyclodextrin in 110 mL of purified water, add 17.5 g of polyethylene glycol 2000 thereto, stir for 1 h, let it stand, filter by suction, collect the filter residue, and dry it under vacuum to obtain a cyclodextrin complex. (4)Prepare a mixed gum: Mix 30 g of gum arabic and 55 g of carrageenan evenly to obtain a mixed gum. (5)Preparation of active collagen tripeptide solution: Take tilapia fish skin, remove excess tissues, scales and fat, wash and drain to obtain the treated fish skin; crush the treated fish skin to a particle size of <5 mm, then soak it in an acetic acid solution with a concentration of 0.1 mol / L for 2 h to obtain the softened fish skin; mix the softened fish skin with purified water at a mass ratio of 1:12, let it stand for 8 h, add pepsin, control the dosage of pepsin to be 8000 U / g substrate, adjust the pH to 2, enzymatically hydrolyze at 37 °C for 8 h, raise the temperature to 85 °C, maintain at 85 °C for 10 min, cool down to 50 °C, add alkaline protease, control the dosage of alkaline protease to be 120 U / g substrate, adjust the pH to 8.5, enzymatically hydrolyze at 50 °C for 3.5 h, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 40 MPa, the number of homogenization times to be 2 times, then cool down to 40 °C, add trypsin, control the dosage of trypsin to be 60 U / g substrate, enzymatically hydrolyze at 40 °C for 1.5 h, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 30 MPa, the number of homogenization times to be 2 times, raise the temperature to 85 °C, maintain at 85 °C for 10 min, adjust the pH to 4.5, centrifuge at a speed of 8000 rpm for 15 min, collect the supernatant to obtain the active collagen tripeptide solution; (6)Preparation of the mixed solution: Mix 2000 mL of active collagen tripeptide solution, 12 g of acerola cherry powder, 9 g of Haematococcus pluvialis powder, 50 g of cyclodextrin complex, and 115 g of mixed gum, stir at room temperature for 30 min, add 16000 mL of phosphate buffer solution, 6 g of lecithin, and 5 g of Tween 80, stir for 20 min, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 30 MPa, the number of homogenization times to be 2 times to obtain the mixed solution; The pH of the phosphate buffer solution is 7.4; (7)Microencapsulation: Mix 1800 mL of the mixed solution with 5400 mL of chitosan solution, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 30 MPa, the number of homogenization times to be 3 times to obtain the homogenized solution; stir the 3700 mL of pectin solution at room temperature, and at the same time drop the aforementioned homogenized solution into the 3700 mL of pectin solution, control the dropping time to be 1 h, stir for 30 min after the dropping is completed, add 670 mL of calcium chloride solution with a mass concentration of 2%, then adjust the pH to 5.5, stir for 50 min, centrifuge at a speed of 5000 rpm for 15 min, collect the precipitate, and freeze-dry to obtain the active collagen tripeptide-acerola cherry-Haematococcus pluvialis microcapsule powder; 2. Preparation of dispersant: Stir 3000 mL of calcium chloride solution with a mass concentration of 5% at room temperature, add dropwise 300 mL of pectin solution with a mass concentration of 5%, control the dropping time to 50 min, stir for 40 min after the dropping is completed, perform suction filtration, collect the filter residue, wash it with purified water, and then dry it under vacuum to obtain crosslinked microspheres; Add the aforementioned crosslinked microspheres to 1400 mL of sodium citrate solution with a mass concentration of 5%, stir at room temperature for 1.5 h, perform suction filtration, collect the filter residue, and dry it under vacuum to obtain the dispersant; 3. Preparation of sodium hyaluronate with multiple molecular weights: Mix 100 g of high-molecular-weight sodium hyaluronate, 100 g of medium-molecular-weight sodium hyaluronate, and 100 g of low-molecular-weight sodium hyaluronate evenly to obtain sodium hyaluronate with multiple molecular weights; The molecular weight of the high-molecular-weight sodium hyaluronate is 1 million Da; The molecular weight of the medium-molecular-weight sodium hyaluronate is 250,000 Da; The molecular weight of the low-molecular-weight sodium hyaluronate is 80,200 Da; 4. Mixing: By mass, add 1.5 parts of sodium hyaluronate with multiple molecular weights, 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 into a mixer, mix for 10 min, then add 114 parts of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder, and mix for 20 min to obtain an oral skin-beautifying composition based on the enterocutaneous axis theory.
[0024] This example also provides an oral skin-beautifying composition based on the enterocutaneous axis theory prepared by the aforementioned preparation method.
[0025] Example 2 A preparation method of an oral skin-beautifying composition based on the enterocutaneous axis theory is as follows: 1. Preparation of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder: (1) Preparation of chitosan solution: Dissolve 20 g of chitosan in 1100 mL of acetic acid solution with a mass concentration of 1% to obtain a chitosan solution; The molecular weight of the chitosan is 50 KDa, and the degree of deacetylation is 90%; (2) Preparation of pectin solution: Dissolve 20 g of pectin in 1100 mL of purified water to obtain a pectin solution; (3) Preparation of cyclodextrin complex: At 65 °C, dissolve 10.2 g of β-cyclodextrin in 115 mL of purified water, add 18 g of polyethylene glycol 2000 thereto, stir for 1 h, let it stand, perform suction filtration, collect the filter residue, and dry it under vacuum to obtain the cyclodextrin complex; (4) Preparation of mixed gum: Mix 30 g of gum arabic and 58 g of carrageenan evenly to obtain a mixed gum; (5) Preparation of active collagen tripeptide solution: Take tilapia fish skin, remove excess tissues, fish scales, and fat, wash and drain to obtain the treated fish skin; crush the treated fish skin to a particle size of <5 mm, then soak it in an acetic acid solution with a concentration of 0.1 mol / L for 2 h to obtain the softened fish skin; mix the softened fish skin and purified water at a mass ratio of 1:12, let it stand for 8 h, add pepsin, control the dosage of pepsin to be 8000 U / g of substrate, adjust the pH to 2, enzymatically hydrolyze at 37 °C for 8 h, raise the temperature to 85 °C, maintain at 85 °C for 10 min, lower the temperature to 50 °C, add alkaline protease, control the dosage of alkaline protease to be 120 U / g of substrate, adjust the pH to 8.5, enzymatically hydrolyze at 50 °C for 3.5 h, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 45 MPa, the number of homogenization times to be 2 times, then lower the temperature to 40 °C, add trypsin, control the dosage of trypsin to be 60 U / g of substrate, enzymatically hydrolyze at 40 °C for 1.5 h, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 35 MPa, the number of homogenization times to be 2 times, raise the temperature to 85 °C, maintain at 85 °C for 10 min, adjust the pH to 4.5, centrifuge at a centrifugal speed of 8000 rpm for 15 min, collect the supernatant to obtain the active collagen tripeptide solution; (6) Preparation of the mixed solution: Mix 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 gum, stir at room temperature for 35 min, add 16000 mL of phosphate buffer solution, 6.5 g of lecithin, and 5.2 g of Tween 80, stir for 25 min, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 30 MPa, the number of homogenization times to be 2 times, to obtain the mixed solution; The pH of the phosphate buffer solution is 7.4; (7) Microencapsulation: Mix 1800 mL of the mixed solution and 5500 mL of chitosan solution, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 35 MPa, the number of homogenization times to be 3 times, to obtain the homogenized solution; Stir the 3750 mL of pectin solution at room temperature, and at the same time dropwise add the aforementioned homogenized solution to the 3750 mL of pectin solution, control the dropping time to be 1 h, stir for 32 min after the dropping is completed, add 680 mL of calcium chloride solution with a mass concentration of 2%, then adjust the pH to 5.5, stir for 52 min, centrifuge at a centrifugal speed of 5000 rpm for 15 min, collect the precipitate, and freeze-dry to obtain the active collagen tripeptide-acerola cherry-Haematococcus pluvialis microcapsule powder; 2. Preparation of the dispersant: Stir 3100 mL of a calcium chloride solution with a mass concentration of 5% at room temperature, dropwise add 320 mL of a pectin solution with a mass concentration of 5%, control the dropping time to be 52 min, stir for 45 min after the dropping is completed, perform suction filtration, collect the filter residue, wash it with purified water, and then dry it in vacuo to obtain crosslinked microspheres; Add the aforementioned crosslinked microspheres to 1450 mL of a sodium citrate solution with a mass concentration of 5%, stir at room temperature for 1.5 h, perform suction filtration, collect the filter residue, and dry it in vacuo to obtain the dispersant; 3. Preparation of hyaluronic acid sodium with multiple molecular weights: Mix 120 g of high-molecular-weight hyaluronic acid sodium, 100 g of medium-molecular-weight hyaluronic acid sodium, and 120 g of low-molecular-weight hyaluronic acid sodium evenly to obtain hyaluronic acid sodium with multiple molecular weights; The molecular weight of the high-molecular-weight hyaluronic acid sodium is 2 million Da; The molecular weight of the medium-molecular-weight hyaluronic acid sodium is 500,000 Da; The molecular weight of the low-molecular-weight hyaluronic acid sodium is 100,000 Da; 4. Mixing: By mass, add 1.7 parts of hyaluronic acid sodium with multiple molecular weights, 2.5 parts of epigallocatechin gallate, 1.7 parts of salmon nasal cartilage proteoglycan, 2.8 parts of chitosan oligosaccharide, 11 parts of the dispersant, and 4 parts of bonito elastin peptide to a mixer, mix for 12 min, add 120 parts of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder, and mix for 23 min to obtain an oral skin-beautifying composition based on the intestinal-skin axis theory.
[0026] This example also provides an oral skin-beautifying composition based on the intestinal-skin axis theory prepared by the aforementioned preparation method.
[0027] Example 3 A preparation method of an oral skin-beautifying composition based on the intestinal-skin axis theory is as follows: 1. Preparation of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder: (1) Preparation of the chitosan solution: Dissolve 20 g of chitosan in 1150 mL of an acetic acid solution with a mass concentration of 1% to obtain the chitosan solution; The molecular weight of the chitosan is 50 KDa, and the degree of deacetylation is 90%; (2) Preparation of the pectin solution: Dissolve 20 g of pectin in 1150 mL of purified water to obtain the pectin solution; (3) Preparation of the cyclodextrin complex: At 65 °C, dissolve 10.4 g of β-cyclodextrin in 125 mL of purified water, add 19 g of polyethylene glycol 2000 thereto, stir for 1.5 h, let it stand, perform suction filtration, collect the filter residue, and dry it in vacuo to obtain the cyclodextrin complex; (4) Preparation of the mixed gum: Mix 30 g of gum arabic and 62 g of carrageenan evenly to obtain the mixed gum; (5) Preparation of active collagen tripeptide solution: Take tilapia fish skin, remove excess tissues, scales and fat, wash and drain to obtain the treated fish skin; crush the treated fish skin to a particle size of <5 mm, then soak it in an acetic acid solution with a concentration of 0.1 mol / L for 2 h to obtain the softened fish skin; mix the softened fish skin with purified water at a mass ratio of 1:12, let it stand for 8.5 h, add pepsin, control the dosage of pepsin to be 8000 U / g of substrate, adjust the pH to 2, enzymatically hydrolyze at 37 °C for 8.5 h, raise the temperature to 85 °C, maintain at 85 °C for 10 min, cool down to 50 °C, add alkaline protease, control the dosage of alkaline protease to be 120 U / g of substrate, adjust the pH to 8.5, enzymatically hydrolyze at 50 °C for 4 h, perform high-pressure homogenization treatment, control the pressure of the high-pressure homogenization treatment to be 45 MPa, and the number of homogenization times to be 3 times, then cool down to 40 °C, add trypsin, control the dosage of trypsin to be 60 U / g of substrate, enzymatically hydrolyze at 40 °C for 2 h, perform high-pressure homogenization treatment, control the pressure of the high-pressure homogenization treatment to be 35 MPa, and the number of homogenization times to be 3 times, raise the temperature to 85 °C, maintain at 85 °C for 10 min, adjust the pH to 4.5, centrifuge at a speed of 8000 rpm for 15 min, collect the supernatant to obtain the active collagen tripeptide solution; (6) Preparation of the mixed solution: Mix 2000 mL of the active collagen tripeptide solution, 14 g of acerola cherry powder, 9.8 g of Haematococcus pluvialis powder, 54 g of cyclodextrin complex, and 125 g of mixed gum, stir at room temperature for 35 min, add 16000 mL of phosphate buffer solution, 6.8 g of lecithin, and 5.5 g of Tween 80, stir for 35 min, perform high-pressure homogenization treatment, control the pressure of the high-pressure homogenization treatment to be 35 MPa, and the number of homogenization times to be 3 times to obtain the mixed solution; The pH of the phosphate buffer solution is 7.4; (7) Microencapsulation: Mix 1800 mL of the mixed solution with 5550 mL of chitosan solution, perform high-pressure homogenization treatment, control the pressure of the high-pressure homogenization treatment to be 40 MPa, and the number of homogenization times to be 4 times to obtain the homogenized solution; stir the 3800 mL of pectin solution at room temperature, and at the same time drop the aforementioned homogenized solution into the 3800 mL of pectin solution, control the dropping time to be 1.5 h, stir for 40 min after the dropping is completed, add 690 mL of calcium chloride solution with a mass concentration of 2%, then adjust the pH to 5.5, stir for 55 min, centrifuge at a speed of 5000 rpm for 15 min, collect the precipitate, and freeze-dry to obtain the active collagen tripeptide-acerola cherry-Haematococcus pluvialis microcapsule powder; 2. Preparation of the dispersant: Stir 3150 mL of a calcium chloride solution with a mass concentration of 5% at room temperature, add dropwise 340 mL of a pectin solution with a mass concentration of 5%, control the dropping time to be 55 min, stir for 50 min after the dropping is completed, perform suction filtration, collect the filter residue, wash it with purified water, and then dry it in vacuo to obtain crosslinked microspheres; add the aforementioned crosslinked microspheres to 1500 mL of a sodium citrate solution with a mass concentration of 5%, stir at room temperature for 2 h, perform suction filtration, collect the filter residue, and dry it in vacuo to obtain the dispersant; 3. Preparation of multi-molecular-weight sodium hyaluronate: Mix 180 g of high-molecular-weight sodium hyaluronate, 100 g of medium-molecular-weight sodium hyaluronate, and 180 g of low-molecular-weight sodium hyaluronate evenly to obtain multi-molecular-weight sodium hyaluronate; The molecular weight of the high-molecular-weight sodium hyaluronate is 3 million Da; The molecular weight of the medium-molecular-weight sodium hyaluronate is 0.8 million Da; The molecular weight of the low-molecular-weight sodium hyaluronate is 0.2 million Da; 4. Mixing: By mass, add 1.8 parts of multi-molecular-weight sodium hyaluronate, 2.7 parts of epigallocatechin gallate, 1.8 parts of salmon nasal cartilage proteoglycan, 2.8 parts of chitosan oligosaccharide, 12 parts of the dispersant, and 4 parts of bonito elastin peptide into a mixer, mix for 14 min, then add 140 parts of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder, and mix for 24 min to obtain an oral skin-beautifying composition based on the gut-skin axis theory.
[0028] This example also provides an oral skin-beautifying composition based on the gut-skin axis theory prepared by the aforementioned preparation method.
[0029] Example 4 A preparation method of an oral skin-beautifying composition based on the gut-skin axis theory is as follows: 1. Preparation of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder: (1) Preparation of the chitosan solution: Dissolve 20 g of chitosan in 1200 mL of an acetic acid solution with a mass concentration of 1% to obtain the chitosan solution; The molecular weight of the chitosan is 50 KDa, and the degree of deacetylation is 90%; (2) Preparation of the pectin solution: Dissolve 20 g of pectin in 1200 mL of purified water to obtain the pectin solution; (3) Preparation of the cyclodextrin complex: At 65 °C, dissolve 10.5 g of β-cyclodextrin in 130 mL of purified water, add 20 g of polyethylene glycol 2000 thereto, stir for 1.5 h, let it stand, perform suction filtration, collect the filter residue, and dry it in vacuo to obtain the cyclodextrin complex; (4) Preparation of the mixed gum: Mix 30 g of gum arabic and 65 g of carrageenan evenly to obtain the mixed gum; (5) Preparation of active collagen tripeptide solution: Take tilapia fish skin, remove excess tissue, fish scales and fat, wash and drain to obtain the treated fish skin; crush the treated fish skin to a particle size of <5 mm, then soak it in an acetic acid solution with a concentration of 0.1 mol / L for 2.5 h to obtain the softened fish skin; mix the softened fish skin with purified water at a mass ratio of 1:15, let it stand for 9 h, add pepsin, control the dosage of pepsin to be 8000 U / g of substrate, adjust the pH to 2, enzymatically hydrolyze at 37 °C for 8.5 h, raise the temperature to 85 °C, maintain at 85 °C for 15 min, cool down to 50 °C, add alkaline protease, control the dosage of alkaline protease to be 120 U / g of substrate, adjust the pH to 8.5, enzymatically hydrolyze at 50 °C for 4 h, perform high-pressure homogenization treatment, control the pressure of the high-pressure homogenization treatment to be 50 MPa, and the number of homogenization times to be 3 times, then cool down to 40 °C, add trypsin, control the dosage of trypsin to be 60 U / g of substrate, enzymatically hydrolyze at 40 °C for 2 h, perform high-pressure homogenization treatment, control the pressure of the high-pressure homogenization treatment to be 40 MPa, and the number of homogenization times to be 3 times, raise the temperature to 85 °C, maintain at 85 °C for 15 min, adjust the pH to 4.5, centrifuge at a speed of 8000 rpm for 15 min, collect the supernatant to obtain the active collagen tripeptide solution; (6) Preparation of the mixed solution: Mix 2000 mL of active collagen tripeptide solution, 15 g of acerola cherry powder, 10 g of Haematococcus pluvialis powder, 55 g of cyclodextrin complex, and 130 g of mixed gum, stir at room temperature for 30 - 40 min, add 16000 mL of phosphate buffer solution, 7 g of lecithin, and 6 g of Tween 80, stir for 40 min, perform high-pressure homogenization treatment, control the pressure of the high-pressure homogenization treatment to be 40 MPa, and the number of homogenization times to be 3 times to obtain the mixed solution; The pH of the phosphate buffer solution is 7.4; (7) Microencapsulation: Mix 1800 mL of the mixed solution with 5600 mL of chitosan solution, perform high-pressure homogenization treatment, control the pressure of the high-pressure homogenization treatment to be 40 MPa, and the number of homogenization times to be 4 times to obtain the homogenized solution; stir the 3800 mL of pectin solution at room temperature, and at the same time drop the aforementioned homogenized solution into the 3800 mL of pectin solution, control the dropping time to be 1.5 h, stir for 40 min after the dropping is completed, add 700 mL of calcium chloride solution with a mass concentration of 2%, then adjust the pH to 5.5, stir for 60 min, centrifuge at a speed of 5000 rpm for 15 min, collect the precipitate, and freeze-dry to obtain the active collagen tripeptide-acerola cherry-Haematococcus pluvialis microcapsule powder; 2. Preparation of dispersant: Stir 3200 mL of calcium chloride solution with a mass concentration of 5% at room temperature, add 350 mL of pectin solution with a mass concentration of 5% dropwise, control the dropping time to 60 min, stir for 40 min after the dropping is completed, perform suction filtration, collect the filter residue, wash it with purified water, and then dry it under vacuum to obtain crosslinked microspheres; Add the aforementioned crosslinked microspheres to 1600 mL of sodium citrate solution with a mass concentration of 5%, stir at room temperature for 2 h, perform suction filtration, collect the filter residue, and dry it under vacuum to obtain the dispersant; 3. Preparation of sodium hyaluronate with multiple molecular weights: Mix 200 g of high-molecular-weight sodium hyaluronate, 100 g of medium-molecular-weight sodium hyaluronate, and 200 g of low-molecular-weight sodium hyaluronate evenly to obtain sodium hyaluronate with multiple molecular weights; The molecular weight of the high-molecular-weight sodium hyaluronate is 4 million Da; The molecular weight of the medium-molecular-weight sodium hyaluronate is 950,000 Da; The molecular weight of the low-molecular-weight sodium hyaluronate is 240,000 Da; 4. Mixing: By mass, add 2 parts of sodium hyaluronate with multiple molecular weights, 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, mix for 15 min, then add 146 parts of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder, and mix for 25 min to obtain an oral skin-beautifying composition based on the gut-skin axis theory.
[0030] This example also provides an oral skin-beautifying composition based on the gut-skin axis theory prepared by the aforementioned preparation method.
[0031] Comparative Example 1 Based on Example 1, in the preparation of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder in Step 1 of this comparative example, the step (3) of preparing the cyclodextrin complex is omitted, and in the step (6) of preparing the mixed solution, the addition of the cyclodextrin mixture is omitted.
[0032] The rest is the same as Example 1.
[0033] Comparative Example 2 Based on Example 1, in the preparation of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder in Step 1 of this comparative example, in the step (5) of preparing the active collagen tripeptide solution, only alkaline protease is used for enzymatic hydrolysis. Specifically, the step (5) of preparing the active collagen tripeptide solution is changed to: (5) Preparation of active collagen tripeptide solution: Take tilapia fish skin, remove excess tissues, scales and fat, wash and drain to obtain the treated fish skin; Crush the treated fish skin to a particle size of <5 mm, then soak it in acetic acid with a concentration of 0.1 mol / L for 2 h to obtain the softened fish skin; Mix the softened fish skin and purified water at a mass ratio of 1:12, let it stand for 8 h, add alkaline protease, control the dosage of alkaline protease to be 120 U / g of substrate, adjust the pH to 8.5, enzymatically hydrolyze at 50 °C for 3.5 h, perform high-pressure homogenization treatment, control the pressure of high-pressure homogenization treatment to be 40 MPa, and the number of homogenization times to be 2 times, then raise the temperature to 85 °C, maintain at 85 °C for 10 min, adjust the pH to 4.5, centrifuge at a speed of 8000 rpm for 15 min, collect the supernatant to obtain the active collagen tripeptide solution.
[0034] The rest is the same as in Example 1.
[0035] Comparative Example 3 Based on Example 1, this comparative example omits the preparation of the dispersant in the second step and the addition of the dispersant in the fourth step of mixing.
[0036] The rest is the same as in Example 1.
[0037] Test Example 1 Take 5 g of each of the oral beauty compositions prepared in Examples 1-4 and Comparative Examples 1-3, disperse them in 50 mL of purified water respectively, stir for 1 min, let it stand for 10 min, observe whether there is precipitation, and the observation results are shown in Table 1.
[0038] Table 1 Precipitation situation of samples
[0039] It can be seen from the above results that the dispersant is beneficial to improving the dispersibility of the oral beauty composition in water.
[0040] Test Example 2 Take 25 g of each of the oral beauty compositions prepared in Examples 1-4 and Comparative Examples 1-3, disperse them in 50 mL of purified water respectively, add 2 g of peach concentrate for flavoring, stir for 1 min, fill and sterilize, specifically sterilize at 115 °C for 30 min to obtain the test samples, let the test samples stand at 50 °C for 10 d, and then use the spectrophotometric method to determine the content of hydroxymethylfurfural (HMF) in the sterilized samples. The specific determination method is as follows: Standard curve drawing: Accurately weigh 0.1000 g of HMF standard into a 100 mL volumetric flask, dilute to the mark with purified water to prepare a 1000 μg / mL HMF stock solution. Respectively pipette 0.00 mL, 0.50 mL, 1.00 mL, 1.50 mL, 2.00 mL, 2.50 mL, 3.00 mL of the HMF stock solution into 50 mL volumetric flasks, 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, 60 μg / mL respectively. Preheat the spectrophotometer for 30 min, adjust the wavelength to 284 nm, use purified water as the blank control, and sequentially measure the absorbance of HMF standard solutions with different concentrations. Take the HMF concentration (μg / mL) as the abscissa and the absorbance as the ordinate to draw the standard curve and calculate the linear regression equation.
[0041] Weigh 10.000 g of the sample into a 100 mL centrifuge tube, add 30 mL of acetonitrile, vortex for 10 min to precipitate proteins and extract HMF, centrifuge at 5000 r / min for 15 min, transfer the supernatant to another centrifuge tube, concentrate it to nearly dry under reduced pressure at 40 °C, add 10 mL of purified water for reconstitution, and then filter through a 0.22 μm microporous membrane to obtain the test solution. Take an appropriate amount of the pretreated sample solution in a cuvette, measure the absorbance of the sample at a wavelength of 284 nm with purified water as the blank. According to the measured absorbance, substitute it into the linear regression equation of the standard curve to calculate the content of HMF in the sample, and the calculation results are shown in Table 2.
[0042] Table 2 Content of hydroxymethylfurfural HMF in the sample
[0043] It can be seen from the above results that no cyclodextrin complex was added in Comparative Example 1, resulting in poor stability of the formed microcapsules. During sterilization and static treatment, it is easy to cause leakage of active collagen tripeptide, leading to an increase in the content of hydroxymethylfurfural.
[0044] Test Example 3 Seal the oral beauty compositions prepared in Examples 1 - 4 and Comparative Examples 1 - 3 respectively, and let them stand in an environment with a temperature of 40 °C and a relative humidity of 50% for 30 d to obtain treated samples. Then test the treated samples according to the method of Test Example 2, and the content of hydroxymethylfurfural HMF in the obtained treated samples is shown in Table 3.
[0045] Table 3 Content of hydroxymethylfurfural HMF in the samples stored for 30 d
[0046] After comparing the above results with those of Test Example 2, it was found that the lack of cyclodextrin complex in Comparative Example 1 and the lack of dispersant in Comparative Example 2 both led to poor storage stability of the prepared oral beauty composition.
[0047] Test Example 4 In vitro simulated gastrointestinal fluid release test Prepare simulated gastric fluid: Measure 8.3 mL of concentrated hydrochloric acid and add it to 800 mL of purified water, stir and mix evenly, then add purified water to make up to 1 L, mix evenly, and adjust the pH to 1.2. Weigh 3.2 g of pepsin (porcine gastric origin, activity ≥ 800 U / mg) and add it to the hydrochloric acid solution, stir until completely dissolved.
[0048] Prepare simulated intestinal fluid: Weigh 6.8 g of potassium dihydrogen phosphate and 7.5 g of disodium hydrogen phosphate and add them to 800 mL of purified water, stir until completely dissolved, continue to add purified water to make up to 1 L, mix evenly, and adjust the pH to 6.8. Weigh 10 g of pancreatin (extracted from porcine pancreas, activity ≥ 8 USP units / mg) and add it to the phosphate buffer solution, stir until completely dissolved.
[0049] Preheat the release media, simulated gastric fluid and simulated intestinal fluid, to 37 ± 0.5 °C. Take 5 g each of the oral beauty compositions prepared in Examples 1-4 and Comparative Examples 1-3, and add them separately to 50 mL of preheated simulated gastric fluid. Stir at a stirring speed of 100 rpm at 37 °C, and take 5 mL of the solution at 0.5 h, 1 h, and 2 h respectively (while supplementing an equal volume of fresh media), and test the release concentration of collagen tripeptide and calculate the cumulative release rate; and after 2 h, draw out all the gastric fluid, add 50 mL of preheated simulated intestinal fluid respectively, stir at a stirring speed of 100 rpm at 37 °C, and take 5 mL of the solution at 3 h, 4 h, 6 h, and 8 h respectively (while supplementing an equal volume of fresh media), 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 of in vitro simulated gastrointestinal fluid release test
[0051] From the above results, it can be seen that the cumulative release rate of Comparative Example 1 in simulated gastric fluid is relatively fast, indicating that the cyclodextrin complex can play a role in fixing collagen tripeptide and improving the sustained release effect.
[0052] Test Example 5 Mix the oral beauty compositions prepared in Example 1 and Comparative Example 2 with purified water at a mass-to-volume ratio of 1 g:10 mL, stir evenly to prepare an oral beauty drink. Select 60 healthy subjects aged 25-50 years, randomly divide them into 2 groups, and drink the oral beauty drinks prepared from the oral beauty compositions of Example 1 and Comparative Example 2 respectively, 200 mL of the oral beauty drink per day; A third-party testing agency measured the water content of the skin stratum corneum and skin glossiness of each group of healthy subjects before and after using the test samples to compare the effects of the oral beauty composition. The test results are shown in Tables 5-8.
[0053] Table 5 Test results of the water content of the skin stratum corneum after using the oral beauty composition of Example 1 (unit: c.u.)
[0054] Table 6 Test results of the water content of the skin stratum corneum after using the oral beauty composition of Comparative Example 2 (unit: c.u.)
[0055] It can be seen from the above results that the oral beauty composition prepared in Example 1 is superior to the oral beauty composition prepared in Comparative Example 2 in increasing the water content of the skin stratum corneum.
[0056] Table 7 Test results of the skin glossiness after using the oral beauty composition of Example 1
[0057] Table 8 Test results of the skin glossiness after using the oral beauty composition of Comparative Example 2
[0058] It can be seen from the above results that the oral beauty composition prepared in Example 1 is superior to the oral beauty composition prepared in Comparative Example 2 in increasing the skin glossiness.
[0059] Combining the results of Test Examples 1-5, it can be seen that the oral beauty composition prepared in Example 1 is better in absorbability than the oral beauty composition prepared in Comparative Example 2.
[0060] Test Example 6 To further study the beauty effects of the oral beauty compositions prepared in Examples 1-4, the oral beauty composition prepared in Example 1 was mixed with purified water at a mass-to-volume ratio of 1 g:10 mL, stirred evenly to prepare an oral beauty drink. Thirty healthy subjects aged 25-50 were selected. A third-party testing agency analyzed skin firmness parameters, skin roughness, skin smoothness, number of wrinkles, wrinkle area, wrinkle volume, stratum corneum thickness, epidermal thickness, ECLOR, SAAID by measuring the skin elasticity of each group of healthy subjects before and after using the test samples to evaluate the beauty effects of the oral beauty composition prepared in Example 1. The evaluation results are shown in Tables 9-19.
[0061] Table 9 Test results of the skin elasticity R2 value
[0062] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, there was a highly significant difference in the R2 value of skin elasticity; after 14 days of using the oral beauty composition of Example 1, there was a highly significant difference in the R2 value of skin elasticity; after 28 days of using the oral beauty composition of Example 1, there was a highly significant difference in the R2 value of skin elasticity. It shows that after 28 days of using the oral beauty composition of Example 1, there is a firming effect.
[0063] Table 10 Test results of skin firming parameter F4 value
[0064] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, there was a highly significant difference in the F4 value of skin firming parameter; after 14 days of using the oral beauty composition of Example 1, there was a highly significant difference in the F4 value of skin firming parameter; after 28 days of using the oral beauty composition of Example 1, there was a highly significant difference in the F4 value of skin firming parameter. It shows that after 28 days of using the oral beauty composition of Example 1, there is a firming effect.
[0065] Table 11 Test results of skin roughness SEr value
[0066] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, there was no significant difference in the SEr value of skin roughness; after 14 days of using the oral beauty composition of Example 1, there was a significant difference in the SEr value of skin roughness; after 28 days of using the oral beauty composition of Example 1, there was a highly significant difference in the SEr value of skin roughness. It shows that after 28 days of using the oral beauty composition of Example 1, there is a nourishing effect.
[0067] Table 12 Test results of skin smoothness SEsm value
[0068] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, there was no significant difference in the SEsm value of skin smoothness; after 14 days of using the oral beauty composition of Example 1, there was no significant difference in the SEsm value of skin smoothness; after 28 days of using the oral beauty composition of Example 1, there was no significant difference in the SEsm value of skin smoothness.
[0069] Table 13 Test results of skin wrinkle number
[0070] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, there was a significant difference in the number of skin wrinkles; after 14 days of using the oral beauty composition of Example 1, there was a significant difference in the number of skin wrinkles; it shows that after 14 days of using the oral beauty composition of Example 1, there is an anti-wrinkle effect.
[0071] Table 14 Skin wrinkle area test results (unit: mm 2 )
[0072] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, there was a significant difference in the skin wrinkle area; after 14 days of using the oral beauty composition of Example 1, there was a highly significant difference in the skin wrinkle area; it shows that after 14 days of using the oral beauty composition of Example 1, there is an anti-wrinkle effect.
[0073] Table 15 Skin wrinkle volume test results (unit: mm 3 )
[0074] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, there was no significant difference in the skin wrinkle volume; after 14 days of using the sample, there was a highly significant difference in the skin wrinkle volume; it shows that after 14 days of using the oral beauty composition of Example 1, there is an anti-wrinkle effect.
[0075] Table 16 Stratum corneum thickness test results
[0076] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, the skin stratum corneum thickness improved by 18.38%; after 14 days of using the oral beauty composition of Example 1, the skin stratum corneum thickness improved by 18.38%; after 28 days of using the oral beauty composition of Example 1, the skin stratum corneum thickness improved by 20.98%.
[0077] Table 17 Epidermal thickness test results
[0078] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, the skin epidermal thickness improved by 4.82%; after 14 days of using the oral beauty composition of Example 1, the skin epidermal thickness improved by 19.60%; after 28 days of using the oral beauty composition of Example 1, the skin epidermal thickness improved by 25.23%.
[0079] Table 18 ELCOR test results
[0080] Compared with before use, after 7 days of using the oral beauty composition of Example 1 by 30 subjects, the ELCOR improved by 6.74%; after 14 days of using the oral beauty composition of Example 1, the ELCOR improved by 17.98%; after 28 days of using the oral beauty 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 beauty composition of Example 1 by 30 subjects, the SAAID improved by 36.36%; after 14 days of using the oral beauty composition of Example 1, the SAAID improved by 54.55%; after 28 days of using the oral beauty composition of Example 1, the SAAID improved by 109.09%.
[0083] In summary, the oral beauty composition prepared in Example 1 not only has the effects of moisturizing and improving skin gloss, but also has the effects of anti-wrinkle, firming and nourishing.
Claims
1. A preparation method of an oral skin-beautifying composition based on the enterocutaneous axis theory, characterized in that, Including: Preparing active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder, preparing a dispersant, preparing sodium hyaluronate with multiple molecular weights, and mixing; The preparation of active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder includes: preparing a chitosan solution, preparing a pectin solution, preparing a cyclodextrin complex, preparing a mixed gum, preparing an active collagen tripeptide solution, preparing a mixed solution, and microencapsulation; For the preparation of the cyclodextrin complex, at 65 °C, dissolve β - cyclodextrin in purified water, add polyethylene glycol 2000 thereto, stir, let stand, filter by suction, collect the filter residue, and vacuum dry to obtain the cyclodextrin complex; For the microencapsulation, after mixing the mixed solution with the chitosan solution, perform high - pressure homogenization treatment to obtain a homogenized solution; stir the pectin solution at room temperature, and at the same time dropwise add the homogenized solution to the pectin solution. After the addition is completed, stir, add a calcium chloride solution, then adjust the pH to 5.5, stir, centrifuge, collect the precipitate, and freeze - dry to obtain active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder; For the preparation of the dispersant, stir the calcium chloride solution at room temperature, dropwise add the pectin solution, stir after the addition is completed, filter by suction, collect the filter residue, wash it with purified water, and then vacuum dry to obtain cross - linked microspheres; add the cross - linked microspheres to a sodium citrate solution, stir at room temperature, filter by suction, collect the filter residue, and vacuum dry to obtain the dispersant.
2. The preparation method of the oral beauty skin composition based on the gut-skin axis theory according to claim 1, wherein For the preparation of the chitosan solution, dissolve chitosan in an acetic acid solution to obtain a chitosan solution; In the preparation of the chitosan solution, the dosage ratio of chitosan to the acetic acid solution is 20 g: 1000 - 1200 mL; The molecular weight of the chitosan is 50 KDa, and the degree of deacetylation is 90%; The mass concentration of the acetic acid solution is 1%; For the preparation of the pectin solution, dissolve pectin in purified water to obtain a pectin solution; In the preparation of the pectin solution, the dosage ratio of pectin to purified water is 20 g: 1000 - 1200 mL.
3. The preparation method of the oral beauty composition based on the gut-skin axis theory according to claim 1, wherein, In the preparation of the cyclodextrin complex, the dosage ratio of β - cyclodextrin, purified water, and polyethylene glycol 2000 is 10 - 10.5 g: 110 - 130 mL: 17.5 - 20 g.
4. The preparation method of the oral beauty composition based on the gut-skin axis theory according to claim 1, wherein, For the preparation of the mixed gum, mix gum arabic and carrageenan evenly to obtain the mixed gum; In the preparation of the mixed gum, the mass ratio of gum arabic to carrageenan is 30: 55 - 65; For the preparation of the active collagen tripeptide solution, take tilapia fish skin, remove excess tissues, fish scales, and fat, wash and drain to obtain the treated fish skin; crush the treated fish skin, then soak it in an acetic acid solution to obtain the softened fish skin; mix the softened fish skin with purified water, let stand, add pepsin, adjust the pH to 2, enzymatically hydrolyze at 37 °C, inactivate the enzyme, cool down to 50 °C, add alkaline protease, adjust the pH to 8.5, enzymatically hydrolyze at 50 °C, perform the first high - pressure homogenization treatment, then cool down to 40 °C, add trypsin, enzymatically hydrolyze at 40 °C, perform the second high - pressure homogenization treatment, inactivate the enzyme, adjust the pH to 4.5, centrifuge, and 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 the softened fish skin to purified water is 1:12 - 15; The dosage of pepsin is 8000U / g of substrate; The dosage of alkaline protease is 120U / g of substrate; The dosage of trypsin is 60U / g of substrate; The pressure of the first high-pressure homogenization treatment is 40 - 50MPa, and the number of homogenization times is 2 - 3 times; The pressure of the second high-pressure homogenization treatment is 30 - 40MPa, and the number of homogenization times is 2 - 3 times.
5. The preparation method of the oral skin-beautifying composition based on the gut-skin axis theory according to claim 1, wherein For the preparation of the mixed solution, after mixing the active collagen tripeptide solution, acerola cherry powder, haematococcus pluvialis powder, cyclodextrin complex, and mixed gum, stir at room temperature, add phosphate buffer solution, lecithin, and Tween 80, stir, and perform high-pressure homogenization treatment to obtain the mixed solution; In the preparation of the mixed solution, the dosage ratio of the active collagen tripeptide solution, acerola cherry powder, haematococcus pluvialis powder, cyclodextrin complex, mixed gum, phosphate buffer solution, 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 pressure of the high-pressure homogenization treatment is 30 - 40MPa, and the number of homogenization times is 2 - 3 times.
6. The preparation method of the oral beauty composition based on the gut-skin axis theory according to claim 1, characterized in that, In the microencapsulation, the dosage ratio of the mixed solution, chitosan solution, pectin solution, and calcium chloride solution is 1800mL:5400 - 5600mL:3700 - 3800mL:670 - 700mL; The mass concentration of the calcium chloride solution is 2%; The pressure of the high-pressure homogenization treatment is 30 - 40MPa, and the number of homogenization times is 3 - 4 times; The dropping time of the homogenate is 1 - 1.5h.
7. The preparation method of the oral beauty composition based on the gut-skin axis theory according to claim 1, characterized in that, In the preparation of the dispersant, the volume ratio of the calcium chloride solution, pectin solution, and sodium citrate solution is 3000 - 3200:300 - 350:1400 - 1600; The mass concentration of the calcium chloride solution is 5%; The mass concentration of the pectin solution is 5%; The mass concentration of the sodium citrate solution is 5%; The dropping time of the pectin solution is 50 - 60min.
8. The preparation method of the oral beauty composition based on the gut-skin axis theory according to claim 1, characterized in that, For the preparation of multi-molecular weight sodium hyaluronate, mix the high-molecular weight sodium hyaluronate, medium-molecular weight sodium hyaluronate, and low-molecular weight sodium hyaluronate evenly to obtain multi-molecular weight sodium hyaluronate; In the preparation of multi-molecular weight sodium hyaluronate, the mass ratio of the high-molecular weight sodium hyaluronate, medium-molecular weight sodium hyaluronate, and low-molecular weight sodium hyaluronate is 100 - 200:100:100 - 200; The molecular weight of the high-molecular weight sodium hyaluronate is 1 million - 4 million Da; The molecular weight of the medium-molecular weight sodium hyaluronate is 0.25 million - 1 million Da; The molecular weight of the low-molecular weight sodium hyaluronate is 0.0802 million - 0.25 million Da.
9. The preparation method of the oral beauty composition based on the gut-skin axis theory according to claim 1, wherein For the mixing, by mass, add the multi-molecular weight sodium hyaluronate, epigallocatechin gallate, salmon nasal cartilage proteoglycan, chitosan oligosaccharide, dispersant, and bonito elastin peptide into a mixer, mix, add the active collagen tripeptide - acerola cherry - haematococcus pluvialis microcapsule powder, and mix to obtain an oral skin beautifying composition based on the intestinal-skin 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, and active collagen tripeptide - acerola 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.
10. An oral skin - beautifying composition based on the enterocutaneous axis theory prepared by the preparation method according to any one of claims 1 - 9.