A method for preparing a polypeptide composition having anti-wrinkle efficacy
Patent Information
- Application Number
- CN202611100729.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-07-23
- Publication Date
- 2026-10-30
AI Technical Summary
[0002]面部皱纹分为动态表情纹与静态衰老纹，单一多肽仅能作用单一通路，抗皱效果有限，目前市面上主流抗皱活性多肽主要包括类肉毒素多肽，分别从抑制神经递质释放、促进真皮胶原合成、修复皮肤屏障、舒缓肌肉收缩四条通路改善皱纹，行业常规方案是将多种多肽简单复配，搭配多元醇、保湿剂制成多肽复合原液，直接添加至护肤产品中，依靠多肽协同作用提升抗皱功效，现有常规制备工艺多采用单反应釜一步式投料，将水、保湿剂、多肽粉末同步高温搅拌溶解，设备仅采用普通单层搅拌反应釜，无独立多肽预溶、精准温控、在线pH自动调控模块，为克服传统一步式多肽复配工艺活性损耗大、多肽易析出、pH难以稳定、透皮效果差、生产设备集成度低、产品刺激性高的缺陷，本发明设计专用分段温控多肽制备装置，提供两种改良复配工艺（脂质体包埋增效工艺、天然植物小分子肽复配温和工艺），通过独立预溶、PLC分段控温、在线pH联动调节、无菌低温过滤一体化设计，解决多肽高温降解、团聚沉淀、储存易氧化等行业痛点，同时兼顾透皮吸收与敏感肌适用性，实现高活性、高稳定性、可连续工业化生产的抗皱多肽组合物制备，因此需要一种具有抗皱功效的多肽组合物的制备方法
[0018]采用改进方案，通过多罐体独立温控分离高温基质配制与多肽投料，PLC超温联锁保护，避免多肽高温降解失活，同时多肽单独预溶罐实现多肽提前充分溶解，防止直接入水团聚析出，在线pH实时联动缓冲计量泵，全程稳定多肽活性适宜pH区间，并且脂质均质系统可实现多肽脂质体包裹，提升透皮吸收与蓝铜肽抗氧化稳定性，末端0.22μm无菌过滤单元，无需高温灭菌，全程低温保证多肽活性，成品无防腐剂刺激风险。
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Figure CN122997983A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of cosmetic polypeptide active ingredient preparation technology, specifically a method for preparing a polypeptide composition with anti-wrinkle effects. Background Technology
[0002] Facial wrinkles are divided into dynamic expression lines and static aging lines. Single peptides can only act on a single pathway, resulting in limited anti-wrinkle effects. Currently, the mainstream anti-wrinkle active peptides on the market mainly include botulinum toxin-like peptides, which improve wrinkles through four pathways: inhibiting neurotransmitter release, promoting dermal collagen synthesis, repairing the skin barrier, and relaxing muscle contraction. The industry's conventional approach is to simply combine multiple peptides with polyols and moisturizers to create a peptide complex stock solution, which is then directly added to skincare products, relying on the synergistic effect of peptides to enhance anti-wrinkle efficacy. Existing conventional preparation processes mostly use a single-reactor one-step feeding method, simultaneously dissolving water, moisturizers, and peptide powder at high temperatures. The equipment only uses a common single-layer stirred reactor, lacking independent peptide pre-dissolution, precise temperature control, and online automatic pH adjustment modules. To overcome the shortcomings of traditional one-step peptide compounding processes, such as high activity loss, easy peptide precipitation, difficulty in pH stability, poor transdermal effect, low integration of production equipment, and high product irritation, this invention designs a dedicated segmented temperature-controlled peptide preparation device, providing two improved compounding processes (liposome encapsulation enhancement process and mild natural plant small molecule peptide compounding process). Through independent pre-dissolution, PLC segmented temperature control, online pH linkage adjustment, and aseptic low-temperature filtration integrated design, it solves industry pain points such as high-temperature degradation, aggregation and precipitation, and easy oxidation during storage of peptides. At the same time, it takes into account transdermal absorption and suitability for sensitive skin, realizing the preparation of anti-wrinkle peptide compositions with high activity, high stability, and continuous industrial production. Therefore, a method for preparing peptide compositions with anti-wrinkle effects is needed.
[0003] Currently used peptide compositions suffer from several drawbacks: high temperatures cause peptide bonds to break, copper peptides to oxidize and become ineffective, resulting in low activity retention; direct contact of peptide powder with water leads to agglomeration and the formation of insoluble microparticles, resulting in poor product transparency; the pH of the system fluctuates greatly due to manual adjustment, shortening the shelf life; free peptides have difficulty penetrating the stratum corneum, resulting in weak deep anti-wrinkle effects; synthetic peptide systems are highly irritating and unsuitable for sensitive skin; traditional equipment lacks integrated modules for segmented temperature control, independent pre-dissolution, and aseptic filtration, leading to poor batch stability and an inability to achieve integrated production of liposome encapsulation or plant peptide compounding. Summary of the Invention
[0004] The purpose of this invention is to provide a method for preparing a polypeptide composition with anti-wrinkle effects, so as to solve the problems mentioned in the background art.
[0005] To achieve the above objectives, the present invention provides the following technical solution:
[0006] A method for preparing a polypeptide composition with anti-wrinkle effects includes a core anti-wrinkle polypeptide component, moisturizing and stabilizing excipients, a complete standard preparation process, and a natural plant compound polypeptide process.
[0007] Preferably, the core anti-wrinkle polypeptide components include acetyl hexapeptide-8: 0.1% to 0.5%, palmitoyl tripeptide 1 + tetrapeptide 7: 0.08% to 0.3%, blue copper peptide GHK-Cu: 0.02% to 0.15%, and snake venom-like peptide: 0.05% to 0.2%.
[0008] Preferably, the moisturizing and stabilizing excipients include polyols, active agents, stabilizers, mild preservatives, and solvents.
[0009] Preferably, the complete standard preparation process includes aqueous matrix preparation, separate pre-dissolution of peptides, low-temperature compounding and pH adjustment, maturation, and filtration.
[0010] Preferably, the natural plant compound polypeptide process includes plant peptide preparation, formulation optimization, and feeding operations.
[0011] A method for preparing a polypeptide composition with anti-wrinkle effects includes the following steps:
[0012] S1. Start the heating cycle, add deionized water to the main reactor, and stir at 300 r / min to raise the temperature to 48-50℃. Add 1,3-butanediol, glycerol, panthenol, disodium EDTA, and sodium low molecular weight hyaluronic acid sequentially through the top feed port, and stir at a constant temperature for 15-20 min until the materials are completely dissolved. Start the buffer addition unit, monitor the pH in real time with the online pH probe, and add citric acid / sodium citrate buffer solution to adjust the pH of the system to 5.2-6.2. After maintaining the temperature and stabilizing for 10 min, turn off the heating circuit, turn on the cooling circulation system, and quickly cool the materials in the reactor to below 35℃. Keep the reactor at this temperature and let it stand for later use.
[0013] S2. Add 5% of the formulation of 1,3-butanediol to the peptide premixing tank, maintain the temperature of the refrigeration system at 25°C, and start the magnetic stirrer at 200 r / min. Sequentially add acetyl hexapeptide-8, palmitoyl tripeptide-1 / palmitoyl tetrapeptide-7 complex, dipeptide diaminobutyryl benzylamide diacetate, and finally add blue copper peptide GHK-Cu. Continue stirring for 20-25 min until the liquid is completely clear and free of precipitate to obtain the peptide premix. Start the delivery diaphragm pump and set the pipeline flow regulating valve to control the drip rate.
[0014] S3. Maintain the temperature inside the main reactor at 30–35°C, and adjust the stirring speed to 250 r / min. Add the peptide solution from the pre-dissolved peptide tank to the main reactor at a uniform rate through the dropper, with a total droppering time ≥8 min. After all drops are added, maintain the temperature and stir for 25–30 min to ensure uniform dispersion of the peptides. Add the p-hydroxyacetophenone + 1,2-hexanediol preservative mixture through the feed port and stir for 10 min to fully dissolve. Monitor the pH online and add a small amount of buffer solution to fine-tune the pH to 5.3–6.0.
[0015] S4. Continue to slowly cool down the cooling system at a rate of 5℃ / h, and stir at a low speed until the system temperature drops to 25℃. Maintain constant temperature for 30 minutes to eliminate internal stress. Open the discharge valve at the bottom of the main vessel. The material flows through the pre-precision filter and the 0.22μm polyethersulfone sterile filter membrane assembly under negative pressure to remove impurities and microorganisms.
[0016] S5. Finally, hydrolyzed collagen, ginseng protein, and Dendrobium officinale protein are fed into an enzymatic hydrolysis tank for alkaline enzymatic hydrolysis. The ultrafiltration equipment retains peptides with a molecular weight <1000Da and desaltes them. The spray drying unit produces plant polypeptide powder, reducing the original synthetic polypeptide feed amount by 50%. The plant polypeptide powder and synthetic polypeptide powder are fed together into a polypeptide pre-dissolving tank for simultaneous butylene glycol pre-dissolving. After filtration, the material is directly filled into a light-proof brown sterile container through a sterile filling interface and stored in a sealed, light-proof container.
[0017] Compared with the prior art, the beneficial effects of the present invention are:
[0018] An improved design employs a multi-tank independent temperature control system to separate the high-temperature matrix preparation and peptide feeding. PLC over-temperature interlock protection prevents peptide degradation and inactivation at high temperatures. A separate pre-dissolving tank ensures complete pre-dissolution of peptides, preventing aggregation and precipitation upon direct water introduction. An online real-time pH-linked buffer metering pump maintains stable peptide activity within a suitable pH range throughout the process. Furthermore, a lipid homogenization system enables peptide liposome encapsulation, enhancing transdermal absorption and the antioxidant stability of copper peptides. A 0.22μm sterile filtration unit at the end eliminates the need for high-temperature sterilization, ensuring peptide activity at low temperatures throughout the process. The finished product carries no risk of preservative irritation. Attached Figure Description
[0019] Figure 1 This diagram illustrates the core anti-wrinkle polypeptide components in the preparation method of an anti-wrinkle polypeptide composition according to the present invention.
[0020] Figure 2 This is a diagram illustrating the moisturizing and stabilizing excipients in the preparation method of a polypeptide composition with anti-wrinkle effects according to the present invention.
[0021] Figure 3 This is a flowchart of the complete standard preparation process of a polypeptide composition with anti-wrinkle effect according to the present invention;
[0022] Figure 4 This is a flowchart of the natural plant compound polypeptide process for preparing a polypeptide composition with anti-wrinkle effect according to the present invention. Detailed Implementation
[0023] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0024] Please see Figures 1-4 This invention provides a technical solution for preparing a polypeptide composition with anti-wrinkle effects:
[0025] A method for preparing a polypeptide composition with anti-wrinkle effects includes a core anti-wrinkle polypeptide component, moisturizing and stabilizing excipients, a complete standard preparation process, and a natural plant compound polypeptide process.
[0026] The core anti-wrinkle polypeptide components include acetyl hexapeptide-8: 0.1%–0.5%, palmitoyl tripeptide 1 + tetrapeptide 7: 0.08%–0.3%, blue copper peptide GHK-Cu: 0.02%–0.15%, and snake venom-like peptide: 0.05%–0.2%.
[0027] The moisturizing and stabilizing excipients include polyols, active ingredients, stabilizers, mild preservatives, and solvents.
[0028] The complete standard preparation process includes aqueous matrix preparation, separate pre-dissolution of peptides, low-temperature compounding and mixing, pH adjustment, maturation, and filtration.
[0029] The natural plant compound polypeptide process includes plant peptide preparation, formula optimization, and feeding operations.
[0030] A method for preparing a polypeptide composition with anti-wrinkle effects includes the following steps:
[0031] S1. Start the heating cycle, add deionized water to the main reactor, and stir at 300 r / min to raise the temperature to 48-50℃. Add 1,3-butanediol, glycerol, panthenol, disodium EDTA, and sodium low molecular weight hyaluronic acid sequentially through the top feed port, and stir at a constant temperature for 15-20 min until the materials are completely dissolved. Start the buffer addition unit, monitor the pH in real time with the online pH probe, and add citric acid / sodium citrate buffer solution to adjust the pH of the system to 5.2-6.2. After maintaining the temperature and stabilizing for 10 min, turn off the heating circuit, turn on the cooling circulation system, and quickly cool the materials in the reactor to below 35℃. Keep the reactor at this temperature and let it stand for later use.
[0032] S2. Add 5% of the formulation of 1,3-butanediol to the peptide premixing tank, maintain the temperature of the refrigeration system at 25°C, and start the magnetic stirrer at 200 r / min. Sequentially add acetyl hexapeptide-8, palmitoyl tripeptide-1 / palmitoyl tetrapeptide-7 complex, dipeptide diaminobutyryl benzylamide diacetate, and finally add blue copper peptide GHK-Cu. Continue stirring for 20-25 min until the liquid is completely clear and free of precipitate to obtain the peptide premix. Start the delivery diaphragm pump and set the pipeline flow regulating valve to control the drip rate.
[0033] S3. Maintain the temperature inside the main reactor at 30–35°C, and adjust the stirring speed to 250 r / min. Add the peptide solution from the pre-dissolved peptide tank to the main reactor at a uniform rate through the dropper, with a total droppering time ≥8 min. After all drops are added, maintain the temperature and stir for 25–30 min to ensure uniform dispersion of the peptides. Add the p-hydroxyacetophenone + 1,2-hexanediol preservative mixture through the feed port and stir for 10 min to fully dissolve. Monitor the pH online and add a small amount of buffer solution to fine-tune the pH to 5.3–6.0.
[0034] S4. Continue to slowly cool down the cooling system at a rate of 5℃ / h, and stir at a low speed until the system temperature drops to 25℃. Maintain constant temperature for 30 minutes to eliminate internal stress. Open the discharge valve at the bottom of the main vessel. The material flows through the pre-precision filter and the 0.22μm polyethersulfone sterile filter membrane assembly under negative pressure to remove impurities and microorganisms.
[0035] S5. Finally, hydrolyzed collagen, ginseng protein, and Dendrobium officinale protein are fed into an enzymatic hydrolysis tank for alkaline enzymatic hydrolysis. The ultrafiltration equipment retains peptides with a molecular weight <1000Da and desaltes them. The spray drying unit produces plant polypeptide powder, reducing the original synthetic polypeptide feed amount by 50%. The plant polypeptide powder and synthetic polypeptide powder are fed together into a polypeptide pre-dissolving tank for simultaneous butylene glycol pre-dissolving. After filtration, the material is directly filled into a light-proof brown sterile container through a sterile filling interface and stored in a sealed, light-proof container.
[0036] It should be noted that this invention relates to a method for preparing a polypeptide composition with anti-wrinkle effects. First, the heating cycle is activated, and deionized water is added to the main reactor. The stirring speed is 300 rpm, and the temperature is raised to 48–50°C. Then, 1,3-butanediol, glycerol, panthenol, disodium EDTA, and low-molecular-weight sodium hyaluronate are added sequentially through the top feed port. The mixture is stirred at a constant temperature for 15–20 minutes until the materials are completely dissolved. Next, the buffer addition unit is activated, and the pH is monitored in real-time by an online pH probe. Citric acid / sodium citrate buffer solution is added dropwise to adjust the pH of the system to 5.2–6.2. After maintaining the temperature and stabilizing for 10 minutes, the heating circuit is turned off, and the cooling circulation system is activated. Rapidly cool the material in the reactor to below 35°C, keep it at that temperature and let it stand for later use. Add 5% of the formulated 1,3-butanediol to the peptide pre-dissolving tank, maintain the temperature of the refrigeration system at 25°C, and start the magnetic stirrer at 200 rpm. Sequentially add acetyl hexapeptide-8, palmitoyl tripeptide-1 / palmitoyl tetrapeptide-7 complex, dipeptide diaminobutyryl benzylamide diacetate, and finally add blue copper peptide GHK-Cu. Continue stirring for 20-25 minutes until the liquid is completely clear and free of precipitate to obtain the peptide premix. Start the delivery diaphragm pump, set the pipeline flow regulating valve to control the drip rate, maintain the temperature in the main reactor at 30-35°C, and lower the stirrer to... 250 r / min; The peptide solution in the pre-dissolving tank is uniformly dripped into the main vessel through the dripping pipeline, with a total dripping time ≥8 min; after all dripping is completed, the mixture is stirred at a constant temperature for 25–30 min to ensure uniform dispersion of the peptides; p-hydroxyacetophenone + 1,2-hexanediol compound preservative is added through the feeding port and stirred for 10 min to fully dissolve; online pH monitoring is performed, and a small amount of buffer solution is added to finely adjust the pH to 5.3–6.0; then the cooling system is continuously and slowly cooled down at a rate of 5℃ / h, with stirring at a low speed until the system temperature drops to 25℃; the system is then aged at a constant temperature for 30 min to eliminate internal dispersion stress; finally, the discharge valve at the bottom of the main vessel is opened, and the material is discharged according to… The material is first filtered through a pre-precision filter and then through a 0.22μm polyethersulfone sterile filter membrane assembly under negative pressure to remove impurities and microorganisms. Finally, hydrolyzed collagen, ginseng protein, and Dendrobium officinale protein are sent to an enzymatic hydrolysis tank for alkaline enzymatic hydrolysis. Ultrafiltration equipment retains peptides with a molecular weight <1000Da and desalts them. The spray dryer produces plant polypeptide powder, reducing the amount of synthetic polypeptide feed by 50%. The plant polypeptide powder and synthetic polypeptide powder are then fed together into a polypeptide pre-dissolving tank for simultaneous butylene glycol pre-dissolution. After filtration, the material is directly filled into a light-proof brown sterile container through a sterile filling interface and stored in a sealed, light-proof container. This completes the preparation method of a polypeptide composition with anti-wrinkle effects.
[0037] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a polypeptide composition with anti-wrinkle effects, characterized in that: It includes core anti-wrinkle peptide components, moisturizing and stabilizing excipients, a complete standard preparation process, and a natural plant compound peptide process.
2. The method for preparing a polypeptide composition with anti-wrinkle effect according to claim 1, characterized in that: The core anti-wrinkle polypeptide components include acetyl hexapeptide-8: 0.1%–0.5%, palmitoyl tripeptide 1 + tetrapeptide 7: 0.08%–0.3%, blue copper peptide GHK-Cu: 0.02%–0.15%, and snake venom-like peptide: 0.05%–0.2%.
3. The method for preparing a polypeptide composition with anti-wrinkle effect according to claim 1, characterized in that: The moisturizing and stabilizing excipients include polyols, active ingredients, stabilizers, mild preservatives, and solvents.
4. The method for preparing a polypeptide composition with anti-wrinkle effect according to claim 1, characterized in that: The complete standard preparation process includes aqueous matrix preparation, separate pre-dissolution of peptides, low-temperature compounding and mixing, pH adjustment, maturation, and filtration.
5. The method for preparing a polypeptide composition with anti-wrinkle effect according to claim 1, characterized in that: The natural plant compound polypeptide process includes plant peptide preparation, formula optimization, and feeding operations.
6. A method for preparing a polypeptide composition with anti-wrinkle effects, characterized in that: Includes the following steps: S1. Start the heating cycle, add deionized water to the main reactor, and stir at 300 r / min to raise the temperature to 48-50℃. Add 1,3-butanediol, glycerol, panthenol, disodium EDTA, and sodium low molecular weight hyaluronic acid sequentially through the top feed port, and stir at a constant temperature for 15-20 min until the materials are completely dissolved. Start the buffer addition unit, monitor the pH in real time with the online pH probe, and add citric acid / sodium citrate buffer solution to adjust the pH of the system to 5.2-6.
2. After maintaining the temperature and stabilizing for 10 min, turn off the heating circuit, turn on the cooling circulation system, and quickly cool the materials in the reactor to below 35℃. Keep the reactor at this temperature and let it stand for later use. S2. Add 5% of the formulation of 1,3-butanediol to the peptide premixing tank, maintain the temperature of the refrigeration system at 25°C, and start the magnetic stirrer at 200 r / min. Sequentially add acetyl hexapeptide-8, palmitoyl tripeptide-1 / palmitoyl tetrapeptide-7 complex, dipeptide diaminobutyryl benzylamide diacetate, and finally add blue copper peptide GHK-Cu. Continue stirring for 20-25 min until the liquid is completely clear and free of precipitate to obtain the peptide premix. Start the delivery diaphragm pump and set the pipeline flow regulating valve to control the drip rate. S3. Maintain the temperature inside the main reactor at 30-35℃ and adjust the stirring speed to 250r / min. Drop the peptide solution from the peptide pre-dissolving tank into the main reactor at a uniform rate through the dropping pipeline, with a total dropping time of ≥8min. After all the dropping is completed, stir at a constant temperature for 25-30min to ensure uniform dispersion of the peptide. Add p-hydroxyacetophenone + 1,2-hexanediol compound preservative through the feeding port and stir for 10 minutes to dissolve completely; monitor pH online and add a small amount of buffer solution to fine-tune the pH to 5.3-6.0; S4. Continue to slowly cool down the cooling system at a rate of 5℃ / h, and stir at a low speed until the system temperature drops to 25℃. Maintain constant temperature for 30 minutes to eliminate internal stress. Open the discharge valve at the bottom of the main vessel. The material flows through the pre-precision filter and the 0.22μm polyethersulfone sterile filter membrane assembly under negative pressure to remove impurities and microorganisms. S5. Finally, hydrolyzed collagen, ginseng protein, and Dendrobium officinale protein are fed into an enzymatic hydrolysis tank for alkaline enzymatic hydrolysis. The ultrafiltration equipment retains peptides with a molecular weight <1000Da and desaltes them. The spray drying unit produces plant polypeptide powder, reducing the original synthetic polypeptide feed amount by 50%. The plant polypeptide powder and synthetic polypeptide powder are fed together into a polypeptide pre-dissolving tank for simultaneous butylene glycol pre-dissolving. After filtration, the material is directly filled into a light-proof brown sterile container through a sterile filling interface and stored in a sealed, light-proof container.