Composition beneficial to skin phase and bone phase synergistic anti-aging and preparation method thereof
By combining chicory extract, inulin, and carbon dioxide hop extract with milk mineral salts and collagen, a stable Pickering emulsion is formed, which solves the problem of collagen and calcium precipitation in liquid formulations and achieves a safe and long-lasting synergistic anti-aging effect on both bone and skin.
Patent Information
- Application Number
- CN202511105176.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-07
- Publication Date
- 2025-10-28
AI Technical Summary
Existing technologies for delaying bone and skin aging have drawbacks such as high surgical risks, short duration of effect, and muscle stiffness. Furthermore, collagen and calcium tend to precipitate in liquid formulations, affecting medication adherence and stability.
By combining chicory extract, inulin, and carbon dioxide hop extract with milk mineral salts and collagen, a stable Pickering emulsion is formed through chelation and cross-linking, which improves calcium absorption and utilization and antioxidant capacity, and synergistically combats aging.
This invention achieves a composition with high stability and long shelf life, which can effectively prevent facial bone loss, slow down skin aging, improve skin firmness, enhance facial support, improve facial depressions and wrinkles, and improve medication adherence.
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Figure CN120836751A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of health food, and in particular relates to compositions that help the skin and bone structure to work together to resist aging and their preparation methods. Background Technology
[0002] Facial aging is not a gradual process, but rather a progressive aging process from the inside out, from the bones to the skin. Facial bones are the supporting structure for facial soft tissues, providing a framework for muscles, fat, and skin. The main characteristics of skeletal aging are bone loss, weakened support, resulting in sagging and hollowing of the facial bones, a blurred jawline, a longer philtrum, and sunken eye sockets and temples. Skin aging is the most obvious and common manifestation of aging, characterized by dull skin with fine lines, loss of collagen and elasticity, and loose skin.
[0003] Facial bones (especially key areas like the cheekbones and mandible) undergo bone resorption with age, resulting in reduced volume and decreased bone density, significantly weakening their support. This process causes the soft tissues attached to the bones (such as muscles and fat pads) to lose their stable mechanical foundation, becoming a core contributing factor to deepening nasolabial folds and downward displacement of the nasolabial groove. When bone atrophy continues, the fixed position of the soft tissues is forced to change, leading to sagging of the malar fat pads and collapse of the cheekbones, further deepening the structural defects of nasolabial folds and tear troughs.
[0004] Bone loss also disrupts the original facial proportions: for example, brow bone resorption increases the distance between the eyebrows and eyes, while jawbone atrophy shortens the lower face, leading to an overall facial disharmony (such as a flatter and wider face, and a receding jaw), resulting in an uncoordinated aging appearance. Furthermore, changes in facial bones affect local blood circulation and nutrient supply mechanisms, reducing skin metabolism and self-repair capabilities, and accelerating external signs of aging (such as sagging skin, dryness, and wrinkle formation).
[0005] These changes create a chain reaction: loss of cheekbones directly leads to sagging cheeks, while jawbone atrophy causes a "cheeky face" (blurred jawline and soft tissue accumulation), ultimately resulting in a tired and aged appearance. Studies have shown that such combined changes in bone and skin structure can significantly increase visual age. Current technologies for delaying bone and skin aging typically employ bone reshaping surgery or fillers such as hyaluronic acid to improve facial aging. However, these methods have significant drawbacks, including high surgical risks, postoperative asymmetry, short-lasting effects, and muscle stiffness.
[0006] Application number CN201310150625.1 discloses a compound health food for improving menopausal syndrome in women and its preparation method. This invention uses collagen peptides as a base and mixes 5-40 parts by weight of hop hydroalcohol extract, 5-40 parts by weight of collagen peptides, 5-30 parts by weight of glucosamine, 5-30 parts by weight of chondroitin sulfate, 5-30 parts by weight of calcium citrate, calcium carbonate, or calcium lactate, and 0.05-0.3 parts by weight of vitamin D3 or vitamin D to obtain a compound health food containing collagen peptides that has a dual effect of improving menopausal syndrome in women and maintaining bone health. This compound health food, while improving menopausal symptoms and preventing osteoporosis, can also improve women's skin condition and delay aging.
[0007] There is an urgent need to develop a new type of liquid formulation that combines safety and long-lasting effects to improve medication adherence among middle-aged and elderly patients, and to address the problem of collagen and calcium easily precipitating in liquid formulations by optimizing the formula and process. Summary of the Invention
[0008] To address the aforementioned problems, this invention proposes a composition and its preparation method that contribute to the synergistic anti-aging effects of skin and bone tissue, exhibiting high stability, long shelf life, good freeze-thaw stability, and high calcium absorption and utilization rate.
[0009] This invention has the following characteristics: The composition that helps the skin and bone structure fight synergistically includes 1200g of milk mineral salts, 2500g of collagen, 325g of sodium chondroitin sulfate, 225g of N-acetylglucosamine, 20-40g of chicory extract, 20-40g of carbon dioxide hop extract, 40g of thickener, 1000g of inulin, 300g of concentrated fruit juice, 90g of citric acid, and water. The chicory extract is prepared by the following method: (1) the washed and dried chicory fleshy root is cut into thin slices and soaked in a 0.1% citric acid aqueous solution at 40-60℃ for 15 minutes, and then drained; (2) the soaked and drained chicory fleshy root is dried in a microwave oven. (3) The microwave-dried chicory fleshy root is crushed and passed through a 20-mesh sieve. 80% ethanol is added at a solid-liquid ratio of 1:12. After stirring evenly, it is ultrasonically extracted at 0-20℃ for 30-60 min. The first filtrate and the first residue are obtained by filtration. (4) 25% ethanol is added to the first residue. The pH of the added Na2CO3 solution is adjusted to 8.5. The residue is heated and refluxed at 75℃ for 2 h. The second filtrate and the second residue are obtained by filtration. (5) The two filtrates are combined. The pH is adjusted to 7 with citric acid solution. After stirring evenly, the residue is concentrated by rotary evaporation under reduced pressure to a specific gravity of 1.06-1.10 to obtain chicory extract.
[0010] Chicory extract is a dark brown, viscous liquid or paste obtained by roasting slices of chicory's fleshy root and then extracting it with a solvent. It has a roasted aroma similar to coffee and caramel, with a strong coffee flavor. The main components of chicory extract are chicory polysaccharides and aromatic substances. The aromatic substances mainly include flavonoids and polyphenols. Among them, chicoric acid, chlorogenic acid, and caffeic acid all contain phenolic hydroxyl functional groups, which readily chelate with metal ions in milky mineral salts in solution to form chelates.
[0011] The existing chicory extract contains relatively low levels of total chicory flavonoids and total chicory polyphenols. Further increases in these levels are needed to enhance the stability of the emulsion mineral salts, promote calcium absorption, and slow bone loss. Simultaneously, increasing the content of total chicory flavonoids and total chicory polyphenols can also improve the composition's antioxidant capacity, increase collagen content in the skin, improve skin firmness, and prevent facial depressions and wrinkles. This achieves synergistic anti-aging effects on both bone and skin structure.
[0012] Carbon dioxide hop extract is a concentrated extract from hops using supercritical carbon dioxide extraction technology. Hop flavonoids, in particular, have estrogen-like effects and can regulate hormone levels, making them widely used in Europe to alleviate menopausal hot flashes and postmenopausal osteoporosis. Carbon dioxide hop extract also possesses excellent antioxidant capabilities, scavenging free radicals and neutralizing oxidative stress-induced cell damage.
[0013] The combination of chicory extract, inulin, and carbon dioxide hop extract has a synergistic effect, improving the stability of emulsion mineral salts in emulsions. Chicory extract and inulin promote calcium absorption and slow bone loss, while carbon dioxide hop extract regulates hormone levels, maintains facial bone density, and inhibits muscle atrophy. Total chicory flavonoids also possess strong antioxidant capabilities, preventing skin cell aging and degeneration.
[0014] This invention's composition, through calcium supplementation, prevents facial bone loss, delays bone aging, avoids facial bone atrophy and loss, and improves facial support; through the antioxidant capabilities of chicory extract, inulin, and hops extract, it delays skin aging, improves the skin's ability to remove oxygen free radicals, reduces skin damage caused by free radicals, and thus slows down skin aging; and through collagen, it increases the collagen content in the skin, increases skin firmness, and prevents facial depressions and wrinkles. Thus, it achieves synergistic anti-aging effects on both bone and skin.
[0015] In the preparation method of chicory extract, the thin slices are slices with a thickness of 1-2 mm.
[0016] Soaking in a 0.1% citric acid aqueous solution can not only improve the permeability and shorten the soaking time, avoiding starch gelatinization in the chicory fleshy root, but also reduce the oxidative loss of flavonoids during the extraction process and increase the content of total chicory flavonoids in the chicory extract.
[0017] Drain the water until there are no drips on the surface, and it feels moist but not sticky to the touch.
[0018] The preferred method is to centrifuge at 2000 r / min for 30 s to drain the water.
[0019] In step (3), the microwave drying time is 8-12 minutes.
[0020] This invention utilizes microwave drying of chicory fleshy roots, which increases the content of total chicory flavonoids and total chicory polyphenols in chicory extract. This avoids the loss of total chicory flavonoids and total chicory polyphenols during the baking process.
[0021] To prevent localized overheating and carbonization during microwave drying, the chicory root is first soaked and drained to improve the uniformity of microwave drying. The soaking time needs to be strictly controlled. If the time is too short, the chicory root will lack sufficient moisture, making it prone to carbonization during microwave drying; if the soaking time is too long, the starch in the chicory root will gelatinize, affecting the content of total chicory flavonoids and total chicory polyphenols in the chicory extract.
[0022] The first extraction in this invention uses an 80% ethanol solution for low-temperature ultrasonic extraction at 0-20℃ for 30-60 minutes, which improves the extraction efficiency of total chicory flavonoids and total chicory polyphenols, avoids the loss of heat-sensitive components in total chicory flavonoids, and retains the phenolic acid components in total chicory polyphenols. The second extraction uses an alkaline ethanol solution, which increases the content of chicory flavonoids in the chicory extract.
[0023] The total flavonoid content of chicory extract is 31.32-32.57 mg / g, and the total polyphenol content of chicory is 9.73-9.85 mg / g.
[0024] The chicory extract prepared using the method of this invention has high levels of total chicory flavonoids and total chicory polyphenols. The prepared composition, which contributes to synergistic anti-aging of the skin and bone structure, exhibits excellent freeze-thaw stability and a long shelf life.
[0025] The thickener is low-methoxyl pectin.
[0026] Low-methoxyl pectin and inulin, combined with calcium ions, hop extract, and chicory extract, form a three-dimensional network "egg-box" structure, encapsulating and fixing solid milk mineral salts within the "egg-box" structure. This reduces the aggregation and precipitation of milk mineral salts, improves their stability in the emulsion, and prevents precipitation.
[0027] Inulin can improve the absorption and utilization rate of calcium in milk mineral salts. Chicory polyphenols, hop polyphenols, milk mineral salts, low-methoxyl pectin, and inulin can form a multi-component complex in aqueous solution, creating a highly stable Pickering emulsion. This not only avoids protein precipitation caused by polyphenols but also prevents precipitation of milk mineral salts. Furthermore, the researchers of this invention have found that the emulsion of this invention has good freeze-thaw stability, which can significantly extend the shelf life of the composition.
[0028] The composition that promotes synergistic anti-aging of skin and bone structure includes 30g of chicory extract and 30g of carbon dioxide hop extract. The composition is prepared by the following method, comprising the following steps: S1, adding the prescribed amounts of chicory extract, carbon dioxide hop extract, thickener, and inulin to 5L of water and stirring until homogeneous to obtain solution 1; S2, high-speed shearing and stirring solution 1, during which the prescribed amounts of milk mineral salt, N-acetylglucosamine, chondroitin sulfate sodium, and collagen are slowly added to solution 1, maintaining the temperature at 50-60℃ during high-speed shearing and stirring to obtain a mixture; S3, adding the prescribed amounts of citric acid and concentrated fruit juice to 1L of water to obtain solution 2; S4, mixing solution 2 with the mixture, adding water to a total volume of 10L, and homogenizing to obtain the composition that promotes synergistic anti-aging of skin and bone structure.
[0029] Solution 1 is in a pre-gel state. After the addition of solid powder, the carboxyl and phenolic hydroxyl groups of hop polyphenols, chicory flavonoids, and chicory polyphenols will chelate on the surface of the milk mineral salt, while other hydrophilic functional groups will crosslink with inulin, N-acetylglucosamine and chondroitin sulfate in the aqueous solution to form a network structure. Under the action of high-speed shearing, small micelles with milk mineral salt as the core are formed with small particle size and uniform particle size distribution.
[0030] When the mixture is combined with solution 2, the phenolic hydroxyl functional groups in the hop extract and chicory extract chelate with the milk mineral salt first. Other unchelated hydrophilic functional groups, such as hydroxyl groups, cross-link with inulin, N-acetylglucosamine, and chondroitin sulfate. This blocks the covalent cross-linking between phenolic hydroxyl groups and proteins, preventing the formation of flocculent precipitates through hydrophobic binding between the benzene ring of the phenolic hydroxyl group and the protein.
[0031] The high-speed shearing and stirring speed of S2 is 13000-17000 r / min.
[0032] The homogenization conditions in S4 are a pressure of 25 MPa, a flow rate of 6 L / h, and homogenization twice.
[0033] In the preferred S4, the first homogenization conditions are a pressure of 25 MPa, a flow rate of 6 L / h, and a homogenization temperature of 60°C. The second homogenization conditions are a pressure of 25 MPa, a flow rate of 6 L / h, and a homogenization temperature of 25°C.
[0034] Using two different homogenization temperatures can further improve the dispersion of small micelles centered on emulsion mineral salts, thus improving the stability of the emulsion system. Homogenization at high temperatures intensifies intermolecular motion, allowing for thorough mixing of the components. Homogenization at room temperature results in a "egg-box" structure formed by the multi-component complex of thickeners, calcium ions, inulin, and polyphenolic compounds. This structure possesses a certain degree of elasticity and toughness, and its uniformity and stability further enhance the stability of the emulsion.
[0035] In S1, the water temperature is first raised to 80℃. Inulin and thickener are slowly added while stirring. After mixing evenly, the temperature is lowered to room temperature. Then, diluted chicory extract and diluted carbon dioxide hop extract are added and mixed evenly again to obtain solution 1.
[0036] The composition prepared by the method of this invention, which helps to synergistically combat aging of the skin and bone structure, exhibits good stability and a long shelf life. It does not separate or precipitate during long-term storage and maintains good stability even after three freeze-thaw cycles. The synergistic effect between the components can improve facial depressions and sagging, resulting in a more youthful appearance. Attached Figure Description
[0037] Figure 1 Line graph showing the centrifugal sedimentation rate during the accelerated stability experiment.
[0038] Figure 2 This is a bar chart showing the freeze-thaw precipitation rate in the freeze-thaw stability experiment.
[0039] Figure 3 A bar chart showing the content of hydroxyproline (HYP), superoxide dismutase (SOD), and malondialdehyde (MDA) in rat skin tissue.
[0040] Figure 4 This is a bar chart of bone mineral density in the rat skull.
[0041] Figure 5 The bar chart shows the serum calcium and phosphorus levels in rats.
[0042] Figure 6 A bar chart showing the levels of osteocalcin (BGP) and alkaline phosphatase (ALP) in rat serum.
[0043] Figure 7 This is a bar chart of the Comprehensive Aging Score (CAS) in Experiment Example 4. Detailed Implementation Example 1
[0044] Preparation of chicory extract: (1) Cut the washed and dried chicory fleshy root into thin slices, soak in 0.1% citric acid aqueous solution at 40℃ for 15 min, and drain the water; (2) Dry the soaked and drained chicory fleshy root in microwave until the water content is 3%-8%; (3) Crush the microwave-dried chicory fleshy root through a 20-mesh sieve, add 80% ethanol at a solid-liquid ratio of 1:12, and after stirring evenly, extract by ultrasonic extraction at 0℃ for 30 min, and filter to obtain the first filtrate and the first residue; (4) Add 25% ethanol to the first residue, adjust the pH of the added Na2CO3 solution to 8.5, heat and reflux at 75℃ for 2 h, and filter to obtain the second filtrate and the second residue; (5) Combine the two filtrates, adjust the pH to 7 with citric acid solution, stir evenly, and concentrate by rotary evaporation under reduced pressure to a specific gravity of 1.06-1.10 to obtain chicory extract.
[0045] The yield of chicory extract was 12.73%, the total flavonoid content of chicory was 32.07 mg / g, and the total polyphenol content of chicory was 9.85 mg / g.
[0046] Preparation of a composition that promotes synergistic anti-aging of skin and bone structure: S1. Add 20g of chicory extract, 30g of carbon dioxide hop extract, 40g of low-methoxyl pectin, and 1000g of inulin prepared in this example to 5L of water and stir until homogeneous to obtain solution 1; dilute the chicory extract and carbon dioxide hop extract separately, first raise the water temperature to 80℃, and slowly add 1000g of inulin and 40g of low-methoxyl pectin while stirring, mix until homogeneous, then slowly cool to room temperature and add the diluted chicory extract and diluted carbon dioxide hop extract, and mix again until homogeneous to obtain solution 1; S2. High-speed shear stirring of solution 1 at a speed of 13000r / min, and slowly add 120g of inulin to solution 1 during the high-speed shear stirring process. A solid powder composed of 0g milk mineral salt, 225g N-acetylglucosamine, 325g chondroitin sulfate sodium, and 2500g collagen was mixed and stirred at high speed while maintaining the temperature at 50℃ to obtain a mixture; S3, 300g concentrated fruit juice and 90g citric acid were added to 1L of water to obtain solution 2; S4, solution 2 was mixed with the mixture, and water was added to a total volume of 10L. The mixture was homogenized twice to obtain a composition that helps the skin and bone structure to work together to resist aging. The first homogenization conditions were a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 60℃. The temperature was then allowed to stand and decrease to 25℃ at a rate of 5℃ / 30min. The second homogenization was carried out at a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 25℃.
[0047] The composition, which helps to synergistically combat aging of the skin and bone, is degassed, sterilized, and then sealed in strips, 10mL / strip. Example 2
[0048] Preparation of chicory extract: (1) Cut the washed and dried chicory fleshy root into thin slices, soak in 0.1% citric acid aqueous solution at 60℃ for 15 min, and drain the water; (2) Dry the soaked and drained chicory fleshy root in microwave until the water content is 3%-8%; (3) Crush the microwave-dried chicory fleshy root through a 20-mesh sieve, add 80% ethanol at a solid-liquid ratio of 1:12, stir evenly, and extract by ultrasonic extraction at 5℃ for 50 min, and filter to obtain the first filtrate and the first residue; (4) Add 25% ethanol to the first residue, adjust the pH of the added Na2CO3 solution to 8.5, heat and reflux at 75℃ for 2 h, and filter to obtain the second filtrate and the second residue; (5) Combine the two filtrates, adjust the pH to 7 with citric acid solution, stir evenly, and concentrate by rotary evaporation under reduced pressure to a specific gravity of 1.06-1.10 to obtain chicory extract.
[0049] The yield of chicory extract was 12.29%, the total flavonoid content of chicory was 32.57 mg / g, and the total polyphenol content of chicory was 9.82 mg / g.
[0050] Preparation of a composition that promotes synergistic anti-aging of skin and bone structure: S1. Add 30g of chicory extract, 30g of carbon dioxide hop extract, 40g of low-methoxyl pectin, and 1000g of inulin to 5L of water and stir until homogeneous to obtain solution 1; dilute the chicory extract and carbon dioxide hop extract separately, first raise the water temperature to 80℃, and slowly add 1000g of inulin and 40g of low-methoxyl pectin while stirring, mix well, then slowly cool to room temperature, add the diluted chicory extract and diluted carbon dioxide hop extract, and mix well again to obtain solution 1; S2. High-speed shear stirring of solution 1 at 13000r / min, and slowly add 1200g of emulsion to solution 1 during high-speed shear stirring. A solid powder composed of mineral salts, 225g N-acetylglucosamine, 325g sodium chondroitin sulfate, and 2500g collagen was mixed and stirred at high speed while maintaining the temperature at 50℃ to obtain a mixture. S3: 300g concentrated fruit juice and 90g citric acid were added to 1L of water to obtain solution 2. S4: Solution 2 was mixed with the mixture, and water was added to a total volume of 10L. The mixture was homogenized twice to obtain a composition that promotes synergistic anti-aging of the skin and bone. The first homogenization conditions were: pressure 25MPa, flow rate 6L / h, homogenization temperature 60℃, followed by a settling period to lower the temperature to 25℃ at a rate of 5℃ / 30min. The second homogenization was performed at a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 25℃.
[0051] The composition, which helps to synergistically combat aging of the skin and bone, is degassed, sterilized, and then sealed in strips, 10mL / strip. Example 3
[0052] Preparation of chicory extract: (1) Cut the washed and dried chicory fleshy root into thin slices, soak in 0.1% citric acid aqueous solution at 50℃ for 15 min, and drain the water; (2) Dry the soaked and drained chicory fleshy root in microwave until the water content is 3%-8%; (3) Crush the microwave-dried chicory fleshy root through a 20-mesh sieve, add 80% ethanol at a solid-liquid ratio of 1:12, stir evenly, and extract by ultrasonic extraction at 15℃ for 60 min, and filter to obtain the first filtrate and the first residue; (4) Add 25% ethanol to the first residue, adjust the pH of the added Na2CO3 solution to 8.5, heat and reflux at 75℃ for 2 h, and filter to obtain the second filtrate and the second residue; (5) Combine the two filtrates, adjust the pH to 7 with citric acid solution, stir evenly, and concentrate by rotary evaporation under reduced pressure to a specific gravity of 1.06-1.10 to obtain chicory extract.
[0053] The yield of chicory extract was 12.57%, the total flavonoid content of chicory was 31.32 mg / g, and the total polyphenol content of chicory was 9.73 mg / g.
[0054] Preparation of a composition that promotes synergistic anti-aging of skin and bone structure: S1, 40g of carbon dioxide hop extract, 40g of chicory extract prepared in this example, 40g of low-methoxyl pectin, and 1000g of inulin are added to 5L of water and stirred until homogeneous to obtain solution 1; the chicory extract and carbon dioxide hop extract are diluted separately, the water temperature is first raised to 80℃, and 1000g of inulin and 40g of low-methoxyl pectin are slowly added while stirring, and after mixing evenly, the mixture is slowly cooled to room temperature, and then the diluted chicory extract and diluted carbon dioxide hop extract are added, and mixed evenly again to obtain solution 1; S2, solution 1 is sheared and stirred at a high speed of 13000r / min, and 120g of inulin is slowly added to solution 1 during the high-speed shearing and stirring process. A solid powder composed of 0g milk mineral salt, 225g N-acetylglucosamine, 325g chondroitin sulfate sodium, and 2500g collagen was mixed and stirred at high speed while maintaining the temperature at 50℃ to obtain a mixture; S3, 300g concentrated fruit juice and 90g citric acid were added to 1L of water to obtain solution 2; S4, solution 2 was mixed with the mixture, and water was added to a total volume of 10L. The mixture was homogenized twice to obtain a composition that helps the skin and bone structure to work together to resist aging. The first homogenization conditions were a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 60℃. The temperature was then allowed to stand and decrease to 25℃ at a rate of 5℃ / 30min. The second homogenization was carried out at a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 25℃.
[0055] The composition, which helps to synergistically combat aging of the skin and bone, is degassed, sterilized, and then sealed in strips, 10mL / strip. Comparative Example 1
[0056] Preparation of Comparative Example 1 composition: S1, 60g of carbon dioxide hop extract, 40g of low-methoxyl pectin, and 1000g of inulin were added to 5L of water and stirred until homogeneous to obtain solution 1; the carbon dioxide hop extract was diluted by first raising the water temperature to 80℃, and then slowly adding 1000g of inulin and 40g of low-methoxyl pectin while stirring. After mixing evenly, the mixture was slowly cooled to room temperature, and then the diluted carbon dioxide hop extract was added and mixed evenly again to obtain solution 1; S2, solution 1 was sheared and stirred at a high speed of 13000r / min. During the high-speed shearing and stirring process, 1200g of milk mineral salt and 225g of N-acetylglucosamine were slowly added to solution 1. A solid powder composed of sugar, 325g sodium chondroitin sulfate, and 2500g collagen was mixed and stirred at high speed while maintaining the temperature at 50℃ to obtain a mixture. S3: 300g concentrated fruit juice and 90g citric acid were added to 1L of water to obtain solution 2. S4: Solution 2 was mixed with the mixture, and water was added to a total volume of 10L. The mixture was homogenized twice to obtain a composition that helps the skin and bone structure synergistically resist aging. The first homogenization conditions were a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 60℃. The temperature was then allowed to stand and decrease to 25℃ at a rate of 5℃ / 30min. The second homogenization was performed at a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 25℃.
[0057] After degassing and sterilizing the composition of Comparative Example 1, it was sealed and packaged into strips, 10 mL / strip. Comparative Example 2
[0058] Preparation of Comparative Example 2 composition: S1, 60g of commercially available chicory extract, 40g of low-methoxyl pectin, and 1000g of inulin were added to 5L of water and stirred until homogeneous to obtain solution 1; the chicory extract was diluted by first raising the water temperature to 80℃, and then slowly adding 1000g of inulin and 40g of low-methoxyl pectin while stirring, mixing until homogeneous, and then slowly cooling to room temperature before adding the diluted chicory extract, mixing until homogeneous again to obtain solution 1; S2, solution 1 was sheared and stirred at a high speed of 13000r / min, and during the high-speed shearing and stirring process, 1200g of milk mineral salt, 225g of N-acetylglucosamine, and 325g of other ingredients were slowly added to solution 1. A solid powder composed of chondroitin sulfate sodium and 2500g of collagen protein was mixed and stirred at high speed while maintaining the temperature at 50℃ to obtain a mixture; S3, 300g of concentrated fruit juice and 90g of citric acid were added to 1L of water to obtain solution 2; S4, solution 2 was mixed with the mixture, and water was added to a total volume of 10L. The mixture was homogenized twice to obtain a composition that helps the skin and bone structure to work together to resist aging. The first homogenization conditions were a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 60℃. The temperature was then allowed to stand and decrease to 25℃ at a rate of 5℃ / 30min. The second homogenization was carried out at a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 25℃.
[0059] The commercially available chicory extract has a specific gravity of 1.10, a solid content of 25%, a total chicory flavonoid content of 11.94 mg / g, and a total chicory polyphenol content of 5.26 mg / g.
[0060] After degassing and sterilizing the composition of Comparative Example 2, it was sealed and packaged into strips, 10 mL / strip. Comparative Example 3
[0061] Preparation of Comparative Example 3 composition: S1, 30g of carbon dioxide hop extract, 30g of commercially available chicory extract, 40g of low-methoxyl pectin, and 1000g of inulin were added to 5L of water and stirred until homogeneous to obtain solution 1; the chicory extract and carbon dioxide hop extract were diluted separately, the water temperature was first raised to 80℃, and 1000g of inulin and 40g of low-methoxyl pectin were slowly added while stirring, and after mixing evenly, the mixture was slowly cooled to room temperature, and then the diluted chicory extract and diluted carbon dioxide hop extract were added, and mixed evenly again to obtain solution 1; S2, solution 1 was sheared and stirred at a high speed of 13000r / min, and 1200g of milk mineral salt was slowly added to solution 1 during the high-speed shearing and stirring process. A solid powder composed of 225g N-acetylglucosamine, 325g sodium chondroitin sulfate, and 2500g collagen was mixed and stirred at high speed while maintaining the temperature at 50℃ to obtain a mixture. S4. 300g concentrated fruit juice and 90g citric acid were added to 1L of water to obtain solution 2. S5. Solution 2 was mixed with the mixture, and water was added to a total volume of 10L. The mixture was homogenized twice to obtain a composition that helps the skin and bone structure synergistically resist aging. The first homogenization conditions were a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 60℃. The temperature was then allowed to stand and decrease to 25℃ at a rate of 5℃ / 30min. The second homogenization was performed at a pressure of 25MPa, a flow rate of 6L / h, and a homogenization temperature of 25℃.
[0062] The commercially available chicory extract has a specific gravity of 1.10, a solid content of 25%, a total chicory flavonoid content of 11.94 mg / g, and a total chicory polyphenol content of 5.26 mg / g.
[0063] After degassing and sterilizing the composition of Comparative Example 3, it was sealed and packaged into strips, 10 mL / strip. Experimental Example 1
[0064] After degassing and sterilization, the compositions of Examples 1-3 and Comparative Examples 1-3 were sealed and packaged into strip bags, 10 mL / bag. The strip bags were placed at 40°C and 75% humidity for 3 months, and samples were taken at months 0, 1, 2, and 3 to observe the emulsion properties. The compositions prepared in Examples 1-3 maintained a homogeneous emulsion in the accelerated stability test, without agglomeration, precipitation, or stratification. The compositions prepared in Comparative Examples 1 and 2 showed solid precipitation as early as month 0. 10 mL of the emulsion was placed in a centrifuge tube and centrifuged at 3000 rpm for 10 min to examine the precipitation rate. The weight of the centrifuge tube is m; the weight of the emulsion + centrifuge tube before centrifugation is m1; and the weight of the precipitate + centrifuge tube after centrifugation is m2. Sedimentation rate = (m2-m) / (m1-m)×100%. The results of centrifugal sedimentation rate are shown in Table 1.
[0065] Table 1. Sedimentation rate at different times during accelerated stability testing.
[0066] Group Sedimentation rate in month 0 Sedimentation rate in month 1 Sedimentation rate in the second month Sedimentation rate in the third month Example 1 0.23% 0.41% 0.53% 0.68% Example 2 0.28% 0.45% 0.59% 0.72% Example 3 0.26% 0.47% 0.55% 0.61% Comparative Example 1 3.49% 4.37% 6.57% 8.32% Comparative Example 2 3.37% 3.68% 5.14% 7.12% Comparative Example 3 0.84% 1.22% 1.94% 2.32% As shown in Table 1, Figure 1 As shown, in the accelerated stability test, the centrifugal precipitation rate of the compositions in Examples 1-3 was less than 1% in the first 3 months, meeting the quality standard requirements for formulated lactic acid beverages. The precipitation rate change curves of Examples 1-3 showed the same trend. Comparative Examples 1 and 2 showed precipitation in the first month, and the precipitation rate gradually increased over time. This is because, with the extension of time, not only milk mineral salts precipitate in the emulsion, but also some proteins from collagen and milk powder combine with polyphenols from hop extract to form flocculent precipitates. This indicates that chicory extract, carbon dioxide hop extract, and inulin work synergistically to improve the stability of milk mineral salts in the emulsion. Comparative Example 3 used commercially available chicory extract. The precipitation rate met the quality standard requirements for formulated lactic acid beverages in the first month, but the precipitation rate increased from the first month. This indicates that the shelf life of the skin-and-bone synergistic anti-aging composition prepared with chicory extract of this invention is longer than that of compositions prepared with commercially available chicory extract.
[0067] The compositions of Examples 1-3 and Comparative Example 1 of this invention were subjected to three freeze-thaw cycles at -20℃ / 16h → 25℃ / 8h. 10 mL of the emulsion was placed in a centrifuge tube and centrifuged at 3000 rpm for 10 min to examine the freeze-thaw precipitation rate. The results are shown in Table 2.
[0068] Table 2 Freeze-thaw precipitation rate in freeze-thaw stability test.
[0069] Group Freeze-thaw sedimentation rate Example 1 0.37% Example 2 0.42% Example 3 0.36% Comparative Example 1 11.57% Comparative Example 2 12.39% Comparative Example 3 2.38% As shown in Table 2, Figure 2As shown, the compositions of Examples 1-3 of this invention exhibit excellent freeze-thaw stability; after three repeated freeze-thaw cycles, the precipitation rate remains below 5%. Comparative Examples 1 and 2 showed significant precipitation after three repeated freeze-thaw cycles. The precipitation rate of Comparative Example 3 was greater than that of Examples 1-3, indicating that the dynamic stability of the emulsion prepared from commercially available chicory extract is slightly lower than that of the emulsion prepared from the chicory extract of this invention. Experimental Example 3: Study on the anti-aging effect of the composition of the present invention on ovariectomized rats
[0070] Materials and Grouping: SPF-grade female SD rats aged 10-12 months, weighing 500±50g, were randomly divided into 8 groups: blank control group, model group, comparative examples 1-3 groups, and example 1-3 groups, with 10 rats in each group. Experiments began after 7 days of acclimatization feeding. Animal Housing Conditions: Barrier system animal room, temperature 22±2℃, relative humidity 40-60%, controlled lighting time 12 / 12h. Five rats per cage, free access to water and food, timely bedding changes, and regular cage cleaning.
[0071] Establishment of an ovariectomy aging model: SD rats were anesthetized by intraperitoneal injection of 3% sodium pentobarbital (30 mg / kg). In the blank control group, no ovarian tissue was removed; instead, a small amount of peritoneal fat around the ovary was removed via sham surgery. All other groups underwent bilateral ovariectomy. Penicillin was administered intramuscularly for five consecutive days starting on postoperative day 2 to prevent infection. One week postoperatively, vaginal smears were examined to observe exfoliated cells and confirm surgical success. Two weeks postoperatively, oral administration of the emulsion prepared in Examples 1-3 and Comparative Examples 1-3 (2.5 mL / kg) was initiated. The blank control group and model group received an equal volume of physiological saline via oral administration. Oral administration was performed once daily for two consecutive months.
[0072] After two months of continuous drug administration, rats were euthanized by blood collection from the carotid artery. Blood, skin tissue, and skull samples were collected.
[0073] (1) Detection of HYP, SOD and MDA content in rat skin tissue: Hair was removed with 8% Na2S solution, and 2cm of skin tissue was cut from the back. 2 After defatting with ether and drying with filter paper, 0.2g of skin tissue was accurately weighed, cut into small pieces, and poured into a homogenization tube. 1.8g of pre-cooled physiological saline was added, and the mixture was homogenized into a 10% (w / w) tissue homogenate using a tissue homogenizer. Homogenization conditions were 12000 rpm for 40 seconds, with 10-second intervals, repeated 4-5 times in ice water. A small amount of tissue homogenate was smeared and observed under a microscope to assess cell disruption. If cell disruption was incomplete, the homogenization cycles were increased until all cell contents were completely free in the liquid phase. The levels of hydroxyproline (HYP), superoxide dismutase (SOD), and malondialdehyde (MDA) in the tissue homogenate were measured using a kit.
[0074] Table 3. Effects of different doses of the same oral medication on the levels of HYP, SOD, and MDA in rat skin tissue.
[0075] Group HYP (µg / mg wet weight) SOD (U / mg wet weight) MDA (nmol / mg wet weight) Example 1 4.21±0.21 3.26±0.19 1.57±0.09 Example 2 4.23±0.27 3.29±0.27 1.51±0.09 Example 3 4.33±0.24 3.33±0.26 1.51±0.10 Comparative Example 1 3.66±0.34 2.91±0.15 1.87±0.09 Comparative Example 2 3.48±0.36 2.63±0.31 2.03±0.14 Comparative Example 3 4.02±0.33 3.00±0.19 1.71±0.10 Blank control group 4.56±0.28 3.67±0.40 1.27±0.07 Model Group 3.15±0.32 2.39±0.23 2.22±0.11 HYP content represents the amount of collagen fibers in rat skin, as shown in Table 3. Figure 3 As shown, the compositions of Examples 1-3 of this invention can increase the amount of collagen fibers in rat skin tissue, thus delaying skin aging. Superoxide dismutase (SOD) is the only enzyme in the body that uses oxygen free radicals as a substrate. SOD activity indirectly reflects the ability of rat skin to scavenge free radicals, and MDA content indirectly reflects the degree of free radical attack on body cells; both can reflect the degree of aging in the body. The results showed that the model group had significantly lower SOD activity and significantly higher MDA content than the blank control group, proving that the skin aging caused by decreased estrogen levels in ovariectomized rats is manifested as a weakened ability to scavenge oxygen free radicals and an increased degree of free radical damage. In Examples 1-3 and Comparative Examples 1-3, SOD in rats could improve the ability of rats to scavenge oxygen free radicals and reduce the degree of free radical damage in rats. However, compared with other examples and comparative groups, rats in Comparative Examples 1 and 2 showed a weakened ability to remove oxygen free radicals and a greater degree of free radical damage. This indicates that the addition of chicory extract and hop extract has an important effect on the effect of the composition on skin aging. Chicory extract and hop extract have a synergistic effect on increasing the amount of collagen fibers and SOD activity in rat skin.
[0076] (2) Measurement of bone mineral density of rat skull: The bone mineral density of rat skull was measured by dual-energy X-ray absorptiometry. The results are shown in Table 4.
[0077] Table 4. Effects of different doses of drugs administered by gavage on bone mineral density in rat skulls.
[0078] Group <![CDATA[Skull bone density (g / cm 2 ).]]> Example 1 0.359±0.008 Example 2 0.367±0.012 Example 3 0.356±0.013 Comparative Example 1 0.352±0.010 Comparative Example 2 0355±0015 Comparative Example 3 0.356±0.014 Blank control group 0.386±0.008 Model Group 0.210±0.015 From Table 4, Figure 4 As can be seen, the skull bone density of the model group was significantly lower than that of the blank control group, indicating that the osteoporosis model induced by bilateral ovariectomy in rats was successfully established. The bone density of rats in Examples 1-3 and Comparative Examples 1-3 was higher than that of the model group, indicating that the composition of the present invention can promote bone formation and inhibit bone loss, and exert its effect of preventing bone aging by regulating bone metabolism balance.
[0079] (3) Determination of serum calcium, phosphorus, osteocalcin (BGP), and alkaline phosphatase (ALP) levels in rats: Blood samples were collected from each group of rats and centrifuged at 10,000 r / min for 15 min to obtain serum for the determination of rat serum biochemical indicators. A fully automated biochemical analyzer was used to determine rat serum calcium and phosphorus levels by photoelectric colorimetry, and reagent kits were used to detect the levels of osteocalcin (BGP) and alkaline phosphatase (ALP).
[0080] Table 5. Effects of different doses of the same oral medication on serum calcium, phosphorus, BGP and ALP levels in rats.
[0081] Group Serum calcium (mmol / L) Serum phosphorus (mmol / L) BGP (µg / L) ALP (U / L) Example 1 2.23±0.14 1.46±0.16 22.93±2.41 98.24±9.25 Example 2 2.23±0.14 1.39±0.14 22.65±2.56 98.05±9.42 Example 3 2.24±0.12 1.41±0.11 22.92±2.06 98.30±14.28 Comparative Example 1 2.19±0.10 1.42±0.07 22.94±1.38 97.67±9.22 Comparative Example 2 2.18±0.13 1.42±0.11 23.63±1.87 99.18±13.54 Comparative Example 3 2.17±0.10 1.45±0.12 22.90±1.14 97.18±8.75 Blank control group 2.34±0.20 1.24±0.16 20.73±1.49 96.12±9.04 Model Group 2.14±0.31 1.67±0.10 39.53±2.32 131.02±25.13 From Table 5, Figure 5 , Figure 6 As shown, the serum calcium content of rats in Examples 1-3 was close to that of the blank control group, while the serum phosphorus content, BGP, and ALP levels were lower than those in the model group. This indicates that the compositions prepared in Examples 1-3 can effectively regulate serum calcium and phosphorus levels, regulate serum bone turnover levels, reduce bone loss, promote osteoblast differentiation, reduce bone metabolism levels, accelerate bone formation, and improve calcium absorption and utilization. Experimental Example 4: Anti-aging study of the composition of the present invention on facial skin and bone structure in a population aged 55-65.
[0082] Sixty female volunteers aged 55-65 were selected and divided into six groups of 10 each (Experimental Group 1-Experimental Group 6). Perioral aging was assessed according to the comprehensive grading standards in the "Expert Consensus on the Operational Guidelines of Collagen Perioral Rejuvenation Fillers" published in the *Chinese Journal of Aesthetic and Plastic Surgery*, based on six dimensions: skin aging, perioral wrinkles, marionette lines, nasolabial folds, and jawline. Each item was scored from 0 to 4 points, and the scores of all six items were added together to obtain the Comprehensive Aging Score (CAS).
[0083] Experimental groups 1-3 took the compositions prepared in Examples 1-3 of this invention, while experimental groups 4-6 took the compositions prepared in Comparative Examples 1-3 of this invention. Each group took one packet twice daily for two consecutive months, after which the patients were again assessed. The difference in the overall aging score before and after the experiment was calculated to examine the anti-aging effects of the compositions of Examples 1-3 and Comparative Examples 1-3 on facial skin and bone structure in women aged 55-65. The results are shown in Table 6.
[0084] Table 6. Effects of the composition of the present invention on CAS in people aged 55-65 years.
[0085] Group CAS before experiment CAS after experiment Difference Experiment 1 Group 158 135 23 Experiment 2 group 152 126 26 Experimental Group 3 148 124 24 Experiment 4 group 156 141 15 Experiment 5 group 147 139 8 Experiment 6 group 149 135 14 From Table 6, Figure 7 It can be seen that the compositions prepared in Examples 1-3 of this invention have little difference in their effect on the overall aging score. The anti-aging effect of the compositions in Examples 1-3 on the skin and bone structure is better than that of the compositions prepared in Comparative Examples 1-3.
[0086] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A composition that promotes synergistic anti-aging of the skin and bone structure, characterized in that: The composition that promotes synergistic anti-aging of skin and bone structure comprises 1200g of milk mineral salts, 2500g of collagen, 325g of sodium chondroitin sulfate, 225g of N-acetylglucosamine, 20-40g of chicory extract, 20-40g of carbon dioxide hop extract, 40g of thickener, 1000g of inulin, 300g of concentrated fruit juice, 90g of citric acid, and water. The chicory extract is prepared by the following method: Cut the washed and dried chicory fleshy root into thin slices, soak in a 0.1% citric acid aqueous solution at 40-60℃ for 15 minutes, and then drain. After soaking and draining, the fleshy roots of chicory are microwave-dried until the moisture content is 3%-8%. Microwave-dried chicory fleshy roots were crushed and passed through a 20-mesh sieve. 80% ethanol was added at a solid-liquid ratio of 1:
12. After stirring evenly, the roots were ultrasonically extracted at 0-20℃ for 30-60 minutes. The first filtrate and the first residue were obtained by filtration. Add 25% ethanol to the first residue, adjust the pH of the added Na2CO3 solution to 8.5, heat and reflux at 75℃ for 2 hours, and filter to obtain the second filtrate and the second residue. (5) Combine the two filtrates, adjust the pH to 7 with citric acid solution, stir evenly, and then concentrate by rotary evaporation under reduced pressure to a specific gravity of 1.06-1.10 to obtain chicory extract.
2. The composition according to claim 1 that helps to synergistically combat aging of the skin and bone structure, characterized in that: The drying time in step (2) is 8-12 minutes.
3. The composition according to claim 2 that helps to synergistically combat aging of the skin and bone structure, characterized in that: The chicory extract contains 21.32-22.57 mg / g of total chicory flavonoids and 9.73-9.85 mg / g of total chicory polyphenols.
4. The composition according to any one of claims 1-3 that helps to synergistically combat aging of the skin and bone structure, characterized in that: The thickener is low-methoxyl pectin.
5. The composition according to claim 4 that helps to synergistically combat aging of the skin and bone structure, characterized in that: The composition that helps the skin and bone structure work together to combat aging includes 30g of chicory extract and 30g of carbon dioxide hop extract.
6. The composition according to claim 5 that helps to synergistically combat aging of the skin and bone structure, characterized in that: The concentrated fruit juice is apple concentrate.
Citation Information
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