A plant-derived polypeptide and a cosmetic containing the plant-derived polypeptide
The metal chelate of plant polypeptide formed by small molecule peptide produced by mung bean protease and copper ions formed by crosslinking chitosan and sodium alginate, and loading lecithin to prepare cosmetic premature cream with antibacterial and protective effects, solving the problem of the lack of antibacterial and protection of existing cosmetic premature creams and achieving the effect of improving skin permeability, reducing inflammation and irritating effects of cosmetics.
Patent Information
- Application Number
- CN202410440313.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-12
- Publication Date
- 2025-07-18
- Estimated Expiration
- 2044-04-12
AI Technical Summary
The existing makeup premature milk lacks antibacterial and protective effects, which cannot effectively reduce the damage caused by cosmetics to the skin, and is prone to breeding bacteria and affecting skin health.
A metal chelate of plant polypeptide formed by mung bean protease and formed by copper ions is used to combine a composite hydrogel ball formed by crosslinking chitosan and sodium alginate, and loaded with lecithin to prepare a cosmetic premature with antibacterial and protective effects.
Improve skin permeability, reduce inflammation, enhance antibacterial ability, form an oil protective layer, reduce the irritating impact of cosmetics on the skin, and maintain healthy skin.
Smart Images

Figure BDA0004788934830000101 
Figure BDA0004788934830000102 
Figure BDA0004788934830000111
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, in particular to a plant-derived polypeptide and cosmetics containing the plant-derived polypeptide. Background Art
[0002] Primer is a type of cosmetics. In the normal makeup process, primer is usually used first, and then other makeup products are used successively. In other words, primer is the first makeup process where makeup comes into contact with the human facial skin. In this process, primer can build a barrier between the skin and makeup, reducing the occurrence of powder particles in makeup entering the pores and textures. However, after opening cosmetics, they are stored at room temperature, which can easily breed bacteria and affect the health of the skin. Covering the face for a long time can also easily cause inflammation of the skin.
[0003] Most of the primers on the market are whitening cosmetics, which are mainly used to modify the uneven skin color and dullness. Local application can make the skin flawless, but lacks the ability to keep the skin healthy. In order to prevent the impact of subsequent makeup, the primer should also produce a protective oily film while having an antibacterial effect to reduce the damage of cosmetics to the skin. However, there are almost no primers that take into account both protective and antibacterial effects in the current market. The present invention will provide a plant-derived polypeptide and cosmetics containing the plant-derived polypeptide, namely a primer with antibacterial protective effects, to meet market demand. Summary of the invention
[0004] The object of the present invention is to provide a plant-derived polypeptide and cosmetics containing the plant-derived polypeptide to solve the problems existing in the prior art.
[0005] In order to solve the above technical problems, the present invention provides the following technical solutions: a plant-derived polypeptide and a cosmetic containing the plant-derived polypeptide, wherein the cosmetic is a primer prepared by using composite hydrogel spheres that embed plant polypeptide metal chelates and simultaneously load lecithin as an effective factor.
[0006] Furthermore, the plant polypeptide metal chelate is a compound formed by chelating a small molecule peptide hydrolyzed from mung bean protein with copper ions.
[0007] Furthermore, the composite hydrogel sphere is prepared by cross-linking calcium ions by free radical polymerization of chitosan and sodium alginate, and embedding plant polypeptide metal chelates.
[0008] Furthermore, a method for preparing a plant-derived polypeptide and a cosmetic containing the plant-derived polypeptide comprises the following preparation steps:
[0009] (1) Dissolve 40 g of mung bean protein in 1 L of deionized water. First, pretreat it in a water bath at 90 °C for 20 min. After the temperature drops to 55 °C, adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution. Add 5 mL of alkaline protease and maintain the pH at 9 with 0.5 mol / L sodium hydroxide aqueous solution. After hydrolysis for 4 h, inactivate the enzyme in a boiling water bath at 100 °C for 1 h to obtain a hydrolyzate. Cool the hydrolyzate to 25 °C, adjust the pH value to 7 with 1 mol / L hydrochloric acid aqueous solution, and then centrifuge at 5000 rpm for 20 min to obtain the supernatant. Filter the supernatant through an ultrafiltration membrane under a pressure of 0.25 MPa to obtain a filtrate of small molecular peptides of mung bean protein. Lyophilize the filtrate of small molecular peptides of mung bean protein for later use. Dissolve 50 g of small molecular peptides of mung bean protein in 1 L of deionized water, adjust the pH to 6 with 1 mol / L hydrochloric acid aqueous solution, add 1 - 9 mg of copper sulfate hydrate, and stir at a speed of 200 rpm for chelation reaction. The reaction temperature is 50 °C, and the reaction time is 60 - 100 min. After the reaction, cool to 25 °C, precipitate with 3 L of absolute ethanol for 2 - 5 h, centrifuge at 10000 rpm for 15 min, collect the precipitate, and wash it 3 times with absolute ethanol. First, set the temperature of the oven to 65 °C and bake for 1 h, then reduce the temperature to 30 °C and bake the chelate for 3 h to obtain a plant polypeptide metal chelate;
[0010] (2) Dissolve 10 - 20 g of chitosan in 1 L of deionized water, dropwise add 20 - 200 g of methacrylic anhydride, and adjust the pH to 8 - 10 with an alkaline solution, stir at 60 rpm for 20 min to obtain a chitosan aqueous solution. Dissolve 10 - 20 g of sodium alginate in 1 L of deionized water, dropwise add 20 - 200 g of methacrylic anhydride, and adjust the pH to 8 - 10 with an alkaline solution, stir at 60 rpm for 20 min to obtain a sodium alginate aqueous solution. Mix the chitosan aqueous solution and the sodium alginate aqueous solution with a mass ratio of 1:10 - 10:1 to obtain a mixed solution. First, add 0.5 - 1.5% of the plant polypeptide metal chelate based on the total mass of the mixed solution, stir at 60 rpm for 20 min, then add 5 - 15% of calcium chloride based on the mass of sodium alginate, mix and stir at 60 rpm for 30 min. Add a photoinitiator to the solution and irradiate it under a 100 W ultraviolet lamp for 2 - 10 min to obtain hydrogel beads. Put 50 g of hydrogel beads into 1 L of deionized water, add 2 - 5 g of lecithin, and stir slowly at 20 rpm for 2 h. After the reaction is completed, filter to obtain the filtrate, and wash it 3 times with deionized water to prepare composite hydrogel beads;
[0011] (3) Add appropriate amount of deionized water, 2 - 6 g of glycerol, 5 - 9 g of butanediol, and 2 - 3 g of ethanol to the water pot, heat it up to 85 °C, maintain for 10 min, then cool it down to 65 °C, add 1 - 3 g of 1,2 - pentanediol, and stir at 60 rpm for 5 min to prepare the water pot material; then add 2 - 5 g of cyclopentasiloxane, 2 - 3 g of PEG - 10 dimethicone, 3 - 5 g of trimethylsiloxysilicate, 6 - 8 g of phenyltrimethicone, 3 - 5 g of lauryl PEG - 9 dimethicone / dimethicone copolymer, 2 - 6 g of glyceryl tri(ethylhexanoate), 3 - 5 g of octyl polymethylsiloxane, 1 - 3 g of polyglyceryl - 2 isostearate, and 1 - 3 g of composite hydrogel beads into the reaction pot, homogenize and disperse at 20 rpm for 20 min to obtain the reaction pot material; heat up to 65 °C, slowly add the water pot material into the reaction pot in 3 portions, and stir at 20 rpm for 10 min; when stirring and cooling down to 45 °C, add 0.1 - 1 g of phenoxyethanol, stir at 20 rpm for another 10 min, and then cool down to 25 °C to obtain the antibacterial and protective makeup primer.
[0012] Further, in the step (1), the ultrafiltration membrane is composed of ultrafiltration membranes with a molecular weight cut - off of 5 ku and 3 ku.
[0013] Further, in the step (1), the copper sulfate hydrate is CuSO4·5H2O.
[0014] Further, in the step (2), the alkaline solution is an aqueous sodium hydroxide solution with a concentration of 0.5 mol / L.
[0015] Further, in the step (2), the photoinitiator is I2959, and the addition amount of the photoinitiator is 0.05 - 0.25% of the volume of the mixed solution.
[0016] Further, in the step (2), the ultraviolet intensity is 3600 - 6000 μW / cm.
[0017] Further, in the step (3), the addition amount of deionized water is 30 - 40 g.
[0018] Compared with the prior art, the beneficial effects achieved by the present invention are:
[0019] The present invention prepares composite hydrogel beads embedded with plant polypeptide metal chelates and loaded with lecithin at the same time. Using such composite hydrogel beads as an effective factor and adding them into the makeup primer to prepare a makeup primer with antibacterial and protective effects.
[0020] First, mung bean protein is enzymatically hydrolyzed to generate small peptides composed of three to six amino acids. Through the action of coordination covalent chemical bonds, a chemically stable complex is formed between copper ions and mung bean small peptides. Under appropriate conditions, groups such as the amino group on the main component arginine of the small peptide can act as ligands to provide electrons for metal copper ions, forming a stable plant polypeptide-metal chelate. This metal chelate can act on facial skin, improve its permeability, enhance the penetration so that arginine can enter the skin, effectively stimulate mitochondrial activity, accelerate cell metabolism, thereby increasing the resistance of cells to external stimuli and reducing inflammation. Moreover, metal copper ions themselves have a certain antibacterial effect, and the two combine synergistically, making the skin less susceptible to bacterial infection during the subsequent makeup application after using the primer. Mung bean polypeptide, as a plant extract, has low antigenicity and will not cause allergic reactions even when directly acting on the inner layer of the skin.
[0021] Secondly, using natural polymer chitosan and natural extract sodium alginate as the matrix, a hydrogel embedding the chelate is prepared through free radical polymerization, and calcium ion cross-linking is supplemented to form hydrogel beads with a polymer network structure built by two molecular chains, making the hydrogel beads have good acid-base stability. This kind of hydrogel beads has a porous and rough surface structure that provides binding sites. The negatively charged lecithin electrostatically binds with the positively charged calcium ions, making lecithin stably loaded on the hydrogel beads. During use, the hydrogel beads are rubbed and squeezed, releasing the embedded plant polypeptide-metal chelate. While acting on the skin, it adsorbs lecithin to form a thin oil protection layer on the skin surface, making the subsequent makeup products of the primer less likely to have a negative irritating impact on the skin, thus achieving a protective effect. Specific implementation mode
[0022] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in combination with the embodiments of the present invention. Obviously, the described embodiments are only a 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 those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0023] To more clearly illustrate the method provided by the present invention, the following examples are used for detailed description. The test methods for various indicators of a plant-derived polypeptide and a cosmetic containing the plant-derived polypeptide prepared in the following examples are as follows:
[0024] Antibacterial property: The 24-hour slant cultures of the test bacteria (Staphylococcus aureus, Streptococcus, Escherichia coli) are washed down with PBS to make a bacterial suspension (the required concentration is: when 100 μL is dropped on the control sample piece or in 5 mL of the sample solution, the recovered number of bacteria is 1 104 -9 104cfu / ml). Take 5 ml each of the sample aqueous solutions with a concentration of 10% prepared from the samples of the examples and comparative examples and the reference substance (deionized water), with 4 tubes for each. Take the above-mentioned bacterial suspension and add 100 μL to each sample and reference substance respectively, and mix evenly. Start timing. After acting for 1 day, use sterile forceps to take the sample (0.5 mL) and put it into a test tube containing 5 mL of PBS, mix well, make appropriate dilutions, then take 2 - 3 dilution degrees, respectively pipette 0.5 mL, place it in two petri dishes, pour 15 mL of nutrient agar medium cooled to 40 - 45 °C, rotate the petri dish to make it fully uniform. After the agar solidifies, turn the plate over and culture at 35 °C ± 2 °C for 48 h, and perform viable bacterial colony counting. Calculate the antibacterial rate: X = (A - B) / A × 100%.
[0025] Protective property: Distribute the makeup primers prepared from the examples and comparative examples to 30 testers for comparative use. Evenly apply 0.5 ml of the makeup primer on the left face for 20 min, and evenly apply 0.5 ml of the moisturizing lotion without any functional factors on the right face for 20 min. Then evenly apply 1 ml of the same brand of liquid foundation on the whole face. After 8 h, the testers make evaluations according to their own feelings. The trial contents include: whether there is a sense of irritation, whether the facial skin is reddened, and whether the skin around the eyes is reddened when in contact; the evaluation criteria are "yes", "slight", and "no".
[0026] Example 1
[0027] (1) Dissolve 40 g of mung bean protein in 1 L of deionized water, first pretreat it in a water bath at 90 °C for 20 min. After the temperature drops to 55 °C, adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution, add 5 mL of alkaline protease, and use 0.5 mol / L sodium hydroxide aqueous solution to maintain the pH at 9. After hydrolysis for 4 h, inactivate the enzyme in a boiling water bath at 100 °C for 1 h to obtain a hydrolysis solution; cool the hydrolysis solution to 25 °C, adjust the pH value to 7 with 1 mol / L hydrochloric acid aqueous solution, then centrifuge at 5000 rpm for 20 min, and take the supernatant; filter the supernatant through an ultrafiltration membrane under a pressure of 0.25 MPa. The ultrafiltration membrane consists of ultrafiltration membranes with a molecular weight cut-off of 5 ku and 3 ku to obtain a filtrate of small molecular peptides of mung bean protein; freeze-dry the filtrate of small molecular peptides of mung bean protein for later use; dissolve 50 g of small molecular peptides of mung bean protein in 1 L of deionized water, adjust the pH to 6 with 1 mol / L hydrochloric acid aqueous solution, add 1 mg of CuSO4·5H2O, stir at a speed of 200 rpm for chelation reaction, the reaction temperature is 50 °C, the reaction time is 60 min. After the reaction, cool to 25 °C, precipitate with 3 L of absolute ethanol for 2 h, centrifuge at 10000 rpm for 15 min, collect the precipitate, and wash it 3 times with absolute ethanol; first adjust the temperature of the oven to 65 °C and bake for 1 h, then lower the temperature to 30 °C and bake the chelate for 3 h to obtain a plant polypeptide metal chelate;
[0028] (2) Dissolve 10 g of chitosan in 1 L of deionized water, dropwise add 20 g of methacrylic anhydride, and adjust the pH to 8 with a 0.5 mol / L sodium hydroxide aqueous solution. Stir at 60 rpm for 20 min to obtain an aqueous chitosan solution; dissolve 10 g of sodium alginate in 1 L of deionized water, dropwise add 20 g of methacrylic anhydride, and adjust the pH to 8 with a 0.5 mol / L sodium hydroxide aqueous solution. Stir at 60 rpm for 20 min to obtain an aqueous sodium alginate solution; mix the aqueous chitosan solution and the aqueous sodium alginate solution with a mass ratio of 1:10 to obtain a mixed solution. First, add 0.5% of the total mass of the mixed solution of the plant polypeptide metal chelate, stir at 60 rpm for 20 min, then add 5% of the mass of sodium alginate of calcium chloride, mix and stir at 60 rpm for 30 min. Add the photoinitiator I2959 to the solution, and the addition amount of the photoinitiator is 0.05% of the volume of the mixed solution. Irradiate under a 100 W ultraviolet lamp for 2 min, and the ultraviolet intensity is 3600 μW / cm to obtain hydrogel balls; put 50 g of hydrogel balls into 1 L of deionized water, add 2 g of lecithin, and slowly stir and react at 20 rpm for 2 h. After the reaction is completed, filter to obtain the filtrate, and wash it 3 times with deionized water to prepare composite hydrogel balls;
[0029] (3) Add 30 g of deionized water, 2 g of glycerol, 5 g of butanediol, and 2 g of ethanol to a water pot and heat it to 85 °C, keep it for 10 min, cool it to 65 °C, add 1 g of 1,2-pentanediol, and stir at 60 rpm for 5 min to prepare the water pot material; then add 2 g of cyclopentadimethylsiloxane, 2 g of PEG-10 polydimethylsiloxane, 3 g of trimethylsiloxysilicate, 6 g of phenylpolymethylsiloxane, 3 g of lauryl PEG-9 polydimethylsiloxane / polydimethylsiloxane, 2 g of glyceryl tri(ethylhexanoate), 3 g of octyl polymethylsiloxane, 1 g of polyglyceryl-2 isostearate, and 1 g of composite hydrogel balls to a reaction pot, and homogenize and disperse at 20 rpm for 20 min to prepare the reaction pot material; heat it to 65 °C, and slowly add the water pot material to the reaction pot in 3 portions, and stir at a speed of 20 rpm for 10 min; when stirring and cooling to 45 °C, add 0.1 g of phenoxyethanol, stir at a speed of 20 rpm for another 10 min, and cool to 25 °C to obtain the antibacterial protective makeup primer.
[0030] Example 2
[0031] (1) Dissolve 40 g of mung bean protein in 1 L of deionized water. First, pretreat it in a water bath at 90 °C for 20 min. After the temperature drops to 55 °C, adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution. Add 5 mL of alkaline protease and maintain the pH at 9 with 0.5 mol / L sodium hydroxide aqueous solution. After hydrolysis for 4 h, inactivate the enzyme in a boiling water bath at 100 °C for 1 h to obtain a hydrolysate. Cool the hydrolysate to 25 °C, adjust the pH value to 7 with 1 mol / L hydrochloric acid aqueous solution, and then centrifuge at 5000 rpm for 20 min to collect the supernatant. Filter the supernatant through an ultrafiltration membrane under a pressure of 0.25 MPa. The ultrafiltration membrane consists of ultrafiltration membranes with a molecular weight cut-off of 5 ku and 3 ku to obtain a filtrate of small molecular peptides of mung bean protein. Freeze-dry the filtrate of small molecular peptides of mung bean protein for later use. Dissolve 50 g of small molecular peptides of mung bean protein in 1 L of deionized water, adjust the pH to 6 with 1 mol / L hydrochloric acid aqueous solution, add 5 mg of CuSO4·5H2O, and stir at a speed of 200 rpm for chelation reaction. The reaction temperature is 50 °C and the reaction time is 80 min. After the reaction, cool to 25 °C, precipitate with 3 L of absolute ethanol for 3.5 h, centrifuge at 10000 rpm for 15 min, collect the precipitate, and wash it 3 times with absolute ethanol. First, set the temperature of the oven to 65 °C and bake for 1 h, then lower the temperature to 30 °C and bake the chelate for 3 h to obtain a plant polypeptide metal chelate;
[0032] (2) Dissolve 15 g of chitosan in 1 L of deionized water, dropwise add 110 g of methacrylic anhydride, and adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution, and stir at 60 rpm for 20 min to obtain a chitosan aqueous solution. Dissolve 15 g of sodium alginate in 1 L of deionized water, dropwise add 110 g of methacrylic anhydride, and adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution, and stir at 60 rpm for 20 min to obtain a sodium alginate aqueous solution. Mix the chitosan aqueous solution and the sodium alginate aqueous solution with a mass ratio of 1:1 to obtain a mixed solution. First, add 1% of the plant polypeptide metal chelate based on the total mass of the mixed solution, stir at 60 rpm for 20 min, then add 10% of calcium chloride based on the mass of sodium alginate, mix and stir at 60 rpm for 30 min. Add a photoinitiator I2959 to the solution. The addition amount of the photoinitiator is 0.1% of the volume of the mixed solution, and irradiate it under a 100 W ultraviolet lamp for 6 min. The ultraviolet intensity is 4800 μW / cm to obtain hydrogel beads. Put 50 g of hydrogel beads into 1 L of deionized water, add 3.5 g of lecithin, and stir slowly at 20 rpm for 2 h. After the reaction is completed, filter to obtain the filtrate and wash it 3 times with deionized water to prepare composite hydrogel beads;
[0033] (3) Add 35 g of deionized water, 4 g of glycerin, 7 g of butanediol, and 2.5 g of ethanol to the water pot and heat it to 85 °C. Keep it at this temperature for 10 min, then cool it down to 65 °C. Add 2 g of 1,2-pentanediol and stir at 60 rpm for 5 min to prepare the water pot material. Then add 3.5 g of cyclopentasiloxane, 2.5 g of PEG-10 dimethicone, 4 g of trimethylsiloxysilicate, 7 g of phenyl trimethicone, 4 g of lauryl PEG-9 dimethicone copolyol, 4 g of glyceryl triethylhexanoate, 4 g of octyl polymethylsiloxane, 2 g of polyglyceryl-2 isostearate, and 2 g of composite hydrogel beads to the reaction pot and homogenize and disperse them at 20 rpm for 20 min to obtain the reaction pot material. Heat it up to 65 °C and slowly add the water pot material to the reaction pot in 3 portions and stir at 20 rpm for 10 min. When stirring and cooling down to 45 °C, add 0.55 g of phenoxyethanol and stir at 20 rpm for another 10 min. Then cool it down to 25 °C to obtain the antibacterial protective makeup primer.
[0034] Example 3
[0035] (1) Dissolve 40 g of mung bean protein in 1 L of deionized water. First, pretreat it in a water bath at 90 °C for 20 min. After the temperature drops to 55 °C, adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution. Add 5 mL of alkaline protease and maintain the pH at 9 with 0.5 mol / L sodium hydroxide aqueous solution. After hydrolysis for 4 h, inactivate the enzyme in a boiling water bath at 100 °C for 1 h to obtain the hydrolyzate. Cool the hydrolyzate to 25 °C, adjust the pH value to 7 with 1 mol / L hydrochloric acid aqueous solution, and then centrifuge at 5000 rpm for 20 min to take the supernatant. Filter the supernatant through an ultrafiltration membrane under a pressure of 0.25 MPa. The ultrafiltration membrane consists of ultrafiltration membranes with a molecular weight cut-off of 5 ku and 3 ku to obtain the filtrate of mung bean protein small peptides. Freeze-dry the filtrate of mung bean protein small peptides for later use. Dissolve 50 g of mung bean protein small peptides in 1 L of deionized water, adjust the pH to 6 with 1 mol / L hydrochloric acid aqueous solution, add 9 mg of CuSO4·5H2O, and stir at 200 rpm for chelation reaction. The reaction temperature is 50 °C and the reaction time is 100 min. After the reaction, cool it down to 25 °C, precipitate it with 3 L of absolute ethanol for 5 h, centrifuge at 10000 rpm for 15 min, collect the precipitate, and wash it 3 times with absolute ethanol. First, set the temperature of the oven to 65 °C and bake for 1 h, then lower the temperature to 30 °C and bake the chelate for 3 h to obtain the plant polypeptide metal chelate.
[0036] (2) Dissolve 20 g of chitosan in 1 L of deionized water, dropwise add 200 g of methacrylic anhydride, and adjust the pH to 10 with a 0.5 mol / L sodium hydroxide aqueous solution. Stir at 60 rpm for 20 min to obtain a chitosan aqueous solution; dissolve 20 g of sodium alginate in 1 L of deionized water, dropwise add 200 g of methacrylic anhydride, and adjust the pH to 10 with a 0.5 mol / L sodium hydroxide aqueous solution. Stir at 60 rpm for 20 min to obtain a sodium alginate aqueous solution; mix the chitosan aqueous solution and the sodium alginate aqueous solution with a mass ratio of 10:1 to obtain a mixed solution. First, add 1.5% of the total mass of the mixed solution of plant polypeptide metal chelate, stir at 60 rpm for 20 min, then add 15% of the mass of calcium chloride based on sodium alginate, mix and stir at 60 rpm for 30 min. Add photoinitiator I2959 to the solution, and the addition amount of the photoinitiator is 0.25% of the volume of the mixed solution. Irradiate under a 100 W ultraviolet lamp for 10 min, and the ultraviolet intensity is 6000 μW / cm to obtain hydrogel beads; put 50 g of hydrogel beads into 1 L of deionized water, add 5 g of lecithin, and slowly stir and react at 20 rpm for 2 h. After the reaction is completed, filter to obtain the filtrate, and wash it 3 times with deionized water to prepare composite hydrogel beads;
[0037] (3) Add 40 g of deionized water, 6 g of glycerol, 9 g of butanediol, and 3 g of ethanol to a water pot and heat it to 85 °C, keep it for 10 min, cool it to 65 °C, add 3 g of 1,2-pentanediol, and stir at 60 rpm for 5 min to prepare the water pot material; then add 5 g of cyclopentasiloxane, 3 g of PEG-10 dimethicone, 5 g of trimethylsiloxysilicate, 8 g of phenyltrimethicone, 5 g of lauryl PEG-9 dimethicone / dimethicone copolymer, 6 g of glyceryl tri(ethylhexanoate), 5 g of octyl polymethylsiloxane, 3 g of polyglyceryl-2 isostearate, and 3 g of composite hydrogel beads to a reaction pot, and homogenize and disperse at 20 rpm for 20 min to prepare the reaction pot material; heat it to 65 °C, and slowly add the water pot material to the reaction pot in 3 portions, and stir at 20 rpm for 10 min; when stirring and cooling to 45 °C, add 1 g of phenoxyethanol, and stir at 20 rpm for another 10 min, and cool to 25 °C to obtain the antibacterial protective makeup primer.
[0038] Comparative Example 1
[0039] The difference between Comparative Example 1 and Example 2 lies in step (1). Modify step (1) as follows: Dissolve 40 g of mung bean protein in 1 L of deionized water, first pretreat it in a water bath at 90 °C for 20 min. After the temperature drops to 55 °C, adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution, add 5 mL of alkaline protease, and maintain the pH at 9 with 0.5 mol / L sodium hydroxide aqueous solution. After hydrolysis for 4 h, inactivate the enzyme by boiling water bath at 100 °C for 1 h to obtain a hydrolysate; cool the hydrolysate to 25 °C, adjust the pH value to 7 with 1 mol / L hydrochloric acid aqueous solution, then centrifuge at 5000 rpm for 20 min, take the supernatant to obtain a mung bean protein heteropeptide filtrate; freeze-dry the mung bean protein heteropeptide filtrate for later use; dissolve 50 g of mung bean protein heteropeptide in 1 L of deionized water, adjust the pH to 6 with 1 mol / L hydrochloric acid aqueous solution, add 5 mg of CuSO4·5H2O, and stir at a speed of 200 rpm for chelation reaction. The reaction temperature is 50 °C and the reaction time is 80 min. After the reaction, cool to 25 °C, precipitate with 3 L of absolute ethanol for 3.5 h, centrifuge at 10000 rpm for 15 min, collect the precipitate, and wash it 3 times with absolute ethanol; first adjust the temperature of the oven to 65 °C and bake for 1 h, then lower the temperature to 30 °C and bake the chelate for 3 h to obtain a plant polypeptide metal chelate; the remaining steps are the same as those in Example 2.
[0040] Comparative Example 2
[0041] The difference between Comparative Example 2 and Example 2 lies in steps (1) and (2). Modify steps (1) and (2) as follows: (1) Dissolve 40 g of mung bean protein in 1 L of deionized water, first pretreat it in a water bath at 90 °C for 20 min. After the temperature drops to 55 °C, adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution, add 5 mL of alkaline protease, and maintain the pH at 9 with 0.5 mol / L sodium hydroxide aqueous solution. After hydrolysis for 4 h, inactivate the enzyme by boiling water bath at 100 °C for 1 h to obtain a hydrolysate; cool the hydrolysate to 25 °C, adjust the pH value to 7 with 1 mol / L hydrochloric acid aqueous solution, then centrifuge at 5000 rpm for 20 min, take the supernatant; filter the supernatant through an ultrafiltration membrane under a pressure of 0.25 MPa. The ultrafiltration membrane consists of ultrafiltration membranes with a molecular weight cut-off of 5 ku and 3 ku to obtain a mung bean protein small peptide filtrate; centrifuge the mung bean protein small peptide filtrate at 10000 rpm for 15 min, collect the precipitate, and wash it 3 times with absolute ethanol; first adjust the temperature of the oven to 50 °C and bake for 1 h, then lower the temperature to 30 °C and dry for 3 h to obtain a plant polypeptide;
[0042] (2) Dissolve 15 g of chitosan in 1 L of deionized water, dropwise add 110 g of methacrylic anhydride, and adjust the pH to 9 with a 0.5 mol / L sodium hydroxide aqueous solution. Stir at 60 rpm for 20 min to obtain a chitosan aqueous solution; dissolve 15 g of sodium alginate in 1 L of deionized water, dropwise add 110 g of methacrylic anhydride, and adjust the pH to 9 with a 0.5 mol / L sodium hydroxide aqueous solution. Stir at 60 rpm for 20 min to obtain a sodium alginate aqueous solution; mix the chitosan aqueous solution and the sodium alginate aqueous solution with a mass ratio of 1:1 to obtain a mixed solution. First, add 1% of the total mass of the mixed solution of plant polypeptide, stir at 60 rpm for 20 min, then add 10% of the mass of sodium alginate of calcium chloride, mix and stir at 60 rpm for 30 min. Add photoinitiator I2959 to the solution, and the addition amount of the photoinitiator is 0.1% of the volume of the mixed solution. Irradiate under a 100 W ultraviolet lamp for 6 min, and the ultraviolet intensity is 4800 μW / cm to obtain hydrogel balls; put 50 g of hydrogel balls into 1 L of deionized water, add 3.5 g of lecithin, and slowly stir and react at 20 rpm for 2 h. After the reaction is completed, filter to obtain the filtrate, and wash it 3 times with deionized water to prepare composite hydrogel balls; the remaining steps are the same as in Example 2.
[0043] Comparative Example 3
[0044] The difference between Comparative Example 3 and Example 2 is that step (2) is not carried out, and step (3) is changed to: add 35 g of deionized water, 4 g of glycerol, 7 g of butanediol, and 2.5 g of ethanol to the water pot and heat up to 85 °C, keep for 10 min, cool down to 65 °C, add 2 g of 1,2-pentanediol, and stir at 60 rpm for 5 min to prepare the water pot material; then add 3.5 g of cyclopentasiloxane, 2.5 g of PEG-10 dimethicone, 4 g of trimethylsiloxysilicate, 7 g of phenyltrimethylsiloxane, 4 g of lauryl PEG-9 dimethicone dimethicone, 4 g of glyceryl tri(ethylhexanoate), 4 g of octyl polymethylsiloxane, 2 g of polyglyceryl-2 isostearate, 1.5 g of plant polypeptide, and 0.5 g of lecithin to the reaction pot, and homogenize and disperse at 20 rpm for 20 min to prepare the reaction pot material; heat up to 65 °C, and slowly add the water pot material to the reaction pot in 3 portions, and stir at 20 rpm for 10 min; when stirring and cooling down to 45 °C, add 0.55 g of phenoxyethanol, and stir at 20 rpm for another 10 min, and cool down to 25 °C to obtain the antibacterial protective makeup primer; the remaining steps are the same as in Example 2.
[0045] Comparative Example 4
[0046] The difference between Comparative Example 4 and Example 2 lies in step (2). Step (2) is changed to: Dissolve 15 g of chitosan in 1 L of deionized water, dropwise add 110 g of methacrylic anhydride, and adjust the pH to 9 with a 0.5 mol / L sodium hydroxide aqueous solution, stir at 60 rpm for 20 min to obtain a chitosan aqueous solution; dissolve 15 g of sodium alginate in 1 L of deionized water, dropwise add 110 g of methacrylic anhydride, and adjust the pH to 9 with a 0.5 mol / L sodium hydroxide aqueous solution, stir at 60 rpm for 20 min to obtain a sodium alginate aqueous solution; mix the chitosan aqueous solution and the sodium alginate aqueous solution with a mass ratio of 1:1 to obtain a mixed solution. First, add 1% of the total mass of the mixed solution of plant polypeptide metal chelate, stir at 60 rpm for 20 min, then add photoinitiator I2959 to the solution. The addition amount of the photoinitiator is 0.1% of the volume of the mixed solution, irradiate under a 100 W ultraviolet lamp for 6 min, and the ultraviolet intensity is 4800 μW / cm to obtain hydrogel beads; put 50 g of hydrogel beads into 1 L of deionized water, add 3.5 g of lecithin, stir and react at a slow speed of 20 rpm for 2 h. After the reaction is completed, filter to obtain the filtrate, and wash it 3 times with deionized water to prepare composite hydrogel beads; the remaining steps are the same as in Example 2.
[0047] Comparative Example 5
[0048] The difference between Comparative Example 5 and Example 2 lies in step (2). Step (2) is changed to: Dissolve 15 g of chitosan in 1 L of deionized water, dropwise add 110 g of methacrylic anhydride, and adjust the pH to 9 with a 0.5 mol / L sodium hydroxide aqueous solution, stir at 60 rpm for 20 min to obtain a chitosan aqueous solution; dissolve 15 g of sodium alginate in 1 L of deionized water, dropwise add 110 g of methacrylic anhydride, and adjust the pH to 9 with a 0.5 mol / L sodium hydroxide aqueous solution, stir at 60 rpm for 20 min to obtain a sodium alginate aqueous solution; mix the chitosan aqueous solution and the sodium alginate aqueous solution with a mass ratio of 1:1 to obtain a mixed solution. First, add 1% of the total mass of the mixed solution of plant polypeptide metal chelate, stir at 60 rpm for 20 min, then add 10% of calcium chloride based on the mass of sodium alginate, mix and stir at 60 rpm for 30 min, add photoinitiator I2959 to the solution. The addition amount of the photoinitiator is 0.1% of the volume of the mixed solution, irradiate under a 100 W ultraviolet lamp for 6 min, and the ultraviolet intensity is 4800 μW / cm to obtain composite hydrogel beads; the remaining steps are the same as in Example 2.
[0049] Effect Example
[0050] The performance analysis results of a plant-derived polypeptide and a cosmetic containing the plant-derived polypeptide using Examples 1 to 3 and Comparative Examples 1 to 5 of the present invention are given in Table 1 and Table 2 below.
[0051] Table 1
[0052]
[0053] Table 2
[0054]
[0055]
[0056] From the comparison of the experimental data on the antibacterial properties between the examples and the comparative examples, it can be found that in the present invention, mung bean protease is hydrolyzed to generate small molecular peptides composed of three to six amino acids. Through the action of coordination covalent chemical bonds, a chemically stable complex of copper ions and mung bean small molecular peptides is formed. Under appropriate conditions, groups such as amino groups on the main component arginine of the small molecular peptide can serve as ligands to provide electrons for metal copper ions, forming a stable plant polypeptide metal chelate; this metal chelate can act on the facial skin, improve its permeability, enhance the penetration so that arginine can enter the skin interior, effectively stimulate mitochondrial activity, accelerate cell metabolism, thereby increasing the resistance of cells to external stimuli and reducing inflammation; and the metal copper ions themselves have a certain antibacterial effect, and the two combine synergistically, making the skin after using the primer less likely to be infected by bacteria during the subsequent makeup application process. From the comparison of the experimental data on the protection between the examples and the comparative examples, it can be found that in the present invention, a natural polymer chitosan and a natural extract sodium alginate are used as matrices, and a hydrogel embedding the chelate is prepared by free radical polymerization, supplemented with calcium ion cross-linking to form hydrogel spheres with a polymer network structure built by two molecular chains, making the hydrogel spheres have good acid-base stability. The porous and rough surface structure of this hydrogel sphere provides binding sites, and the negatively charged lecithin electrostatically binds with the positively charged calcium ions, making the lecithin stably loaded on the hydrogel spheres; during use, the hydrogel spheres are rubbed and squeezed, releasing the embedded plant polypeptide metal chelate, which acts on the skin and at the same time adsorbs lecithin to form a thin oil protection layer on the skin surface, making the subsequent makeup products of the primer less likely to have a negative irritating effect on the skin, thus achieving a protective effect and significantly reducing the phenomena of sensitivity and redness. As a plant extract, mung bean polypeptide has low antigenicity and will not cause an allergic reaction even when directly acting on the skin interior.
[0057] It is obvious to those skilled in the art that the present invention is not limited to the details of the above-described exemplary embodiments, and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention. Therefore, in any aspect, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Thus, all changes that fall within the meaning and scope of the equivalent elements of the claims are intended to be embraced within the present invention. Any reference signs in the claims should not be construed as limiting the claim concerned.
Claims
1. A cosmetic containing plant-derived polypeptide, wherein the cosmetic is a makeup primer prepared by using composite hydrogel balls embedding plant polypeptide metal chelates to simultaneously load lecithin as an effective factor, and is characterized in that, It includes the following preparation steps: (1) Dissolve 40 g of mung bean protein in 1 L of deionized water, first pretreat it in a water bath at 90 °C for 20 min. After the temperature drops to 55 °C, adjust the pH to 9 with 0.5 mol / L sodium hydroxide aqueous solution, add 5 mL of alkaline protease, and maintain the pH at 9 with 0.5 mol / L sodium hydroxide aqueous solution. After hydrolysis for 4 h, inactivate the enzyme in a boiling water bath at 100 °C for 1 h to obtain a hydrolyzate; cool the hydrolyzate to 25 °C, adjust the pH value to 7 with 1 mol / L hydrochloric acid aqueous solution, then centrifuge at 5000 rpm for 20 min, and take the supernatant; filter the supernatant through an ultrafiltration membrane under a pressure of 0.25 MPa to obtain a filtrate of mung bean protein small peptides; freeze-dry the filtrate of mung bean protein small peptides for later use; dissolve 50 g of mung bean protein small peptides in 1 L of deionized water, adjust the pH to 6 with 1 mol / L hydrochloric acid aqueous solution, add 1 - 9 mg of copper sulfate hydrate, and stir at a speed of 200 rpm for chelation reaction. The reaction temperature is 50 °C, and the reaction time is 60 - 100 min. After the reaction, cool to 25 °C, precipitate with 3 L of absolute ethanol for 2 - 5 h, centrifuge at 10000 rpm for 15 min, collect the precipitate, and wash it 3 times with absolute ethanol; first adjust the temperature of the oven to 65 °C and bake for 1 h, then lower the temperature to 30 °C and bake the chelate for 3 h to obtain a plant polypeptide metal chelate; (2) Dissolve 10 - 20 g of chitosan in 1 L of deionized water, dropwise add 20 - 200 g of methacrylic anhydride, and adjust the pH to 8 - 10 with an alkaline solution, stir at 60 rpm for 20 min to obtain a chitosan aqueous solution; dissolve 10 - 20 g of sodium alginate in 1 L of deionized water, dropwise add 20 - 200 g of methacrylic anhydride, and adjust the pH to 8 - 10 with an alkaline solution, stir at 60 rpm for 20 min to obtain a sodium alginate aqueous solution; mix the chitosan aqueous solution and the sodium alginate aqueous solution with a mass ratio of 1:10 - 10:1 to obtain a mixed solution. First add 0.5 - 1.5% of the plant polypeptide metal chelate based on the total mass of the mixed solution, stir at 60 rpm for 20 min, then add 5 - 15% of calcium chloride based on the mass of sodium alginate, mix and stir at 60 rpm for 30 min. Add a photoinitiator to the solution and irradiate it under a 100 W ultraviolet lamp for 2 - 10 min to obtain hydrogel beads; put 50 g of hydrogel beads into 1 L of deionized water, add 2 - 5 g of lecithin, stir slowly at 20 rpm for 2 h, after the reaction is completed, filter to obtain the filtrate, and wash it 3 times with deionized water to prepare composite hydrogel beads; (3) Add appropriate amount of deionized water, 2 - 6 g of glycerol, 5 - 9 g of butanediol, and 2 - 3 g of ethanol into the water pot, heat up to 85 °C, maintain for 10 min, cool down to 65 °C, add 1 - 3 g of 1,2 - pentanediol, stir at 60 rpm for 5 min to prepare the water pot material; then add 2 - 5 g of cyclopentasiloxane, 2 - 3 g of PEG - 10 dimethicone, 3 - 5 g of trimethylsiloxysilicate, 6 - 8 g of phenyltrimethicone, 3 - 5 g of lauryl PEG - 9 dimethicone / dimethicone copolymer, 2 - 6 g of glyceryl tri(ethylhexanoate), 3 - 5 g of octyl polymethylsiloxane, 1 - 3 g of polyglyceryl - 2 isostearate, and 1 - 3 g of composite hydrogel beads into the reaction pot, homogenize and disperse at 20 rpm for 20 min to obtain the reaction pot material; heat up to 65 °C, slowly add the water pot material into the reaction pot in 3 portions, stir at 20 rpm for 10 min; when stirring and cooling down to 45 °C, add 0.1 - 1 g of phenoxyethanol, stir at 20 rpm for another 10 min, and cool down to 25 °C to obtain the antibacterial protective makeup primer.
2. The cosmetic containing plant-derived polypeptide according to claim 1, characterized in that, In the step (1), the ultrafiltration membrane is composed of ultrafiltration membranes with a molecular weight cut - off of 5 ku and 3 ku.
3. The cosmetic containing plant-derived polypeptide according to claim 1, characterized in that, In the step (1), the copper sulfate hydrate is CuSO4·5H2O.
4. The cosmetic containing a plant-derived polypeptide according to claim 1, characterized in that, In the step (2), the alkaline solution is a 0.5 mol / L aqueous sodium hydroxide solution.
5. The cosmetic containing a plant-derived polypeptide according to claim 1, wherein In the step (2), the photoinitiator is I2959, and the addition amount of the photoinitiator is 0.05 - 0.25% of the volume of the mixed solution.
6. The cosmetic containing a plant-derived polypeptide according to claim 1, characterized in that, In the step (2), the ultraviolet intensity is 3600 - 6000 μW / cm.
7. The cosmetic containing a plant-derived polypeptide according to claim 1, characterized in that, In the step (3), the addition amount of deionized water is 30 - 40 g.
Citation Information
Patent Citations
Self-assembled polypeptide nano hydrogel chelated with copper ions and preparation method of self-assembled polypeptide nano hydrogel
CN113480601A