Cosmetic jade composition additive and preparation method thereof
The cosmetic jade composition additive addresses the absorption and irritation issues of jade powder by using quinoa starch microspheres and a long-acting moisturizing composition, achieving improved skin care benefits and reduced adverse reactions.
Patent Information
- Application Number
- CN202411617677.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-13
- Publication Date
- 2024-12-20
AI Technical Summary
Jade powder is not easily absorbed by the skin, leading to limited effectiveness in beauty and skin care, and can cause discomfort such as skin redness, swelling, and sensitivity.
A cosmetic jade composition additive comprising quinoa starch microspheres loaded with inclusion complexes and a long-acting moisturizing and antibacterial composition, prepared by combining jade powder with quinoa starch, β-cyclodextrin, Artemisia argyi polysaccharide, Dendrobium polysaccharide, and hyaluronic acid, to enhance absorption and reduce skin irritation.
The additive improves the absorption and utilization of jade powder, enhancing moisturizing, oil absorption, and antibacterial properties while reducing skin irritation, resulting in better skin care effects.
Smart Images

Figure CN119157778A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetics, and specifically refers to a cosmetic jade composition additive and a preparation method thereof. Background Art
[0002] In traditional medicine, jade is believed to have health-preserving and beauty-enhancing effects. Jade rolling can calm facial nerves and make the skin as smooth as fat. Jade contains a large amount of trace elements, such as silicon, iron, calcium, magnesium, etc. These elements have a good effect on skin nutrition and moisturizing. The minerals and negative ions in jade can penetrate into the human body through the skin, playing a role in cleansing, detoxifying and regulating body balance.
[0003] Jade skin care is the process of adding processed and maintained jade into cosmetics for skin care. Jade is often added in powder form in the hope of achieving deep and efficient beauty effects. Jade skin care has been widely used in beauty SPA and other fields, and is regarded as a very high-end personal care product.
[0004] The existing technology currently has the following problems:
[0005] Jade powder is not easily absorbed by the skin, which limits its effectiveness in beauty and skin care. It can also easily cause discomfort symptoms such as skin redness, swelling, and sensitivity. Summary of the invention
[0006] In view of the above situation, in order to overcome the defects of the prior art, the present invention proposes a cosmetic jade composition additive, comprising the following components in parts by weight: 50-60 parts of quinoa starch microspheres loaded with inclusion complexes and 10-20 parts of long-lasting moisturizing and antibacterial composition.
[0007] The quinoa starch microspheres loaded with inclusion compounds include the following components in parts by weight: 5-8 parts of quinoa starch porous microsphere base, 10-20 parts of beta-cyclodextrin, and 30-40 parts of jade powder.
[0008] The long-acting moisturizing and antibacterial composition comprises the following components in parts by weight: 20-25 parts of Artemisia argyi polysaccharide, 20-25 parts of Dendrobium polysaccharide, and 5-10 parts of hyaluronic acid.
[0009] The method for preparing quinoa starch microspheres loaded with inclusion compounds specifically comprises the following steps:
[0010] (1) Grind the leftover materials of Xinjiang Hetian jade into coarse jade powder, then place it in an all-round planetary ball mill at a speed of 100-200rpm for 1-2h, then grind it manually, sieve it, and dry it. Jade powder has the function of absorbing dirt and grease, and can effectively absorb dirt and grease on the surface of the skin, deeply clean the pores, and make the skin refreshed and non-greasy. The natural minerals and trace elements in the jade powder can penetrate into the bottom layer of the skin, replenish moisture for the skin, and make the skin supple and plump. Jade powder also has a certain anti-inflammatory effect, which can relieve skin inflammation and redness, while inhibiting bacterial growth, effectively reducing the occurrence of acne and blackheads, and obtaining jade powder;
[0011] (2) Wash the red and black quinoa seeds and dry them in a 40°C oven to constant weight. Use a grinder to grind the coarse powder, pass it through an 80-100 mesh sieve, add 5.0-10.0 g of quinoa powder to 10-20 mL of petroleum ether, soak overnight, filter out the petroleum ether, and dry it in a fume hood. Add 10-20 mL of 0.3% sodium hydroxide solution to the defatted quinoa powder, stir evenly, and place it in a constant temperature shaker at a controlled temperature of 25-30°C and a shaker speed of 100-160 rpm. The extraction time is 8-12 h, and the powder is centrifuged to remove the upper The clear liquid and the precipitate are divided into three layers. The middle white layer of precipitate is taken and washed with deionized water until the pH is neutral, sieved to remove large particles of residual impurities, and the filtrate is centrifuged again to remove impurities on the top and bottom layers of the starch. The washing and centrifugation operations can be repeated until the starch is milky white and free of yellow and black impurities, and then freeze-dried and ground. The quinoa starch obtained by this process has excellent water retention and solubility, presents a polyhedral sphere, and has a uniform and narrow particle size distribution of about 1.0-3.0 μm. The particle size is significantly lower than that of other starches and is more suitable for preparing starch microspheres to obtain quinoa starch;
[0012] (3) Pour the quinoa starch described in step (1) into 2 times the amount of distilled water, mix and stir for 2-3 hours, freeze at -25°C for 5-6 hours, then ultrasonically treat at room temperature for 1-2 hours, dry and crush, then add the ultrasonically frozen-thawed quinoa starch to 3 times the amount of acetic acid buffer solution with a pH of 4.0-5.0, mix evenly, bath in a constant temperature water bath at 50-55°C for 10-15 minutes, then add 10-15% α-amylase and 5% saccharifying enzyme, bath in a constant temperature water bath at 50-55°C for 12-24 hours, add mass The pH value is adjusted to 11.0 with a 5% sodium hydroxide solution, and the hydrolysis reaction is terminated. A 2-fold amount of anhydrous ethanol is added to inactivate the enzyme, and the enzyme is repeatedly washed with anhydrous ethanol and distilled water for 3-5 times, filtered, dried, and crushed. The quinoa starch is ultrasonically pretreated before enzymolysis to increase the number and proportion of starch micropores, thereby increasing the sensitivity of starch to enzymatic hydrolysis. Therefore, the ultrasonic freeze-thaw combined with enzymolysis technology can obtain porous starch with a larger specific surface area and total pore volume, and has better swelling performance and adsorption performance, thereby obtaining quinoa porous starch;
[0013] (4) Add 2-3 times the amount of the quinoa porous starch described in step (3) to a 4% sodium hydroxide solution, mix well, and place in a constant temperature water bath at 50-60°C, stir for 20-30 minutes, cool the starch paste at room temperature and use it as the water phase, measure 50-80 mL of soybean oil in a beaker, place it in a constant temperature water bath at 50-60°C, add 0.5-1.0 g of Span 80 for emulsification, stir magnetically for 10 minutes, cool to room temperature and use it as the oil phase, add the water phase to the oil phase at a rate of 1 mL / min, stir at high speed for 30-40 minutes, and stir at a speed of 1000-2000 rpm. Add 50-60% epichlorohydrin solution by mass, stir for 20-30 minutes, stir at a speed of 600-800 rpm, after the reaction is completed, remove the upper oil phase by centrifugation, wash the precipitate with ethyl acetate, anhydrous ethanol and acetone solution for 3-5 times, vacuum dry, grind, and the prepared microspheres can absorb more active ingredients, and continuously release the active ingredients on the skin through a sustained release effect, thereby improving the absorption and utilization of the active substances and reducing the irritation to the skin. The quinoa starch microspheres can also absorb dirt and grease on the skin, keeping it fresh and non-greasy, thereby enhancing the moisturizing and grease removal effects, and obtaining a quinoa starch porous microsphere substrate;
[0014] (5) Add 1.0-2.0 g of β-cyclodextrin to 100 mL of distilled water, heat and stir at a constant temperature for 20-30 min with magnetic stirring, control the temperature at 60° C., stir at a speed of 300-400 rpm, slowly add the jade powder described in step (1), continue stirring for 2-3 h, cool to room temperature, freeze-dry, and grind. Through the inclusion action of β-cyclodextrin, the active substance in the jade powder can be encapsulated in the structure, thereby improving its solubility and stability, promoting the penetration and absorption of the active ingredients, and allergic reactions.
[0015] (6) The quinoa starch porous microsphere substrate described in step (4) and the active inclusion compound described in step (5) are added to 100-200 mL of distilled water, ultrasonicated at room temperature for 30-40 min, and then placed in a constant temperature magnetic stirrer for stirring for 1-2 h, the stirring temperature is 37° C., the stirring speed is 300-400 rpm, centrifuged, the upper liquid is removed, the precipitate is washed with deionized water 3 times, vacuum dried, and ground. The quinoa starch porous microspheres are used as the substrate, and the active inclusion compound is loaded in the pores. By slowly releasing the active compound, the active compound is prolonged. The residence time of the ingredients on the skin improves its penetration and absorption efficiency, avoids the irritation and discomfort caused by rapid and direct contact with the skin, and reduces the occurrence of adverse skin reactions. Its porous microsphere structure also further enhances the performance of moisturizing and oil absorption. After releasing the active inclusion compound, β-cyclodextrin penetrates through the skin stratum corneum, hair follicles and sweat ducts, thereby improving the absorption and utilization of jade powder in the skin, which is conducive to better exerting its oil absorption, moisturizing effect and antibacterial and anti-inflammatory effects, and obtaining quinoa starch microspheres loaded with inclusion compounds;
[0016] Preferably, in step (3), during the ultrasonic treatment, the frequency is 30-40 KHz and the power is 400-500 W, and the cavitation effect of the ultrasound is conducive to the generation of more pores inside the starch;
[0017] Preferably, in step (4), the amount of epichlorohydrin solution added is 5-10 mL, and epichlorohydrin reacts with hydroxyl groups on the surface of starch microspheres to form epoxy compounds, thereby cross-linking the starch microspheres and increasing the stability of the starch microspheres.
[0018] The present invention also provides a method for preparing a cosmetic jade composition additive, which specifically comprises the following steps:
[0019] S1, wash, dry and grind the wormwood leaf into fine powder, weigh 4.0-5.0g wormwood leaf powder and add it to 200mL water, stir evenly, add 1-2% cellulase, ultrasonically treat for 1-2h, ultrasonic temperature 40-50℃, ultrasonic frequency 30-40KHz, ultrasonic power 500-550W, centrifuge while hot, collect the filtrate, add 5-10 times the amount of anhydrous ethanol, let it stand overnight in a refrigerator, centrifuge, dry and grind the precipitate, extract the wormwood polysaccharide by this method, have good hygroscopicity, moisture retention and antibacterial and anti-inflammatory properties, reduce the infection and inflammation caused by bacterial growth, help keep the skin fresh and healthy, and also have the effect of whitening and increasing skin elasticity, to obtain wormwood polysaccharide;
[0020] S2, dissolving dendrobium polysaccharide, hyaluronic acid and wormwood polysaccharide described in step S1 in 100 mL of water to prepare a polysaccharide composite solution, magnetically stirring at room temperature for 1-2 hours, and then bathing in water at 70-80°C for 1-2 hours to obtain a long-acting moisturizing and antibacterial composition, and then adding quinoa starch microspheres loaded with inclusion complex, high pressure homogenization, homogenization pressure 600-800 bar, homogenization time 2-3 minutes, freeze drying, and crushing, cross-linking and compounding of traditional Chinese medicine plant polysaccharides and hyaluronic acid to form a larger and uniform three-dimensional network structure, with good safety, film-forming and moisturizing properties, quinoa starch microspheres loaded with inclusion complex, forming a gel by capturing water, thereby effectively adhering to the skin, increasing the effective contact between the quinoa starch microspheres loaded with inclusion complex and the skin, which is beneficial to enhancing transdermal absorption and better exerting skin care effects, and obtaining a cosmetic jade composition additive;
[0021] Preferably, in step S2, in the polysaccharide composite solution, the mass fraction of dendrobium polysaccharide is 4-5%, the mass fraction of hyaluronic acid is 1-2%, and the mass fraction of wormwood polysaccharide is 4-5%. The composite use of the three polysaccharides has good long-lasting moisturizing properties.
[0022] The beneficial effects achieved by the present invention are as follows:
[0023] The present invention increases the contact between the quinoa starch microspheres loaded with the inclusion compound and the skin through the composite synergistic effect of the quinoa starch microspheres loaded with the inclusion compound and the long-acting moisturizing and antibacterial composition, so that the active substance jade powder is continuously released on the skin, and the absorption and utilization are improved, thereby increasing the adsorption, moisturizing and antibacterial and anti-inflammatory properties of oil and fat, and reducing the stimulation of the jade powder to the skin, thereby achieving a better use effect; in the quinoa starch microspheres loaded with the inclusion compound, β-cyclodextrin is coated with the jade powder, and then attached to the pores of the quinoa starch porous microsphere substrate, thereby increasing the solubility and stability of the jade powder, and through the microspheres and the inclusion compound, the slow release of the jade powder is achieved, which not only increases the contact time with the skin, but also is conducive to promoting the penetration and absorption of the active ingredients, thereby improving the moisturizing, oil absorption and antibacterial effects of the jade powder, and effectively reducing its unpleasant effects on the skin. The invention discloses a kind of cosmetic jade composition additive, which is a kind of good stimulation, wherein the porous quinoa starch microsphere substrate further enhances the ability of moisturizing and absorbing oil; in the long-acting moisturizing and antibacterial composition, the Chinese medicinal plant polysaccharide and the natural polysaccharide are cross-linked to form a large and uniform three-dimensional network structure, which can carry the quinoa starch microspheres loaded with the inclusion compound, and form a gel film on the skin surface, which has long-lasting moisturizing and antibacterial and anti-inflammatory properties, and also prolongs the effective contact between the quinoa starch microspheres loaded with the inclusion compound and the skin, which is beneficial to enhance its transdermal absorption and better exert the cosmetic effects of moisturizing, oil absorption and antibacterial and anti-inflammatory properties; the invention uses the quinoa starch microspheres loaded with the inclusion compound and the long-acting moisturizing and antibacterial composition to prepare a cosmetic jade composition additive, which improves the penetration utilization of jade powder, enhances the moisturizing, oil absorption and antibacterial properties, and reduces the occurrence of adverse reactions such as skin allergies, and has excellent cosmetic skin care use effects. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] Figure 1 This is a scanning electron microscope image of quinoa starch microspheres loaded with inclusion complex prepared in Example 1 of the present invention;
[0025] Figure 2 This is a scanning electron microscope image of the long-acting moisturizing and antibacterial composition prepared in Example 1 of the present invention;
[0026] Figure 3 The moisturizing oil absorption result diagram of Examples 1-4 and Comparative Examples 1-3 of the present invention;
[0027] Figure 4 The diagram is a result diagram of the diameter of the inhibition zone of Examples 1-4 and Comparative Examples 1-3 of the present invention;
[0028] Figure 5 This is a graph showing the frequency of adverse skin reactions in Examples 1-4 of the present invention and Comparative Examples 1-3. DETAILED DESCRIPTION
[0029] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
[0030] Unless otherwise defined, all professional and scientific terms used herein have the same meanings as those familiar to those skilled in the art. In addition, any methods and materials similar or equivalent to those described herein may be applied to the present invention. The preferred implementation methods and materials described herein are for demonstration purposes only and are not intended to limit the content of this application.
[0031] The experimental methods in the following examples are conventional methods unless otherwise specified; the experimental materials used in the following examples are purchased from commercial channels unless otherwise specified.
[0032] The sources of the reagents used in the examples are as follows:
[0033] Dendrobium polysaccharide brand source leaf, item number S27808-1g;
[0034] Hyaluronic acid CAS No: 9004-61-9, brand Apinno, item number GC36971;
[0035] β-cyclodextrin CAS No: 7585-39-9, brand Innochem, product number A02847;
[0036] Petroleum ether CAS No: 8032-32-4, brand Innochem, product number G10002;
[0037] Acetic acid buffer solution brand: Zunlijia, product number: 31085753;
[0038] Soybean oil CAS No: 8001-22-7, brand Yuanye, item number S24362-250ml;
[0039] Siban 80 CAS No: 1338-43-8, brand Innochem, product number A04343;
[0040] Epichlorohydrin CAS No: 106-89-8, brand Innochem, product number A18396;
[0041] Ethyl acetate CAS No: 141-78-6, brand Innochem, product number G00003;
[0042] Acetone CAS No: 67-64-1, brand Acros, product number 326801000;
[0043] Glucoamylase CAS No: 9032-08-0, brand Mreda, product number M047343-250g, specification 100u / mg;
[0044] α-Amylase CAS No: 9000-90-2, brand Macklin, product number A769410-5g, specification 50u / mg;
[0045] Cellulase CAS No: 9012-54-8, brand source leaf, product number S10041-5g, specification 50u / mg;
[0046] Sodium hydroxide CAS No: 1310-73-2, brand Innochem, product number A36865;
[0047] Anhydrous ethanol CAS No: 64-17-5, brand Innochem, product number G00004.
[0048] Example 1
[0049] This embodiment proposes a cosmetic jade composition additive, comprising the following components in parts by weight: 60 parts of quinoa starch microspheres loaded with inclusion complexes and 20 parts of a long-lasting moisturizing and antibacterial composition.
[0050] The quinoa starch microspheres loaded with inclusion compound comprise the following components in parts by weight: 8 parts of quinoa starch porous microsphere base, 20 parts of beta-cyclodextrin and 40 parts of jade powder.
[0051] The long-acting moisturizing and antibacterial composition comprises the following components in parts by weight: 25 parts of Artemisia argyi polysaccharide, 25 parts of Dendrobium polysaccharide and 10 parts of hyaluronic acid.
[0052] The preparation method of quinoa starch microspheres loaded with inclusion compound specifically comprises the following steps:
[0053] (1) Grind the leftover materials of Xinjiang Hetian jade into coarse jade powder, then place it in an all-round planetary ball mill at a speed of 200rpm for 2h, and then grind it manually, sieve it, and dry it. Jade powder has the function of absorbing dirt and grease, and can effectively absorb dirt and grease on the surface of the skin, deeply clean the pores, and make the skin refreshed and non-greasy. The natural minerals and trace elements in the jade powder can penetrate into the bottom layer of the skin, replenish moisture for the skin, and make the skin supple and plump. Jade powder also has a certain anti-inflammatory effect, which can relieve skin inflammation and redness, while inhibiting bacterial growth, effectively reducing the occurrence of acne and blackheads, and obtaining jade powder;
[0054] (2) Wash the red and black quinoa seeds and dry them in a 40°C oven to constant weight. Use a grinder to grind them, and pass the coarse powder through a 100-mesh sieve. Add 10.0 g of quinoa powder to 20 mL of petroleum ether and soak overnight. Filter to remove the petroleum ether and dry in a fume hood. Add 20 mL of 0.3% sodium hydroxide solution to the defatted quinoa powder, stir evenly, and place in a constant temperature shaker at 30°C and a shaker speed of 160 rpm. The extraction time is 12 h. Centrifuge and remove the supernatant. The precipitate is divided into three layers and taken. The middle white layer of precipitate is washed with deionized water until the pH is neutral, sieved to remove large particles of residual impurities, and the filtrate is centrifuged again to remove impurities on the top and bottom layers of the starch. The washing and centrifugation operations can be repeated until the starch is milky white and free of yellow and black impurities, and then freeze-dried and ground. The quinoa starch obtained by this process has excellent water retention and solubility, presents a polyhedral sphere, and has a uniform particle size distribution and a narrow range of about 1.0-3.0 μm. The particle size is significantly lower than that of other starches and is more suitable for preparing starch microspheres to obtain quinoa starch;
[0055] (3) Pour the quinoa starch described in step (1) into 2 times the amount of distilled water, mix and stir for 3 hours, freeze at -25°C for 6 hours, and then ultrasonically treat at room temperature for 2 hours. During the ultrasonic treatment, the frequency is 40KHz and the power is 500W. The cavitation effect of ultrasound is conducive to the generation of more pores inside the starch. Dry and crush, then add 3 times the amount of acetic acid buffer solution with a pH of 5.0 to the ultrasonically frozen-thawed quinoa starch, mix evenly, and place in a constant temperature water bath at 55°C for 15 minutes, then add 15% α-amylase and 5% saccharifying enzyme, and keep constant temperature at 55°C. Warm water bath for 24 hours, add 5% sodium hydroxide solution by mass to adjust the pH to 11.0, the hydrolysis reaction is completed, add 2 times the amount of anhydrous ethanol to inactivate the enzyme, wash repeatedly with anhydrous ethanol and distilled water for 5 times, filter, dry, crush, and ultrasonic pretreatment of quinoa starch before enzymolysis increases the number and proportion of starch micropores, thereby increasing the sensitivity of starch to enzymatic hydrolysis. Therefore, the ultrasonic freeze-thaw combined with enzymolysis technology can obtain porous starch with larger specific surface area and total pore volume, better swelling performance and adsorption performance, and obtain quinoa porous starch;
[0056] (4) Add 3 times the amount of 4% sodium hydroxide solution in the porous quinoa starch of step (3), mix well, and then place in a constant temperature water bath at 60°C and stir for 30 minutes. Cool the starch paste at room temperature and use it as the water phase. Measure 80 mL of soybean oil in a beaker, place it in a constant temperature water bath at 60°C, add 1.0 g of Span 80 for emulsification, stir magnetically for 10 minutes, cool to room temperature and use it as the oil phase. Add the water phase to the oil phase at a rate of 1 mL / min, stir at high speed for 40 minutes at a stirring speed of 2000 rpm, add a 60% epichlorohydrin solution, stir for 30 minutes at a stirring speed of 800 rpm, and stir until the mixture is dry. The amount of epichlorohydrin solution added is 10 mL, and epichlorohydrin reacts with hydroxyl groups on the surface of starch microspheres to form epoxy compounds, thereby cross-linking the starch microspheres and increasing the stability of the starch microspheres. After the reaction is completed, the upper oil phase is removed by centrifugation, and the precipitate is washed 5 times with ethyl acetate, anhydrous ethanol and acetone solution respectively, vacuum dried, and ground. The prepared microspheres can absorb more active ingredients and continuously release the active ingredients on the skin through a sustained release effect, thereby improving the absorption and utilization of active substances and reducing their irritation to the skin. The quinoa starch microspheres can also absorb dirt and grease on the skin, keeping it fresh and non-greasy, thereby enhancing the moisturizing and grease removal effects, and obtaining a quinoa starch porous microsphere substrate;
[0057] (5) Add 2.0 g of β-cyclodextrin to 100 mL of distilled water, heat and stir at a constant temperature for 30 min with magnetic stirring, control the temperature at 60° C., stir at 400 rpm, slowly add the jade powder described in step (1), continue stirring for 3 h, cool to room temperature, freeze-dry, and grind. Through the inclusion action of β-cyclodextrin, the active substance in the jade powder can be encapsulated in the structure, thereby improving its solubility and stability, promoting the penetration and absorption of the active ingredients, and allergic reactions.
[0058] (6) The quinoa starch porous microsphere substrate described in step (4) and the active inclusion compound described in step (5) are added to 200 mL of distilled water, ultrasonicated at room temperature for 40 minutes, and then placed in a constant temperature magnetic stirrer for stirring for 2 hours at a stirring temperature of 37° C. and a stirring speed of 400 rpm. The mixture is centrifuged to remove the upper liquid, and the precipitate is washed with deionized water for 3 times, vacuum dried, and ground. The quinoa starch porous microspheres are used as the substrate, and the active inclusion compound is loaded in the pores. By slowly releasing the quinoa starch porous microspheres, the residence time of the active ingredient on the skin is prolonged, the penetration and absorption efficiency is improved, and the irritation and discomfort caused by rapid and direct contact with the skin are avoided, and the occurrence of adverse skin reactions is reduced. The porous microsphere structure also further enhances the moisturizing and oil absorption properties. After releasing the active inclusion compound, β-cyclodextrin penetrates through the skin stratum corneum, hair follicles, sweat ducts, etc., thereby improving the absorption and utilization of jade powder in the skin, which is conducive to better exerting its oil adsorption, moisturizing effect, and antibacterial and anti-inflammatory effects, thereby obtaining quinoa starch microspheres loaded with inclusion compounds.
[0059] This embodiment provides a method for preparing a cosmetic jade composition additive, which specifically comprises the following steps:
[0060] S1. Wash, dry and grind the wormwood leaf into fine powder, weigh 5.0g of wormwood leaf powder and add it to 200mL of water, stir evenly, add 2% of cellulase, and ultrasonically treat for 2h, the ultrasonic temperature is 50°C, the ultrasonic frequency is 40KHz, and the ultrasonic power is 550W. Centrifuge while hot, collect the filtrate, add 10 times the amount of anhydrous ethanol, let it stand overnight in a refrigerator, centrifuge, dry and grind the precipitate, and extract the wormwood polysaccharide by this method. It has good hygroscopicity, moisture retention, antibacterial and anti-inflammatory properties, reduces the infection and inflammation caused by bacterial growth, is conducive to keeping the skin fresh and healthy, and also has the effects of whitening and increasing skin elasticity, and obtains wormwood polysaccharide;
[0061] S2. Dissolve dendrobium polysaccharide, hyaluronic acid and wormwood polysaccharide described in step S1 in 100 mL of water to prepare a polysaccharide composite solution. In the polysaccharide composite solution, the mass fraction of dendrobium polysaccharide is 5%, hyaluronic acid is 2%, and the mass fraction of wormwood polysaccharide is 5%. The composite use of the three polysaccharides has good long-lasting moisturizing properties. Magnetic stirring is carried out at room temperature for 2 hours, and then the mixture is in a water bath at 80°C for 2 hours to obtain a long-lasting moisturizing and antibacterial composition. Then, quinoa starch microspheres loaded with inclusion complex are added, high-pressure homogenized, the homogenization pressure is 800 bar, the homogenization time is 3 minutes, freeze-dried and crushed, and a large and uniform three-dimensional network structure is formed by cross-linking and compounding traditional Chinese medicine plant polysaccharides with hyaluronic acid, which has good safety, film-forming properties and moisturizing properties. The quinoa starch microspheres loaded with inclusion complex form gels by capturing water, thereby effectively adhering to the skin, increasing the effective contact between the quinoa starch microspheres loaded with inclusion complex and the skin, which is beneficial to enhancing transdermal absorption and better exerting skin care effects, thereby obtaining a cosmetic jade composition additive.
[0062] In this example, the prepared quinoa starch microspheres loaded with inclusion complex and the long-acting moisturizing and antibacterial composition were subjected to scanning electron microscopy to observe their microscopic morphology. Figure 1 This is a 5000-fold magnified SEM image of the quinoa starch microspheres loaded with inclusion complex prepared in Example 1. Figure 2 This is a 40-fold magnified SEM image of the long-lasting moisturizing and antibacterial composition prepared in Example 1. Figure 1 The quinoa starch microspheres loaded with inclusion compounds prepared in this embodiment present a porous spherical structure, such as Figure 2 The long-lasting moisturizing and antibacterial composition prepared in this embodiment has a sheet-like network structure.
[0063] Example 2
[0064] This embodiment proposes a cosmetic jade composition additive, comprising the following components in parts by weight: 50 parts of quinoa starch microspheres loaded with inclusion complexes and 10 parts of a long-lasting moisturizing and antibacterial composition.
[0065] The quinoa starch microspheres loaded with inclusion compound comprise the following components in parts by weight: 5 parts of quinoa starch porous microsphere base, 10 parts of beta-cyclodextrin and 30 parts of jade powder.
[0066] The long-acting moisturizing and antibacterial composition comprises the following components in parts by weight: 20 parts of Artemisia argyi polysaccharide, 20 parts of Dendrobium polysaccharide and 5 parts of hyaluronic acid.
[0067] The preparation method of quinoa starch microspheres loaded with inclusion compound specifically comprises the following steps:
[0068] (1) Grind the leftover materials of Xinjiang Hetian jade into coarse jade powder, then place it in an all-round planetary ball mill at a speed of 100rpm for 1h, and then grind it manually, sieve it, and dry it. Jade powder has the function of absorbing dirt and grease, and can effectively absorb dirt and grease on the surface of the skin, deeply clean the pores, and make the skin refreshed and non-greasy. The natural minerals and trace elements in the jade powder can penetrate into the bottom layer of the skin, replenish moisture for the skin, and make the skin supple and plump. Jade powder also has a certain anti-inflammatory effect, which can relieve skin inflammation and redness, while inhibiting bacterial growth, effectively reducing the occurrence of acne and blackheads, and obtaining jade powder;
[0069] (2) Wash the red and black quinoa seeds and dry them in a 40°C oven to constant weight. Use a grinder to grind the seeds. Pass the coarse powder through an 80-mesh sieve. Add 5.0 g of quinoa powder to 10 mL of petroleum ether and soak overnight. Filter to remove the petroleum ether and dry in a fume hood. Add 10 mL of 0.3% sodium hydroxide solution to the defatted quinoa powder. Stir evenly and place in a constant temperature shaker. Control the temperature at 25°C and the shaker speed at 100 rpm. Extract for 8 h. Centrifuge and remove the supernatant. The precipitate is divided into three layers. Take the middle layer. The white layer of precipitate is washed with deionized water until the pH is neutral, sieved to remove large particles of residual impurities, and the filtrate is centrifuged again to remove impurities on the top and bottom layers of the starch. The washing and centrifugation operations can be repeated until the starch is milky white and free of yellow and black impurities, and then freeze-dried and ground. The quinoa starch obtained by this process has excellent water retention and solubility, presents a polyhedral sphere, and has a uniform particle size distribution and a narrow range of about 1.0-3.0 μm. The particle size is significantly lower than that of other starches and is more suitable for preparing starch microspheres to obtain quinoa starch;
[0070] (3) Pour the quinoa starch described in step (1) into 2 times the amount of distilled water, mix and stir for 2 hours, freeze at -25°C for 5 hours, and then ultrasonically treat at room temperature for 1 hour. During the ultrasonic treatment, the frequency is 30KHz and the power is 400W. The cavitation effect of ultrasound is conducive to the formation of more pores inside the starch. Dry and crush, then add 3 times the amount of acetic acid buffer solution with a pH of 4.0 after ultrasonic freeze-thaw, mix evenly, and place in a constant temperature water bath at 50°C for 10 minutes, then add 10% α-amylase and 5% saccharifying enzyme, and keep constant temperature at 50°C. Warm water bath for 12 hours, add 5% sodium hydroxide solution by mass to adjust the pH to 11.0, the hydrolysis reaction is completed, add 2 times the amount of anhydrous ethanol to inactivate the enzyme, wash repeatedly with anhydrous ethanol and distilled water for 3 times, filter, dry, crush, and ultrasonic pretreatment of quinoa starch before enzymolysis increases the number and proportion of starch micropores, thereby increasing the sensitivity of starch to enzymatic hydrolysis. Therefore, the ultrasonic freeze-thaw combined with enzymolysis technology can obtain porous starch with larger specific surface area and total pore volume, better swelling performance and adsorption performance, and obtain quinoa porous starch;
[0071] (4) Add 2 times the amount of 4% sodium hydroxide solution in the porous quinoa starch of step (3), mix well, and then place in a constant temperature water bath at 50°C and stir for 20 minutes. Cool the starch paste at room temperature and use it as the water phase. Measure 50 mL of soybean oil in a beaker, place it in a constant temperature water bath at 50°C, add 0.5 g of Span 80 for emulsification, stir magnetically for 10 minutes, cool to room temperature and use it as the oil phase. Add the water phase to the oil phase at a rate of 1 mL / min, stir at high speed for 30 minutes at a stirring speed of 1000 rpm, add 50% epichlorohydrin solution, stir for 20 minutes at a stirring speed of 600 rpm, and stir until the mixture is dry. The amount of epichlorohydrin solution added is 5 mL, and epichlorohydrin reacts with hydroxyl groups on the surface of starch microspheres to form epoxy compounds, thereby cross-linking the starch microspheres and increasing the stability of the starch microspheres. After the reaction is completed, the upper oil phase is removed by centrifugation, and the precipitate is washed 3 times with ethyl acetate, anhydrous ethanol and acetone solution respectively, vacuum dried, and ground. The prepared microspheres can absorb more active ingredients and continuously release the active ingredients on the skin through a sustained release effect, thereby improving the absorption and utilization of active substances and reducing their irritation to the skin. The quinoa starch microspheres can also absorb dirt and grease on the skin, keeping it fresh and non-greasy, thereby enhancing the moisturizing and grease removal effects, and obtaining a quinoa starch porous microsphere substrate;
[0072] (5) Add 1.0 g of β-cyclodextrin to 100 mL of distilled water, heat and stir at a constant temperature for 20 min with magnetic stirring, control the temperature at 60° C., stir at 300 rpm, slowly add the jade powder described in step (1), continue stirring for 2 h, cool to room temperature, freeze-dry, and grind. Through the inclusion action of β-cyclodextrin, the active substance in the jade powder can be encapsulated in the structure, thereby improving its solubility and stability, promoting the penetration and absorption of the active ingredients, and allergic reactions.
[0073] (6) The quinoa starch porous microsphere substrate described in step (4) and the active inclusion compound described in step (5) are added to 100 mL of distilled water, ultrasonicated at room temperature for 30 minutes, and then placed in a constant temperature magnetic stirrer for stirring for 1 hour at a stirring temperature of 37° C. and a stirring speed of 300 rpm. The mixture is centrifuged to remove the upper liquid, and the precipitate is washed with deionized water for 3 times, vacuum dried, and ground. The quinoa starch porous microspheres are used as the substrate, and the active inclusion compound is loaded in the pores. By slowly releasing the quinoa starch porous microspheres, the residence time of the active ingredient on the skin is prolonged, the penetration and absorption efficiency is improved, and the irritation and discomfort caused by rapid and direct contact with the skin are avoided, and the occurrence of adverse skin reactions is reduced. The porous microsphere structure also further enhances the moisturizing and oil absorption properties. After releasing the active inclusion compound, β-cyclodextrin penetrates through the skin stratum corneum, hair follicles, sweat ducts, etc., thereby improving the absorption and utilization of jade powder in the skin, which is conducive to better exerting its oil adsorption, moisturizing effect, and antibacterial and anti-inflammatory effects, thereby obtaining quinoa starch microspheres loaded with inclusion compounds.
[0074] This embodiment provides a method for preparing a cosmetic jade composition additive, which specifically comprises the following steps:
[0075] S1. Wash, dry and grind the wormwood leaf into fine powder, weigh 4.0g of wormwood leaf powder and add it to 200mL of water, stir evenly, add 1% of cellulase, and ultrasonically treat for 1h, the ultrasonic temperature is 40°C, the ultrasonic frequency is 30KHz, and the ultrasonic power is 500W. Centrifuge while hot, collect the filtrate, add 5 times the amount of anhydrous ethanol, let it stand overnight in a refrigerator, centrifuge, dry and grind the precipitate, and extract the wormwood polysaccharide by this method. It has good hygroscopicity, moisture retention, antibacterial and anti-inflammatory properties, reduces the infection and inflammation caused by bacterial growth, is conducive to keeping the skin fresh and healthy, and also has the effects of whitening and increasing skin elasticity, and obtains wormwood polysaccharide;
[0076] S2. Dissolve dendrobium polysaccharide, hyaluronic acid and wormwood polysaccharide described in step S1 in 100 mL of water to prepare a polysaccharide composite solution. In the polysaccharide composite solution, the mass fraction of dendrobium polysaccharide is 4%, hyaluronic acid is 1%, and the mass fraction of wormwood polysaccharide is 4%. The composite use of the three polysaccharides has good long-lasting moisturizing properties. Magnetic stirring is carried out at room temperature for 1-2 hours, and then the mixture is in a water bath at 70-80°C for 1 hour to obtain a long-lasting moisturizing and antibacterial composition. Then, quinoa starch microspheres loaded with inclusion complex are added, high pressure homogenized, the homogenization pressure is 600 bar, the homogenization time is 2 min, freeze-dried and crushed, and a large and uniform three-dimensional network structure is formed by cross-linking and compounding traditional Chinese medicine plant polysaccharides with hyaluronic acid, which has good safety, film-forming properties and moisturizing properties. The quinoa starch microspheres loaded with inclusion complex form gels by capturing water, thereby effectively adhering to the skin, increasing the effective contact between the quinoa starch microspheres loaded with inclusion complex and the skin, which is beneficial to enhancing transdermal absorption and better exerting skin care effects, thereby obtaining a cosmetic jade composition additive.
[0077] Example 3
[0078] This embodiment proposes a cosmetic jade composition additive, comprising the following components in parts by weight: 55 parts of quinoa starch microspheres loaded with inclusion complexes and 15 parts of a long-lasting moisturizing and antibacterial composition.
[0079] The quinoa starch microspheres loaded with inclusion compound include the following components in parts by weight: 6.5 parts of quinoa starch porous microsphere base, 15 parts of beta-cyclodextrin, and 35 parts of jade powder.
[0080] The long-acting moisturizing and antibacterial composition comprises the following components in parts by weight: 22.5 parts of Artemisia argyi polysaccharide, 22.5 parts of Dendrobium officinale polysaccharide, and 7.5 parts of hyaluronic acid.
[0081] The preparation method of quinoa starch microspheres loaded with inclusion compound specifically comprises the following steps:
[0082] (1) Grind the leftover materials of Xinjiang Hetian jade into coarse jade powder, then place it in an all-round planetary ball mill at a speed of 150rpm for 1.5 hours, and then grind it manually, sieve it, and dry it. Jade powder has the function of absorbing dirt and grease, and can effectively absorb dirt and grease on the surface of the skin, deeply clean the pores, and make the skin refreshed and non-greasy. The natural minerals and trace elements in the jade powder can penetrate into the bottom layer of the skin, replenish moisture for the skin, and make the skin supple and plump. Jade powder also has a certain anti-inflammatory effect, which can relieve skin inflammation and redness, while inhibiting bacterial growth, effectively reducing the occurrence of acne and blackheads, and obtaining jade powder;
[0083] (2) Wash the red and black quinoa seeds and dry them in a 40°C oven to constant weight. Use a grinder to grind the seeds. Pass the coarse powder through a 90-mesh sieve. Add 7.5 g of quinoa powder to 15 mL of petroleum ether and soak overnight. Filter to remove the petroleum ether and dry in a fume hood. Add 15 mL of 0.3% sodium hydroxide solution to the defatted quinoa powder. Stir evenly and place in a constant temperature shaker at 27.5°C and 130 rpm. Extract for 10 h. Centrifuge and remove the supernatant. The precipitate is divided into three layers and the extract is taken. The middle white layer of precipitate is washed with deionized water until the pH is neutral, sieved to remove large particles of residual impurities, and the filtrate is centrifuged again to remove impurities on the top and bottom layers of the starch. The washing and centrifugation operations can be repeated until the starch is milky white and free of yellow and black impurities, and then freeze-dried and ground. The quinoa starch obtained by this process has excellent water retention and solubility, presents a polyhedral sphere, and has a uniform particle size distribution and a narrow range of about 1.0-3.0 μm. The particle size is significantly lower than that of other starches and is more suitable for preparing starch microspheres to obtain quinoa starch;
[0084] (3) Pour the quinoa starch described in step (1) into 2 times the amount of distilled water, mix and stir for 2.5 hours, freeze at -25°C for 5.5 hours, and then ultrasonically treat at room temperature for 1.5 hours. During the ultrasonic treatment, the frequency is 35KHz and the power is 450W. The cavitation effect of ultrasound is conducive to the formation of more pores inside the starch. Dry and crush, then add the ultrasonically frozen-thawed quinoa starch to 3 times the amount of acetic acid buffer solution with a pH of 4.5, mix evenly, keep in a constant temperature water bath at 52.5°C for 12.5 minutes, and then add 12.5% α-amylase and 5% saccharifying enzyme , 52.5℃ constant temperature water bath for 18h, adding 5% sodium hydroxide solution by mass to adjust the pH to 11.0, the hydrolysis reaction is completed, adding 2 times the amount of anhydrous ethanol to inactivate the enzyme, washing with anhydrous ethanol and distilled water for 4 times, filtering, drying, crushing, ultrasonic pretreatment of quinoa starch before enzymolysis increases the number and proportion of starch micropores, thereby increasing the sensitivity of starch to enzymatic hydrolysis. Therefore, the ultrasonic freeze-thaw combined with enzymolysis technology can obtain porous starch with larger specific surface area and total pore volume, better swelling performance and adsorption performance, and obtain quinoa porous starch;
[0085] (4) Add 2.5 times the amount of 4% sodium hydroxide solution to the porous quinoa starch described in step (3), mix well, and then place in a constant temperature water bath at 55°C and stir for 25 minutes. Cool the starch paste at room temperature and use it as the water phase. Measure 65 mL of soybean oil in a beaker, place it in a constant temperature water bath at 55°C, add 0.75 g of Span 80 for emulsification, stir magnetically for 10 minutes, cool to room temperature and use it as the oil phase. Add the water phase to the oil phase at a rate of 1 mL / min, stir at high speed for 35 minutes at a stirring speed of 1500 rpm, add 55% epichlorohydrin solution, stir for 25 minutes at a stirring speed of 700 rpm, The amount of epichlorohydrin solution added is 7.5 mL. Epichlorohydrin reacts with hydroxyl groups on the surface of starch microspheres to form epoxy compounds, thereby cross-linking the starch microspheres and increasing the stability of the starch microspheres. After the reaction is completed, the upper oil phase is removed by centrifugation, and the precipitate is washed 4 times with ethyl acetate, anhydrous ethanol and acetone solution respectively, vacuum dried and ground. The prepared microspheres can absorb more active ingredients and continuously release the active ingredients on the skin through a sustained release effect, thereby improving the absorption and utilization of active substances and reducing their irritation to the skin. The quinoa starch microspheres can also absorb dirt and grease on the skin, keeping it fresh and non-greasy, thereby enhancing the moisturizing and grease removal effects, and obtaining a quinoa starch porous microsphere substrate;
[0086] (5) Add 1.5 g of β-cyclodextrin to 100 mL of distilled water, heat at a constant temperature and stir with a magnetic stirrer for 25 min, control the temperature at 60° C., stir at 350 rpm, slowly add the jade powder described in step (1), continue stirring for 2.5 h, cool to room temperature, freeze-dry, and grind. Through the inclusion action of β-cyclodextrin, the active substance in the jade powder can be encapsulated in the structure, thereby improving its solubility and stability, promoting the penetration and absorption of the active ingredients, and allergic reactions.
[0087] (6) The quinoa starch porous microsphere substrate described in step (4) and the active inclusion compound described in step (5) are added to 150 mL of distilled water, ultrasonicated at room temperature for 35 minutes, and then placed in a constant temperature magnetic stirrer for stirring for 1.5 hours, with a stirring temperature of 37° C. and a stirring speed of 350 rpm. The mixture is centrifuged, the upper layer of liquid is removed, and the precipitate is washed with deionized water for 3 times, vacuum dried, and ground. The quinoa starch porous microspheres are used as the substrate, and the active inclusion compound is loaded in the pores. By slowly releasing the quinoa starch porous microspheres, the residence time of the active ingredient on the skin is prolonged, the penetration and absorption efficiency is improved, and the irritation and discomfort caused by rapid and direct contact with the skin are avoided, and the occurrence of adverse skin reactions is reduced. The porous microsphere structure also further enhances the moisturizing and oil absorption properties. After releasing the active inclusion compound, β-cyclodextrin penetrates through the skin stratum corneum, hair follicles, sweat ducts, etc., thereby improving the absorption and utilization of jade powder in the skin, which is conducive to better exerting its oil adsorption, moisturizing effect, and antibacterial and anti-inflammatory effects, thereby obtaining quinoa starch microspheres loaded with inclusion compounds.
[0088] This embodiment provides a method for preparing a cosmetic jade composition additive, which specifically comprises the following steps:
[0089] S1, wash, dry and grind the wormwood leaf into fine powder, weigh 4.5g of wormwood leaf powder and add it to 200mL of water, stir evenly, add 1.5% of cellulase, ultrasonically treat for 1.5h, ultrasonic temperature 45°C, ultrasonic frequency 35KHz, ultrasonic power 525W, centrifuge while hot, collect the filtrate, add 7.5 times the amount of anhydrous ethanol, let it stand overnight in a refrigerator, centrifuge, dry and grind the precipitate, and extract the wormwood polysaccharide by this method, which has good hygroscopicity, moisture retention and antibacterial and anti-inflammatory properties, reduces the infection and inflammation caused by bacterial growth, is conducive to keeping the skin fresh and healthy, and also has the effect of whitening and increasing skin elasticity, to obtain wormwood polysaccharide;
[0090] S2, dendrobium polysaccharide, hyaluronic acid and wormwood polysaccharide described in step S1 are dissolved in 100mL water to prepare a polysaccharide composite solution, in which the mass fraction of dendrobium polysaccharide is 4.5%, hyaluronic acid is 1.5%, and the mass fraction of wormwood polysaccharide is 4.5%. The composite use of the three polysaccharides has good long-lasting moisturizing properties, and magnetic stirring is performed at room temperature for 1.5h, and then in a water bath at 75°C for 1.5h to obtain a long-lasting moisturizing and antibacterial composition, and then quinoa starch microspheres loaded with inclusion complex are added, and high pressure homogenization is performed. The homogenization pressure is 700 bar, the homogenization time is 2.5 min, and the product is freeze-dried and crushed. The Chinese medicinal plant polysaccharides and hyaluronic acid are cross-linked to form a large and uniform three-dimensional network structure with good safety, film-forming and moisturizing properties. The quinoa starch microspheres carrying the inclusion compound form a gel by capturing water, thereby effectively adhering to the skin, increasing the effective contact between the quinoa starch microspheres carrying the inclusion compound and the skin, which is beneficial to enhancing transdermal absorption and better exerting the skin care effect, thereby obtaining a cosmetic jade composition additive.
[0091] Example 4
[0092] This embodiment proposes a cosmetic jade composition additive, comprising the following components in parts by weight: 60 parts of quinoa starch microspheres loaded with inclusion complexes and 10 parts of a long-lasting moisturizing and antibacterial composition.
[0093] The quinoa starch microspheres loaded with inclusion compound comprise the following components in parts by weight: 8 parts of quinoa starch porous microsphere base, 10 parts of beta-cyclodextrin and 40 parts of jade powder.
[0094] The long-acting moisturizing and antibacterial composition comprises the following components in parts by weight: 20 parts of Artemisia argyi polysaccharide, 20 parts of Dendrobium officinale polysaccharide, and 10 parts of hyaluronic acid.
[0095] The preparation method of quinoa starch microspheres loaded with inclusion compound specifically comprises the following steps:
[0096] (1) Grind the leftover materials of Xinjiang Hetian jade into coarse jade powder, then place it in an all-round planetary ball mill at a speed of 200rpm for 1h, and then grind it manually, sieve it, and dry it. Jade powder has the function of absorbing dirt and grease, and can effectively absorb dirt and grease on the surface of the skin, deeply clean the pores, and make the skin refreshed and non-greasy. The natural minerals and trace elements in the jade powder can penetrate into the bottom layer of the skin, replenish moisture for the skin, and make the skin supple and plump. Jade powder also has a certain anti-inflammatory effect, which can relieve skin inflammation and redness, while inhibiting bacterial growth, effectively reducing the occurrence of acne and blackheads, and obtaining jade powder;
[0097] (2) Wash the red and black quinoa seeds and dry them in a 40°C oven to constant weight. Use a grinder to grind them, and pass the coarse powder through a 100-mesh sieve. Add 10.0 g of quinoa powder to 20 mL of petroleum ether and soak overnight. Filter to remove the petroleum ether and dry in a fume hood. Add 20 mL of 0.3% sodium hydroxide solution to the defatted quinoa powder, stir evenly, and place in a constant temperature shaker at 30°C and a shaker speed of 160 rpm. The extraction time is 8 h. Centrifuge and remove the supernatant. The precipitate is divided into three layers, and the middle layer is taken. The white layer of precipitate is washed with deionized water until the pH is neutral, sieved to remove large particles of residual impurities, and the filtrate is centrifuged again to remove impurities on the top and bottom layers of the starch. The washing and centrifugation operations can be repeated until the starch is milky white and free of yellow and black impurities, and then freeze-dried and ground. The quinoa starch obtained by this process has excellent water retention and solubility, presents a polyhedral sphere, and has a uniform particle size distribution and a narrow range of about 1.0-3.0 μm. The particle size is significantly lower than that of other starches and is more suitable for preparing starch microspheres to obtain quinoa starch;
[0098] (3) Pour the quinoa starch described in step (1) into 2 times the amount of distilled water, mix and stir for 2 hours, freeze at -25°C for 5 hours, and then ultrasonically treat at room temperature for 1 hour. During the ultrasonic treatment, the frequency is 40KHz and the power is 500W. The cavitation effect of ultrasound is conducive to the formation of more pores inside the starch. Dry and crush, then add the ultrasonically frozen-thawed quinoa starch to 3 times the amount of acetic acid buffer solution with a pH of 5.0, mix evenly, and place in a constant temperature water bath at 55°C for 10 minutes, then add 10% α-amylase and 5% saccharifying enzyme, and keep it at 55°C for 10 minutes. Warm water bath for 12 hours, add 5% sodium hydroxide solution by mass to adjust the pH to 11.0, the hydrolysis reaction is completed, add 2 times the amount of anhydrous ethanol to inactivate the enzyme, wash repeatedly with anhydrous ethanol and distilled water for 5 times, filter, dry, crush, and ultrasonic pretreatment of quinoa starch before enzymolysis increases the number and proportion of starch micropores, thereby increasing the sensitivity of starch to enzymatic hydrolysis. Therefore, the ultrasonic freeze-thaw combined with enzymolysis technology can obtain porous starch with larger specific surface area and total pore volume, better swelling performance and adsorption performance, and obtain quinoa porous starch;
[0099] (4) Add 3 times the amount of 4% sodium hydroxide solution in the porous quinoa starch of step (3), mix well, and then place in a constant temperature water bath at 60°C and stir for 20 minutes. Cool the starch paste at room temperature and use it as the water phase. Measure 80 mL of soybean oil in a beaker, place it in a constant temperature water bath at 60°C, add 1.0 g of Span 80 for emulsification, stir magnetically for 10 minutes, cool to room temperature and use it as the oil phase. Add the water phase to the oil phase at a rate of 1 mL / min, stir at high speed for 30 minutes at a stirring speed of 2000 rpm, add a 60% epichlorohydrin solution, stir for 20 minutes at a stirring speed of 800 rpm, and stir until the mixture is dry. The amount of epichlorohydrin solution added is 5 mL, and epichlorohydrin reacts with hydroxyl groups on the surface of starch microspheres to form epoxy compounds, thereby cross-linking the starch microspheres and increasing the stability of the starch microspheres. After the reaction is completed, the upper oil phase is removed by centrifugation, and the precipitate is washed 5 times with ethyl acetate, anhydrous ethanol and acetone solution respectively, vacuum dried, and ground. The prepared microspheres can absorb more active ingredients and continuously release the active ingredients on the skin through a sustained release effect, thereby improving the absorption and utilization of active substances and reducing their irritation to the skin. The quinoa starch microspheres can also absorb dirt and grease on the skin, keeping it fresh and non-greasy, thereby enhancing the moisturizing and grease removal effects, and obtaining a quinoa starch porous microsphere substrate;
[0100] (5) Add 1.0 g of β-cyclodextrin to 100 mL of distilled water, heat and stir at a constant temperature for 20 min with magnetic stirring, control the temperature at 60° C., stir at 400 rpm, slowly add the jade powder described in step (1), continue stirring for 2 h, cool to room temperature, freeze-dry, and grind. Through the inclusion action of β-cyclodextrin, the active substance in the jade powder can be encapsulated in the structure, thereby improving its solubility and stability, promoting the penetration and absorption of the active ingredients, and allergic reactions.
[0101] (6) The quinoa starch porous microsphere substrate described in step (4) and the active inclusion compound described in step (5) are added to 200 mL of distilled water, ultrasonicated at room temperature for 30 minutes, and then placed in a constant temperature magnetic stirrer for stirring for 1 hour, the stirring temperature is 37° C., the stirring speed is 400 rpm, centrifuged, the upper liquid is removed, and the precipitate is washed with deionized water 3 times, vacuum dried, and ground. The quinoa starch porous microspheres are used as the substrate, and the active inclusion compound is loaded in the pores. Through the slow release method, the residence time of the active ingredient on the skin is prolonged, the penetration and absorption efficiency are improved, and the irritation and discomfort caused by rapid and direct contact with the skin are avoided, and the occurrence of adverse skin reactions is reduced. The porous microsphere structure also further enhances the moisturizing and oil absorption properties. After releasing the active inclusion compound, β-cyclodextrin penetrates through the skin stratum corneum, hair follicles and sweat ducts, thereby improving the absorption and utilization of jade powder in the skin, which is conducive to better exerting its oil adsorption effect, moisturizing effect and antibacterial and anti-inflammatory effects, and obtaining quinoa starch microspheres loaded with inclusion compounds.
[0102] This embodiment provides a method for preparing a cosmetic jade composition additive, which specifically comprises the following steps:
[0103] S1. Wash, dry and grind the wormwood leaf into fine powder, weigh 4.0g of wormwood leaf powder and add it to 200mL of water, stir evenly, add 2% of cellulase, and ultrasonically treat for 1h, the ultrasonic temperature is 50°C, the ultrasonic frequency is 40KHz, and the ultrasonic power is 550W. Centrifuge while hot, collect the filtrate, add 10 times the amount of anhydrous ethanol, let it stand overnight in a refrigerator, centrifuge, dry and grind the precipitate, and extract the wormwood polysaccharide by this method. It has good hygroscopicity, moisture retention, antibacterial and anti-inflammatory properties, reduces the infection and inflammation caused by bacterial growth, is conducive to keeping the skin fresh and healthy, and also has the effects of whitening and increasing skin elasticity, and obtains wormwood polysaccharide;
[0104] S2. Dissolve dendrobium polysaccharide, hyaluronic acid and wormwood polysaccharide described in step S1 in 100 mL of water to prepare a polysaccharide composite solution. In the polysaccharide composite solution, the mass fraction of dendrobium polysaccharide is 4%, hyaluronic acid is 2%, and the mass fraction of wormwood polysaccharide is 4%. The composite use of the three polysaccharides has good long-lasting moisturizing properties. Magnetic stirring is carried out at room temperature for 1 hour, and then the mixture is in a water bath at 80°C for 1 hour to obtain a long-lasting moisturizing and antibacterial composition. Then, quinoa starch microspheres loaded with inclusion complex are added, high-pressure homogenized, the homogenization pressure is 800 bar, the homogenization time is 2 min, freeze-dried and crushed, and a large and uniform three-dimensional network structure is formed by cross-linking and compounding traditional Chinese medicine plant polysaccharides with hyaluronic acid, which has good safety, film-forming properties and moisturizing properties. The quinoa starch microspheres loaded with inclusion complex form gels by capturing water, thereby effectively adhering to the skin, increasing the effective contact between the quinoa starch microspheres loaded with inclusion complex and the skin, which is beneficial to enhancing transdermal absorption and better exerting skin care effects, thereby obtaining a cosmetic jade composition additive.
[0105] Comparative Example 1
[0106] This comparative example provides a cosmetic jade composition additive, which differs from Example 1 in that the quinoa starch microspheres loaded with inclusion complex do not contain quinoa starch porous microsphere substrate; the preparation method of the quinoa starch microspheres loaded with inclusion complex does not include steps (2), (3), and (4); and the preparation method of the cosmetic jade composition additive is the same as that of Example 1.
[0107] Comparative Example 2
[0108] This comparative example provides a cosmetic jade composition additive, which differs from Example 1 in that the quinoa starch microspheres loaded with the inclusion compound do not contain β-cyclodextrin; the preparation method of the quinoa starch microspheres loaded with the inclusion compound does not include step (5); and the preparation method of the cosmetic jade composition additive is the same as that of Example 1.
[0109] Comparative Example 3
[0110] This comparative example provides a cosmetic jade composition additive, which differs from Example 1 in that the long-lasting moisturizing and antibacterial composition does not contain mugwort polysaccharide and dendrobium polysaccharide; the preparation method of quinoa starch microspheres loaded with inclusion complex is the same as that of Example 1; and the preparation method of the cosmetic jade composition additive does not include step S1.
[0111] Experimental Example 1
[0112] Moisturizing oil absorption test
[0113] Test sample: the cosmetic jade composition additive prepared in Examples 1-4 and Comparative Examples 1-3.
[0114] Test method: (1) Moisturizing performance: Weigh 1 g of the test sample that has been dried to a constant weight, weigh it accurately, put it into a weighing bottle, add 40 mL of purified water, rotate the weighing bottle to mix evenly, put it into a desiccator filled with dry micro-powder silica gel, place it for 48 hours, then weigh it, and calculate the moisture retention rate (%) according to the following formula;
[0115] (2) Oil absorption performance: Weigh 1 g of the test sample, add 50 mL of vegetable oil, stir on a stirrer at 300 rpm for 5 min, mix well and pour into a centrifuge tube, let stand at room temperature for about 30 min, then centrifuge at a speed of 3000 tpm for 30 min. Remove the upper layer of liquid, weigh the two separately, and calculate the oil absorption capacity per gram of the test sample according to the formula;
[0116] Moisture retention rate (%) = weight after placement / weight before placement × 100%
[0117] Oil absorption capacity (g / g) = (weight after oil absorption - weight before oil absorption) / weight before oil absorption
[0118] Figure 3 The moisturizing and oil absorption results of Examples 1-4 and Comparative Examples 1-3 are shown in the figure; as shown in the figure, the moisturizing rate and oil absorption capacity of Examples 1-4 are 78-82% and 0.83-0.88 g / g, respectively, indicating that the moisturizing and oil absorption performances are good; the moisturizing rate and oil absorption capacity of Comparative Examples 1-3 are 62-71% and 0.63-0.72 g / g, respectively, indicating that the moisturizing and oil absorption performances are poor; the quinoa starch microspheres loaded with the inclusion compound of Comparative Example 1 do not contain the quinoa starch porous microsphere substrate, and the active inclusion compound cannot be loaded, and the contact time of the active substance with the skin and the absorption and utilization cannot be increased in the form of slow release, which limits the Its moisturizing and oil absorption properties cannot be exerted, and the porous microsphere structure itself cannot exert its moisturizing and oil absorption effects, resulting in poor moisturizing and oil absorption properties; the quinoa starch microspheres loaded with inclusion complexes in Comparative Example 2 do not contain β-cyclodextrin, and cannot form inclusion complexes with jade powder, which is not conducive to improving the solubility of jade powder, and is not conducive to promoting its penetration and absorption, resulting in poor moisturizing and oil absorption properties; the long-acting moisturizing and antibacterial composition of Comparative Example 3 does not contain wormwood polysaccharides and dendrobium polysaccharides, and cannot form a gel film with lasting moisturizing properties, which is not conducive to prolonging the effective contact between the quinoa starch microspheres loaded with inclusion complexes and the skin, resulting in poor moisturizing and oil absorption properties.
[0119] Experimental Example 2
[0120] Antibacterial performance experiment
[0121] Test sample: the cosmetic jade composition additive prepared in Examples 1-4 and Comparative Examples 1-3.
[0122] Test method: In this experiment, Staphylococcus aureus and Escherichia coli, which are common causes of skin inflammation, were selected as experimental bacteria for antibacterial experiments. First, 1 g of the test sample was dissolved in 20 mL of water to obtain the test sample solution for standby use; the Oxford cup method was used to determine the antibacterial activity of the test sample. In a single-person double-sided clean workbench under sterile conditions, 15 mL of agar culture medium was poured into a sterile culture dish. After the culture medium was cooled and solidified, 200 μL of Staphylococcus aureus and Escherichia coli bacterial suspension was taken to the culture dish with a 200 μL pipette, and the bacterial solution was evenly spread with a coating rod. A 6 mm diameter Oxford cup was placed on the culture dish, and 200 μL of physiological saline was added to the Oxford cup. Three samples of each test sample solution were tested in parallel, and then the culture dish was placed in a biochemical incubator at (37±1) ℃ and cultured for 24 hours. The diameter (mm) of the inhibition zone was observed and measured; the larger the diameter of the inhibition zone, the stronger the inhibitory effect on the experimental bacteria.
[0123] Figure 4 The results of the antibacterial zone diameters of Examples 1-4 and Comparative Examples 1-3 are shown in FIG. As shown in the figure, the antibacterial zone diameters of Staphylococcus aureus and Escherichia coli of Examples 1-4 are 38-43 mm and 36-41 mm, respectively, both ≥ 36 mm, indicating that the antibacterial activity is relatively strong; the antibacterial zone diameters of Staphylococcus aureus and Escherichia coli of Comparative Examples 1-3 are 15-26 mm and 12-21 mm, respectively, both ≤ 26 mm, indicating that the antibacterial activity is relatively weak; the quinoa starch microspheres loaded with the inclusion complex of Comparative Example 1 do not contain quinoa starch porous microspheres The base cannot enhance the absorption and utilization rate of jade powder through sustained release, resulting in weak antibacterial activity; the quinoa starch microspheres loaded with inclusion complex in comparative example 2 do not contain β-cyclodextrin, and cannot enhance the penetration and absorption of jade powder through inclusion complex, resulting in weak antibacterial activity; the long-acting moisturizing antibacterial composition of comparative example 3 does not contain wormwood polysaccharides and dendrobium polysaccharides, and cannot exert the antibacterial effect of traditional Chinese medicine plant polysaccharides, nor is it conducive to enhancing transdermal absorption by prolonging the effective contact between the quinoa starch microspheres loaded with inclusion complex and the skin, resulting in weak antibacterial activity.
[0124] Experimental Example 3
[0125] Skin adverse reaction test
[0126] Test sample: the cosmetic jade composition additive prepared in Examples 1-4 and Comparative Examples 1-3.
[0127] Test method: 70 female volunteers aged 25-55 were selected and divided into 7 groups, with 10 people in each group. 1g of the test sample was added to other skin care products or cosmetics for skin testing once a day. After 30 days, the adverse skin reactions after use (common manifestations include redness, itching, pain, inflammation, etc.) were statistically analyzed.
[0128] Figure 5It is a result graph of the frequency of adverse skin reactions of Examples 1-4 and Comparative Examples 1-3; as shown in the figure, the frequency of adverse skin reactions of Examples 1-4 is 8-12 times, indicating that the occurrence of adverse skin reactions is effectively reduced; the frequency of adverse skin reactions of Comparative Examples 1-3 is 23-30 times, indicating that the occurrence of adverse skin reactions cannot be effectively reduced; the quinoa starch microspheres loaded with inclusion complexes in Comparative Example 1 do not contain quinoa starch porous microsphere substrate, cannot load active inclusion complexes, cannot exert a sustained-release effect, increase the irritation of jade powder to the skin, and result in the inability to effectively reduce the occurrence of adverse skin reactions; the quinoa starch microspheres loaded with inclusion complexes in Comparative Example 2 do not contain β-cyclodextrin, cannot reduce the irritation of jade powder to the skin through inclusion complexes, and result in the inability to effectively reduce the occurrence of adverse skin reactions; the long-acting moisturizing and antibacterial composition of Comparative Example 3 does not contain wormwood polysaccharides and dendrobium polysaccharides, and cannot exert the therapeutic effect of traditional Chinese medicine plant polysaccharides on skin inflammation, resulting in the inability to effectively reduce the occurrence of adverse skin reactions.
[0129] The above experimental results show that the moisturizing oil absorption, antibacterial property and skin adverse reactions of Examples 1-4 of the present invention are significantly better than those of Comparative Examples 1-3. Among them, the moisturizing oil absorption, antibacterial property and skin adverse reactions of Example 1 using quinoa starch microspheres loaded with inclusion compounds and long-term moisturizing antibacterial composition are better, more antibacterial and less adverse skin reactions. β-cyclodextrin is coated with jade powder and attached to the pores of the quinoa starch porous microsphere substrate. Through the microspheres and inclusion action, the slow release of jade powder is achieved, which not only increases the contact time with the skin, but also promotes the penetration and absorption of active ingredients, improves the moisturizing, oil absorption and antibacterial effects of jade powder, and effectively reduces its adverse stimulation to the skin. The long-term moisturizing and antibacterial composition formed by composite cross-linking of traditional Chinese medicine plant polysaccharides and natural polysaccharides, carries quinoa starch microspheres loaded with inclusion compounds, forms a gel film on the skin surface, has lasting moisturizing and antibacterial and anti-inflammatory properties, and also prolongs the effective contact between the quinoa starch microspheres loaded with inclusion compounds and the skin, which is conducive to enhancing its transdermal absorption and better exerting the beauty effects of moisturizing, oil absorption and antibacterial and anti-inflammatory.
[0130] While the embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that many changes, modifications, substitutions and variations can be made to the embodiments without departing from the principles and spirit of the invention.
[0131] The present invention and its implementation methods are described above, which is not restrictive. The drawings are only one of the implementation methods of the present invention, and the actual application is not limited thereto. In short, if ordinary technicians in the field are inspired by it and design methods and embodiments similar to the technical solution without creativity without departing from the purpose of the invention, they should all fall within the protection scope of the present invention.
Claims
1. A cosmetic jade composition additive, characterized in that: The cosmetic jade composition additive comprises the following components in parts by weight: 50-60 parts of quinoa starch microspheres loaded with inclusion complexes, and 10-20 parts of long-acting moisturizing and antibacterial compositions; the quinoa starch microspheres loaded with inclusion complexes comprise the following components in parts by weight: 5-8 parts of quinoa starch porous microsphere base, 10-20 parts of β-cyclodextrin, and 30-40 parts of jade powder; the long-acting moisturizing and antibacterial composition comprises the following components in parts by weight: 20-25 parts of wormwood polysaccharides, 20-25 parts of dendrobium polysaccharides, and 5-10 parts of hyaluronic acid.
2. A method for preparing the cosmetic jade composition additive according to claim 1, characterized in that: The specific steps include: S1. Wash, dry and grind the wormwood leaf into fine powder, weigh 4.0-5.0g of wormwood leaf powder, add it to 200mL of water, stir evenly, add 1-2% of cellulase, and ultrasonically treat for 1-2h, the ultrasonic temperature is 40-50℃, the ultrasonic frequency is 30-40KHz, the ultrasonic power is 500-550W, centrifuge while hot, collect the filtrate, add 5-10 times the amount of anhydrous ethanol, let it stand in a refrigerator overnight, centrifuge, dry and grind the precipitate to obtain wormwood polysaccharide; S2. Dissolve the dendrobium polysaccharide, hyaluronic acid and the wormwood polysaccharide described in step S1 in 100 mL of water to prepare a polysaccharide complex solution, stir magnetically at room temperature for 1-2 hours, and then bathe in water at 70-80° C. for 1-2 hours to obtain a long-lasting moisturizing and antibacterial composition, then add quinoa starch microspheres loaded with the inclusion complex, homogenize under high pressure at a homogenization pressure of 600-800 bar and a homogenization time of 2-3 minutes, freeze-dry and pulverize to obtain a cosmetic jade composition additive.
3. The method for preparing the cosmetic jade composition additive according to claim 2, wherein: In step S2, in the polysaccharide composite solution, the mass fraction of dendrobium polysaccharide is 4-5%, the mass fraction of hyaluronic acid is 1-2%, and the mass fraction of wormwood polysaccharide is 4-5%.
4. The method for preparing the cosmetic jade composition additive according to claim 3, wherein: The method for preparing quinoa starch microspheres loaded with inclusion compounds specifically comprises the following steps: (1) Grinding the leftover materials of Xinjiang Hetian jade into coarse jade powder, then placing it in an omnidirectional planetary ball mill at a speed of 100-200 rpm for 1-2 hours, and then manually grinding, sieving, and drying to obtain jade powder; (2) Wash the red and black quinoa seeds, dry them in a 40°C oven to constant weight, grind them with a grinder, pass the coarse powder through an 80-100 mesh sieve, add 5.0-10.0 g of quinoa powder to 10-20 mL of petroleum ether, soak overnight, remove the petroleum ether by suction, and dry in a fume hood, add 10-20 mL of 0.3% sodium hydroxide solution to the defatted quinoa powder, stir evenly, and place in a constant temperature shaker, control the temperature at 25-30°C, the shaker speed at 100-160 rpm, the extraction time at 8-12 h, centrifuge, remove the supernatant, and the precipitate is divided into three layers. Take the middle white layer of precipitate, wash it with deionized water until the pH is neutral, sieve it to remove large particles of residual impurities, centrifuge the filtrate again to remove impurities on the top and bottom layers of starch, and repeat the washing and centrifugation and impurity removal operations until the starch is milky white and free of yellow and black impurities, then freeze-dry and grind to obtain quinoa starch; (3) Pour the quinoa starch described in step (1) into 2 times the amount of distilled water, mix and stir for 2-3 hours, freeze at -25°C for 5-6 hours, then ultrasonically treat at room temperature for 1-2 hours, dry and crush, then add 3 times the amount of ultrasonically frozen-thawed quinoa starch to 3 times the amount of acetic acid buffer solution with a pH of 4.0-5.0, mix evenly, bath in a constant temperature water bath at 50-55°C for 10-15 minutes, then add 10-15% α-amylase and 5% saccharifying enzyme, bath in a constant temperature water bath at 50-55°C for 12-24 hours, add a 5% sodium hydroxide solution by mass to adjust the pH to 11.0, complete the hydrolysis reaction, add 2 times the amount of anhydrous ethanol to inactivate the enzyme, repeatedly wash with anhydrous ethanol and distilled water for 3-5 times, filter, dry, and crush to obtain quinoa porous starch; (4) Add 2-3 times the amount of the porous quinoa starch described in step (3) to a 4% sodium hydroxide solution, mix well, and place in a constant temperature water bath at 50-60°C, stir for 20-30 minutes, cool the starch paste at room temperature and use it as the aqueous phase, measure 50-80 mL of soybean oil in a beaker, place in a constant temperature water bath at 50-60°C, add 0.5-1.0 g of Span 80 for emulsification, stir magnetically for 10 minutes, cool to room temperature, and make The oil phase is set aside, the water phase is added to the oil phase at a speed of 1 mL / min, and the mixture is stirred at a high speed for 30-40 min at a stirring speed of 1000-2000 rpm. A 50-60% mass fraction of epichlorohydrin solution is added, and the mixture is stirred for 20-30 min at a stirring speed of 600-800 rpm. After the reaction is completed, the upper oil phase is removed by centrifugation, and the precipitate is washed 3-5 times with ethyl acetate, anhydrous ethanol and acetone solution respectively, and vacuum dried and ground to obtain a quinoa starch porous microsphere substrate; (5) Add 1.0-2.0 g of β-cyclodextrin to 100 mL of distilled water, heat and stir at a constant temperature for 20-30 min, control the temperature at 60°C, and stir at a speed of 300-400 rpm, slowly add the jade powder described in step (1), continue stirring for 2-3 h, cool to room temperature, freeze-dry, and grind to obtain an active inclusion compound; (6) Add the quinoa starch porous microsphere substrate described in step (4) and the active inclusion compound described in step (5) into 100-200 mL of distilled water, ultrasonicate at room temperature for 30-40 min, and then place in a constant temperature magnetic stirrer for stirring for 1-2 h at a stirring temperature of 37° C. and a stirring speed of 300-400 rpm. Centrifuge to remove the upper liquid, wash the precipitate with deionized water three times, vacuum dry, and grind to obtain quinoa starch microspheres loaded with the inclusion compound.
5. The method for preparing the cosmetic jade composition additive according to claim 4, wherein: In step (3), during the ultrasonic treatment, the frequency is 30-40KHz and the power is 400-500W.
6. The method for preparing the cosmetic jade composition additive according to claim 5, wherein: In step (4), the amount of epichlorohydrin solution added is 5-10 mL.
