Preparation method of lipstick containing polypeptide and super A alcohol for fading lip wrinkles through deep maintenance

Abstract

This invention discloses a method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines, relating to the field of lipstick preparation technology. The method includes: S1, Raw material preparation: Recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol are weighed in a mass ratio of 1:1:0.8:0.5 as the core active ingredients. Simultaneously, a composite oil phase, an aqueous matrix, and auxiliary ingredients are prepared. The total mass of the core active ingredients accounts for 5%-8% of the total mass of the lipstick, the mass ratio of the composite oil phase to the aqueous matrix is ​​3:2, and the total mass of the auxiliary ingredients accounts for 0.3%-0.5% of the total mass of the lipstick. This invention designs a targeted composite system of recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol targeting the lip basement membrane. This synergistically activates the expression of COL7A1 and COL17A1 genes, strengthens the structural stability of the basement membrane, and achieves a triple wrinkle-reducing logic of basement membrane repair, collagen regeneration, and keratin metabolism, solving the problems of existing formulas lacking targeting and having limited wrinkle-reducing effects.

Description

Technical Field

[0001] This invention relates to the field of lipstick preparation technology, specifically a method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines. Background Technology

[0002] Lipstick is a core product in the lip care field. Based on natural oils and waxes, it forms a protective film on the lips, providing basic functions such as moisturizing, soothing, and protecting against external environmental irritants. It effectively alleviates problems such as dryness, peeling, and roughness of the lips, making it an indispensable category in daily beauty and skincare. It plays an important role in maintaining the health and beauty of the lips. Lip lines are lines of varying depths formed on the lips due to factors such as physiological aging, environmental irritation, and improper care, caused by the loss of collagen fibers, damage to the basement membrane structure, and abnormal metabolism of the stratum corneum. These lines not only seriously affect the appearance of the lips but also exacerbate moisture loss, leading to dryness, cracking, decreased elasticity, and reduced skin firmness. Lipsticks that reduce lip lines retain basic care functions while adding deep nourishment and line improvement effects. They can specifically address the core problems of lip line formation, meeting consumers' advanced needs for refined lip care, significantly enhancing the product's market competitiveness, and possessing significant practical value and market prospects.

[0003] However, existing technologies for lipsticks that reduce lip lines still have certain shortcomings. Most products only generalize the combination of peptides and retinol active ingredients without fully considering the thin basement membrane and special barrier function of the lips. They lack targeted design, making it difficult for active ingredients to accurately target the core points of lip line formation, resulting in limited and slow-acting effects. Traditional manufacturing processes often use high-temperature melting and mixing, which not only easily causes the inactivation of active ingredients such as peptides and retinol, but also fails to solve the compatibility problem between water-soluble peptides and fat-soluble retinol, leading to uneven dispersion and easy aggregation of ingredients. This reduces the transdermal penetration rate of active ingredients and affects the stability of the product system, ultimately failing to meet consumers' demand for highly effective, gentle, and stable lipsticks that reduce lip lines. Therefore, developing a method for preparing a lipstick containing peptides and super retinol for deep nourishment and reduction of lip lines is of great significance. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of existing technologies and provide a method for preparing a lipstick containing peptides and retinol for deep nourishment and reduction of lip lines. This method utilizes a targeted complex system of recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol to synergistically activate the expression of COL7A1 and COL17A1 genes, enhance the structural stability of the basement membrane, and achieve a triple logic of basement membrane repair, collagen regeneration, and keratin metabolism to reduce lip lines. Combined with an ultrasonic biphasic dispersion-emulsification process at a low temperature of 45°C, this method avoids the inactivation of active ingredients caused by high temperatures, improves the uniformity of ingredient dispersion, and significantly increases the transdermal absorption rate of active ingredients.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines, the method comprising the following steps: S1. Raw material preparation: Weigh recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol as core active ingredients in a mass ratio of 1:1:0.8:0.5. At the same time, prepare a complex oil phase, an aqueous matrix, and auxiliary ingredients. The total mass of the core active ingredients accounts for 5%-8% of the total mass of the lipstick. The mass ratio of the complex oil phase to the aqueous matrix is ​​3:2. The total mass of the auxiliary ingredients accounts for 0.3%-0.5% of the total mass of the lipstick. S2. Preparation of active oil phase: Add super A alcohol to the composite oil phase, place it in a 45℃ constant temperature reactor, turn on a 300W ultrasonic device for 15min, and continuously stir during the process to control the dispersed particle size ≤100nm to obtain the active oil phase. S3. Preparation of active aqueous phase: Recombinant type XVII collagen, palmitoyl tripeptide-5, and acetyl tetrapeptide-9 were added to the aqueous matrix in sequence and stirred at 35°C until the system was homogeneous and transparent. Then, the mixture was passed through a high-pressure homogenizer and homogenized at 80 MPa to obtain the active aqueous phase. S4. Ultrasonic emulsification and fusion: The active oil phase is slowly injected into the active aqueous phase, the system temperature is maintained at 45℃, and the system is treated with an ultrasonic emulsification device at a frequency of 20kHz for 20 minutes to form a stable emulsion system. S5. Molding process: Add auxiliary ingredients to the emulsified mixture and continue stirring for 10 minutes until the system is homogeneous. Then pour it into the lipstick mold and allow it to cool and solidify naturally at room temperature of 25°C for 30 minutes. Demolding will then yield the target lipstick.

[0006] Further, in step S1, the composite oil phase is composed of meadowfoam seed oil and squalane in a mass ratio of 2:1, and the meadowfoam seed oil has an acid value ≤0.5mgKOH / g, an iodine value of 110-120gI2 / 100g, and a squalane purity ≥99%. The aqueous matrix is ​​composed of deionized water and glycerol in a mass ratio of 5:1, wherein the conductivity of deionized water is ≤10μS / cm, and the glycerol purity is ≥99.5%. The auxiliary components include propylparaben and natural fragrance in a mass ratio of 2:1, and the propylparaben purity is ≥99%.

[0007] Furthermore, step S2, in preparing the active oil phase, includes the following steps: First, add the composite oil phase into the constant temperature reactor, turn on the heating device to raise the system temperature to 45℃ and keep it at that temperature for 10 minutes to ensure that the temperature is uniform and stable. Slowly add the weighed super A alcohol to the composite oil phase, turn on the stirring device, control the stirring speed to 300 r / min, and stir for 5 min to allow the super A alcohol to be initially dispersed. Turn on the 300W ultrasonic device, keep the stirring rate constant during the ultrasonic treatment, take a sample every 5 minutes, and detect the dispersed particle size using a laser particle size analyzer. When the particle size is detected to be ≤100nm and the deviation between two consecutive sampling results is ≤5%, the ultrasonic equipment and stirring device are turned off to obtain the active oil phase.

[0008] Furthermore, step S3 includes the following steps in preparing the active aqueous phase: Add the aqueous matrix to the mixing tank, turn on the heating device to raise the system temperature to 35°C, and keep it at that temperature for 5 minutes; Add recombinant type XVII collagen, palmitoyl tripeptide-5, and acetyl tetrapeptide-9 to the aqueous matrix in that order. After each addition of one component, stir at a stirring rate of 250 r / min for 8 min until the component is completely dissolved before adding the next component. Once all the core active ingredients have dissolved and the system is homogeneous and transparent, the mixture is passed into a high-pressure homogenizer and homogenized three times continuously at a pressure of 80 MPa, with each homogenization lasting 2 minutes and an interval of 3 minutes between adjacent homogenizations. After homogenization, the active aqueous phase is obtained.

[0009] Furthermore, in step S4, the rate at which the active oil phase is injected into the active aqueous phase is 5 mL / min, and a stirring rate of 250 r / min is maintained during the injection process to ensure that the active oil phase is uniformly dispersed in the active aqueous phase. During ultrasonic emulsification, the probe of the ultrasonic device is inserted into the system to a depth of 2-3 cm below the liquid surface, and the distance between the probe and the container wall is ≥5 cm. The probe position is adjusted every 4 minutes during the ultrasonic process, with each adjustment increment being 1 cm, to ensure that the two phases are fully fused.

[0010] Furthermore, the purity of the core active ingredients in step S1 is ≥98%, wherein the molecular weight of recombinant type XVII collagen is 150-200kDa, the molecular weight of palmitoyl tripeptide-5 is 497.6Da, the molecular weight of acetyl tetrapeptide-9 is 411.5Da, and the molecular weight of retinol is 328.5Da.

[0011] Furthermore, the lipstick mold used in step S5 is made of food-grade aluminum alloy. The inner wall of the mold is polished and the surface roughness Ra≤0.8μm. Before injecting the mixture, the mold is sterilized at 120℃ for 20min and then cooled to 25℃ for later use. During the cooling and curing process, the relative humidity of the environment is controlled at 40%-60%, and direct sunlight and airflow directly blowing on the mold are avoided.

[0012] Furthermore, in step S2, the ultrasonic frequency of the ultrasonic device is 20kHz, and the ultrasonic mode is intermittent ultrasonic, that is, working for 3 seconds, pausing for 1 second, and continuing for 15 minutes. In step S4, the ultrasonic emulsification device uses continuous ultrasonic mode, and the system temperature is monitored in real time during the ultrasonic process. When the temperature exceeds 45°C, the cooling device is activated to bring the temperature back to 45°C before continuing the ultrasonic treatment.

[0013] Furthermore, in step S3, the feed rate of the high-pressure homogenizer is controlled at 10-15 L / h, and the system temperature is maintained at 35±2℃ during homogenization to avoid temperature fluctuations affecting the stability of the core active ingredients. After homogenization, the active aqueous phase is filtered through a polyethersulfone filter membrane with a pore size of 0.22 μm. During filtration, the filtration pressure is maintained at 0.1-0.15 MPa, and the filtration rate is uniform and stable to remove any trace impurities and incompletely dispersed microparticles that may exist in the system, ensuring the uniformity and cleanliness of the active aqueous phase.

[0014] Furthermore, in step S1, the core active ingredient is placed in a sealed, light-proof container before storage and use. The storage environment temperature is controlled at 2-8℃, the relative humidity is ≤60%, and the storage time does not exceed 6 months. Before use, the core active ingredient is placed in a constant temperature environment of 35℃ for 12 hours to warm up. The ingredient temperature is added only after it is consistent with the temperature of the subsequent preparation system. This avoids insufficient dissolution of the ingredient or local temperature difference in the system due to temperature differences, which would affect the stability and uniformity of the final product.

[0015] Compared with existing technologies, this method for preparing a lipstick containing peptides and retinol for deep nourishment and reducing lip lines has the following beneficial effects: This invention designs a targeted complex system of recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol targeting the lip basement membrane. This system synergistically activates the expression of COL7A1 and COL17A1 genes, strengthens the structural stability of the basement membrane, and achieves a triple wrinkle-reducing logic of basement membrane repair, collagen regeneration, and keratin metabolism. This solves the problems of existing formulas lacking targeting and having limited wrinkle-reducing effects. Combined with an ultrasonic biphasic dispersion-emulsification process at a low temperature of 45°C, it avoids the inactivation of active ingredients caused by high temperatures and improves the uniformity of ingredient dispersion, significantly increasing the transdermal absorption rate of active ingredients. This solves the problems of poor compatibility and low ingredient penetration in existing processes, ultimately resulting in a highly effective, gentle, safe, and stable deep-care lip balm that reduces wrinkles.

[0016] Other advantages, objectives and features of the invention will be set forth in part in the description which follows, and in part will be apparent to those skilled in the art from the following examination or study, or may be learned from the practice of the invention. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the accompanying drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are merely some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without any creative effort.

[0018] Figure 1 A flowchart of a method for preparing a lipstick containing polypeptides and retinol to deeply nourish and reduce lip lines; Figure 2 A flowchart illustrating a method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines. Detailed Implementation

[0019] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features and effects of the present invention, in conjunction with the accompanying drawings and preferred embodiments, is provided below.

[0020] This invention addresses the problems of existing lipsticks for reducing lip lines, such as lack of targeting, limited effect, and easy deactivation of active ingredients. It provides a complete lipstick preparation technology solution, the core of which lies in the combination of a targeted complex active system and low-temperature ultrasonic processing, achieving highly effective line reduction and stable skin care. (See also...) Figure 1 and Figure 2 The specific details are as follows: The core of the technical solution comprises two main parts: raw material formulation and preparation process. Regarding raw materials, the core active ingredients are recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol, in a mass ratio of 1:1:0.8:0.5, accounting for 5%-8% of the lipstick's total mass. These ingredients synergistically activate the expression of COL7A1 and COL17A1 genes, forming a triple wrinkle-reducing logic of basement membrane repair, collagen regeneration, and keratin metabolism. The composite oil phase consists of meadowfoam seed oil and squalane in a 2:1 ratio, with the meadowfoam seed oil having an acid value ≤0.5mgKOH / g and the squalane purity ≥99%. The aqueous matrix is ​​deionized water and glycerin in a 5:1 ratio, with the deionized water having a conductivity ≤10μS / cm and the glycerin purity ≥99.5%, in a mass ratio of 3:2. The auxiliary ingredients are a 2:1 mixture of propylparaben and natural fragrance, accounting for 0.3%-0.5% of the total. The purity of the core active ingredients is ≥98%, and each ingredient has clear physicochemical index requirements.

[0021] The preparation process consists of five steps: First, raw material preparation: weigh each component according to the proportion. The core active ingredient needs to be sealed and stored in a light-proof environment at 2-8℃. Before use, it should be warmed to 35℃ for 12 hours. Second, preparation of the active oil phase: add super retinol to the composite oil phase at a constant temperature of 45℃, stir at 300r / min and intermittently sonicate at 300W for 15min, and control the particle size to ≤100nm. Third, preparation of the active aqueous phase: dissolve the polypeptide components sequentially at 35℃, stir at 250r / min until homogeneous and transparent, and then homogenize three times under high pressure at 80MPa. Fourth, ultrasonic emulsification and fusion: inject the active oil phase into the aqueous phase at a rate of 5mL / min, stir at 250r / min and continuously sonicate at 45℃ and 20kHz for 20min, with the probe depth at 2-3cm and adjusted periodically. Fifth, molding treatment: add auxiliary components and stir for 10min, pour into a food-grade aluminum alloy mold sterilized at 120℃, cool and solidify at 25℃ and 40%-60% humidity for 30min, and then demold.

[0022] This solution precisely targets the formation points of lip lines through a combination of targeted ingredients. The low-temperature ultrasonic process avoids the deactivation of active ingredients and solves the compatibility problem between water-soluble and fat-soluble ingredients, improving the uniformity of ingredient dispersion and transdermal absorption rate. The final product has the advantages of high efficiency in reducing lip lines, gentle safety and system stability, meeting the needs of refined lip care.

[0023] Example 1 This embodiment uses a standard formula with a total mass ratio of 5% for the core active ingredients. The core active ingredients are compounded in a targeted ratio of recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol in a 1:1:0.8:0.5 ratio. It strictly follows the low-temperature ultrasonic-high-pressure homogenization integrated process described in this invention, combined with a complex oil phase composed of meadowfoam seed oil and squalane, an aqueous matrix composed of deionized water and glycerin, and natural auxiliary ingredients. It focuses on gentle, deep nourishment and basic wrinkle reduction needs, achieving lip basement membrane repair and initial collagen regeneration while ensuring high product stability and safety. See [link to relevant documentation]. Figure 1 and Figure 2 The specific content of this embodiment is as follows: Raw material preparation: The core active ingredients, namely recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol, were precisely weighed in a mass ratio of 1:1:0.8:0.5. The recombinant type XVII collagen had a molecular weight of 180 kDa and a purity of 98.5%, the palmitoyl tripeptide-5 had a molecular weight of 497.6 Da and a purity of 99%, the acetyl tetrapeptide-9 had a molecular weight of 411.5 Da and a purity of 98.8%, and the retinol had a molecular weight of 328.5 Da and a purity of 99.2%. The total mass of the four core active ingredients accounted for 5% of the total mass of the lipstick. The complex oil phase was composed of meadowfoam seed oil and squalane mixed in a mass ratio of 2:1. The meadowfoam seed oil had an acid value of 0.4 mg KOH / g and an iodine value of 115 g I2 / 100g, and the squalane had a purity of 99.3%. The aqueous matrix is ​​prepared by mixing deionized water and glycerin in a 5:1 mass ratio. The deionized water has a conductivity of 8 μS / cm, and the glycerin has a purity of 99.6%. The mass ratio of the composite oil phase to the aqueous matrix is ​​strictly controlled at 3:2. The auxiliary ingredient is a combination of propylparaben and natural fragrance in a 2:1 mass ratio. The propylparaben has a purity of 99.2%, and the total mass of the auxiliary ingredients accounts for 0.3% of the total mass of the lipstick. The core active ingredient is stored in a sealed, light-protected environment at 2 to 8°C for 4 months. Before use, it should be placed in a constant temperature environment at 35°C for 12 hours to ensure that the temperature of the ingredient is consistent with the temperature of the subsequent preparation system.

[0024] Preparation of the active oil phase: First, the composite oil phase was added to a constant-temperature reactor, and the heating device was turned on to raise the system temperature to 45℃. This temperature was maintained for 10 minutes to ensure uniform and stable system temperature. Then, the weighed super-retinol was slowly added, and the stirring device was turned on. The stirring speed was controlled at 300 r / min, and stirring was continued for 5 minutes to initially disperse the super-retinol in the composite oil phase. Next, an ultrasonic device with a power of 300W and a frequency of 20kHz was turned on, using an intermittent ultrasonic method (working for 3 seconds, pausing for 1 second), while maintaining a constant stirring speed throughout the ultrasonic treatment. Samples were taken every 5 minutes, and the dispersed particle size was detected using a laser particle size analyzer. Detection was stopped when the detected particle size was ≤100nm and the deviation between two consecutive sampling results was ≤5%. The final measured particle size was 92nm. The ultrasonic device and stirring device were then turned off, yielding a homogeneous and stable active oil phase.

[0025] Preparation of the active aqueous phase: The aqueous matrix was added to a stirred tank, and the heating device was turned on to raise the temperature to 35°C and maintain the temperature for 5 minutes to ensure stability. Recombinant type XVII collagen, palmitoyl tripeptide-5, and acetyl tetrapeptide-9 were added to the aqueous matrix in the following order: after each addition, stirring was maintained at 250 rpm for 8 minutes until the component was completely dissolved before adding the next component. Once all core active ingredients were dissolved and the system was homogeneous and transparent, the mixture was passed through a high-pressure homogenizer at a feed rate of 12 L / h. Homogenization was performed three times at 80 MPa, with each homogenization lasting 2 minutes and a 3-minute interval between homogenizations. After homogenization, the mixture was filtered through a 0.22 μm polyethersulfone membrane at a pressure of 0.12 MPa to ensure a uniform and stable filtration rate, removing any trace impurities and incompletely dispersed particles to obtain a clean and homogeneous active aqueous phase.

[0026] Ultrasonic emulsification and fusion: The prepared active oil phase is slowly injected into the active aqueous phase at a rate of 5 mL / min, while maintaining a stirring rate of 250 r / min during the injection process to ensure uniform dispersion of the active oil phase in the active aqueous phase. The system temperature is maintained at 45℃, and continuous ultrasonic treatment is performed using an ultrasonic emulsification device with a frequency of 20 kHz for 20 minutes. During ultrasonic treatment, the probe of the ultrasonic device is inserted 2.5 cm below the liquid surface, and the distance between the probe and the container wall is ≥5 cm. The probe position is adjusted every 4 minutes, with each adjustment increment of 1 cm, to ensure thorough fusion of the oil and water phases and the formation of a stable emulsion system. The system temperature is monitored in real time during ultrasonic treatment. If the temperature exceeds 45℃, the cooling device is immediately activated to bring the temperature back to 45℃ before continuing ultrasonic treatment.

[0027] Molding Process: Add the prepared auxiliary ingredients to the emulsified mixture and continue stirring for 10 minutes until the mixture is homogeneous and free of granules. Then, pour the mixture into a lipstick mold made of food-grade aluminum alloy with a polished inner wall and a surface roughness Ra of 0.6μm. Before pouring the mixture, the mold was sterilized at 120℃ for 20 minutes and then cooled to 25℃. The cooling and curing process was carried out in an environment with a relative humidity of 50%, avoiding direct sunlight and direct airflow onto the mold. After natural cooling and curing for 30 minutes, the lipstick was demolded to obtain the desired product.

[0028] In summary, this embodiment strictly adheres to the formula ratios and process parameters defined in this invention. The proportion of core active ingredients is moderate, the low-temperature process effectively preserves the bioactivity of all active ingredients, and the combination of ultrasound and high-pressure homogenization ensures uniform dispersion of the ingredients. The product has a uniform and delicate appearance, and causes no irritation to the lips after application, demonstrating excellent gentleness. After 28 days of continuous use by 100 testers, feedback showed significant improvement in shallow lip lines, a reduction in deep lip lines, effective relief from dry and peeling lips, and a noticeable improvement in lip skin elasticity. The transdermal absorption rate of active ingredients reached a good level, and the product showed no delamination, discoloration, or other instability after 3 months of storage. It is suitable for daily basic wrinkle care for all skin types, and is especially suitable for consumers with sensitive skin.

[0029] Example 2 This embodiment employs an optimized formula with a total mass ratio of 6.5% for the core active ingredients. The core active ingredients maintain a targeted compounding ratio of 1:1:0.8:0.5, and the process parameters strictly adhere to the requirements of this invention. By appropriately increasing the concentration of active ingredients, the activation effect of the targeted compound system on the COL7A1 and COL17A1 genes is enhanced. Without compromising the product's gentleness, this achieves an optimal balance between wrinkle-reducing efficacy and system stability, meeting consumers' dual needs for highly effective wrinkle reduction and a comfortable user experience. (See also...) Figure 1 and Figure 2 The specific content of this embodiment is as follows: Raw material preparation: The core active ingredients were weighed in a mass ratio of 1:1:0.8:0.5, namely recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol. The recombinant type XVII collagen had a molecular weight of 160 kDa and a purity of 99%, the palmitoyl tripeptide-5 had a molecular weight of 497.6 Da and a purity of 99.2%, the acetyl tetrapeptide-9 had a molecular weight of 411.5 Da and a purity of 99%, and the retinol had a molecular weight of 328.5 Da and a purity of 99.5%. The total mass of the four core active ingredients accounted for 6.5% of the total mass of the lipstick. The complex oil phase consisted of meadowfoam seed oil and squalane in a mass ratio of 2:1. The meadowfoam seed oil had an acid value of 0.3 mg KOH / g and an iodine value of 118 g I2 / 100g, and the squalane had a purity of 99.5%. The aqueous matrix is ​​prepared by mixing deionized water and glycerin in a 5:1 mass ratio. The deionized water has a conductivity of 5 μS / cm, and the glycerin has a purity of 99.8%. The mass ratio of the composite oil phase to the aqueous matrix is ​​3:2. The auxiliary ingredient is a mixture of propylparaben and natural fragrance in a 2:1 mass ratio. The propylparaben has a purity of 99.3%, and the total mass of the auxiliary ingredients accounts for 0.4% of the total mass of the lipstick. The core active ingredients are stored in a sealed, light-protected environment at 2 to 8°C in strict accordance with the requirements of this invention. Before use, they undergo a 12-hour constant temperature warming treatment at 35°C to ensure that the temperature of the ingredients is consistent with the temperature of the preparation system at the time of addition.

[0030] Preparation of the active oil phase: The composite oil phase was added to a constant-temperature reactor, and the heating device was turned on to raise the temperature to 45°C. The temperature was maintained for 10 minutes to ensure a uniform and stable system temperature. Weighed retinol was slowly added, and the stirring device was turned on, controlling the stirring rate at 300 r / min. Stirring was performed for 5 minutes to complete the initial dispersion of the retinol. Subsequently, a 300W, 20kHz ultrasonic device was turned on, using an intermittent ultrasonic mode with a 3-second operation followed by a 1-second pause, maintaining a constant stirring rate throughout the ultrasonic process. Samples were taken every 5 minutes, and the dispersed particle size was measured using a laser particle size analyzer. The final measured particle size was 85 nm. The deviation between two consecutive sampling results was ≤3%. The ultrasonic device and stirring device were then turned off, yielding a uniformly dispersed active oil phase.

[0031] Preparation of the active aqueous phase: The aqueous matrix was added to a stirred tank and heated to 35°C, then held at that temperature for 5 minutes. Recombinant type XVII collagen, palmitoyl tripeptide-5, and acetyl tetrapeptide-9 were added sequentially, one component at a time, followed by stirring at 250 rpm for 8 minutes until completely dissolved before adding the next component. Once all core active ingredients were dissolved and the system was homogeneous and transparent, the mixture was passed through a high-pressure homogenizer at a feed rate of 10 L / h, homogenized three times continuously at 80 MPa for 2 minutes each time, with a 3-minute interval between homogenizations. After homogenization, the mixture was filtered through a 0.22 μm polyethersulfone membrane at a pressure controlled at 0.1 MPa, ensuring a uniform and stable filtration rate. This process removed trace impurities and small particles, yielding a clean and homogeneous active aqueous phase.

[0032] Ultrasonic emulsification and fusion: The active oil phase is slowly injected into the active aqueous phase at a rate of 5 mL / min, while maintaining a stirring rate of 250 r / min during injection to ensure uniform dispersion of the active oil phase. The system temperature is maintained at 45℃, and continuous ultrasonic treatment is performed using an ultrasonic emulsification device at a frequency of 20 kHz for 20 minutes. During ultrasonication, the probe is inserted 2 cm below the liquid surface and at a distance of ≥5 cm from the container wall. The probe position is adjusted by 1 cm every 4 minutes to ensure thorough fusion of the oil and water phases. The temperature is monitored in real time during ultrasonication. If the temperature exceeds 45℃, a cooling device is activated to lower the temperature to 45℃ before continuing ultrasonication to ultimately form a stable emulsion system.

[0033] Molding Process: Add auxiliary ingredients to the emulsified mixture and stir continuously for 10 minutes until the mixture is homogeneous. Pour the mixture into a lipstick mold made of food-grade aluminum alloy with a surface roughness Ra≤0.8μm after polishing the inner wall. The mold is sterilized at 120℃ for 20 minutes and cooled to 25℃ before use. The cooling and curing process is carried out in an environment with a relative humidity of 45%, avoiding direct sunlight and direct airflow. After natural cooling and curing for 30 minutes, demold to obtain the target lipstick.

[0034] In summary, this embodiment, by optimizing the proportion of the core active ingredient to 6.5%, achieves a perfect balance between targeted wrinkle-reducing efficacy and product gentleness under the process conditions defined by this invention. The targeted complex system significantly enhances the activation effect of the COL7A1 and COL17A1 genes, and fully leverages the synergistic effect of the triple wrinkle-reducing logic of basement membrane repair, collagen regeneration, and keratin metabolism. The product has a delicate and smooth texture, leaving the lips moisturized and non-sticky after application, with no irritation. After 28 days of continuous use by 100 testers, 95% of the testers reported that shallow lip lines had essentially disappeared, deep lip lines were significantly reduced, and lip elasticity and firmness were greatly improved. The transdermal absorption rate of the active ingredients reached an excellent level, and the product remained stable after 6 months of storage, without any separation, discoloration, or odor. Its overall performance is optimal, making it suitable for most consumers with wrinkle-reducing needs, and it is an ideal implementation solution that balances high efficiency, gentleness, and stability.

[0035] Example 3 This embodiment employs a high-concentration formula with a total mass ratio of 8% for the core active ingredients, maintaining a targeted compounding ratio of 1:1:0.8:0.5. Other process parameters strictly adhere to the requirements of this invention, focusing on enhancing the wrinkle-reducing effect. It is designed for consumers with deep lip lines and an urgent need for wrinkle reduction. Simultaneously, it verifies the stability and safety of the high-concentration active ingredients under the low-temperature ultrasonic-high-pressure homogenization process of this invention, providing adaptable solutions for different needs. See [link to relevant documentation]. Figure 1 and Figure 2 The specific content of this embodiment is as follows: Raw material preparation: The core active ingredients were weighed in a mass ratio of 1:1:0.8:0.5, namely recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol. The recombinant type XVII collagen had a molecular weight of 190 kDa and a purity of 98.8%, the palmitoyl tripeptide-5 had a molecular weight of 497.6 Da and a purity of 99%, the acetyl tetrapeptide-9 had a molecular weight of 411.5 Da and a purity of 98.9%, and the retinol had a molecular weight of 328.5 Da and a purity of 99.3%. The total mass of the four core active ingredients accounted for 8% of the total mass of the lipstick. The complex oil phase was a mixture of meadowfoam seed oil and squalane in a mass ratio of 2:1. The meadowfoam seed oil had an acid value of 0.4 mg KOH / g and an iodine value of 112 g I2 / 100g, and the squalane had a purity of 99.2%. The aqueous matrix is ​​prepared by mixing deionized water and glycerin in a 5:1 mass ratio. The deionized water has a conductivity of 7 μS / cm, and the glycerin has a purity of 99.6%. The mass ratio of the composite oil phase to the aqueous matrix is ​​3:2. The auxiliary ingredient is a combination of propylparaben and natural fragrance in a 2:1 mass ratio. The propylparaben has a purity of 99.1%, and the total mass of the auxiliary ingredients accounts for 0.5% of the total mass of the lipstick. The core active ingredient should be stored in a sealed, light-protected environment at 2 to 8°C for no more than 6 months. Before use, it should be warmed to 35°C for 12 hours to ensure that the temperature of the ingredient is consistent with the temperature of the preparation system before being added to the lipstick.

[0036] Preparation of the active oil phase: The composite oil phase was added to a constant-temperature reactor and heated to 45℃, then held at that temperature for 10 minutes to ensure a uniform and stable system temperature. Weighed retinol was slowly added, and the stirring device was turned on, controlling the stirring rate at 300 r / min. The retinol was stirred for 5 minutes to allow for initial dispersion. A 300W, 20kHz ultrasonic device was turned on, using intermittent ultrasonic operation for 3 seconds followed by a 1-second pause, maintaining a constant stirring rate throughout the ultrasonic process. Particle size was sampled every 5 minutes, and the final measured particle size was 90 nm. The deviation between two consecutive sample measurements was ≤4%. The ultrasonic and stirring devices were then turned off, yielding the active oil phase.

[0037] Preparation of the active aqueous phase: The aqueous matrix was added to a stirred tank, heated to 35°C, and held for 5 minutes. Recombinant type XVII collagen, palmitoyl tripeptide-5, and acetyl tetrapeptide-9 were added sequentially, stirring at 250 rpm for 8 minutes after each addition until completely dissolved before adding the next. Once all core active ingredients were dissolved and the system was homogeneous and transparent, the mixture was passed through a high-pressure homogenizer at a feed rate of 15 L / h, homogenized three times continuously at 80 MPa for 2 minutes each time, with a 3-minute interval between each homogenization. After homogenization, the mixture was filtered through a 0.22 μm polyethersulfone membrane at a pressure of 0.15 MPa, ensuring a uniform and stable filtration rate. This removed trace impurities and incompletely dispersed small particles, resulting in a homogeneous and clean active aqueous phase.

[0038] Ultrasonic emulsification and fusion: The active oil phase is injected into the active aqueous phase at a rate of 5 mL / min, while maintaining a stirring rate of 250 r / min to ensure uniform dispersion. The system temperature is maintained at 45℃, and continuous ultrasonic treatment is performed using a 20 kHz ultrasonic emulsifier for 20 minutes. The probe is inserted 3 cm below the liquid surface and at a distance of ≥5 cm from the container wall. The probe position is adjusted by 1 cm every 4 minutes to ensure thorough fusion of the two phases. Temperature is monitored in real time during ultrasonication; if the temperature exceeds the limit, a cooling device is activated to lower the temperature to 45℃ before continuing treatment to form a stable emulsion system.

[0039] Molding process: Add auxiliary ingredients to the emulsion system and stir for 10 minutes until the system is homogeneous. Pour the mixture into a food-grade aluminum alloy mold that has been sterilized at 120°C for 20 minutes and cooled to 25°C. The surface roughness of the inner wall of the mold is Ra≤0.8μm. Cool and cure in a light-protected environment with a relative humidity of 55% for 30 minutes, avoiding direct sunlight and direct airflow. After demolding, the target lipstick is obtained.

[0040] In summary, this embodiment achieves the maximum permitted concentration of the core active ingredient (8%) as defined in this invention, resulting in the most prominent targeted wrinkle-reducing effect and significant improvement in deep lip lines. The low-temperature process described in this invention effectively inhibits the degradation of high-concentration retinol, while the ultrasonic and high-pressure homogenization processes ensure uniform dispersion of the high-concentration ingredient, resulting in good product system stability. After 28 days of continuous use by 100 testers, 98% reported that shallow lip lines completely disappeared, deep lip lines were significantly reduced, and the firmness and elasticity of the lip skin were greatly improved. However, due to the high concentration of retinol, 3% of testers experienced slight lip redness within the first 3 days of use, without other discomfort. The symptoms completely subsided after 1 day of discontinuation. People with sensitive skin should use with caution. The product achieves excellent transdermal absorption and showed no significant instability after 6 months of storage. It is suitable for consumers with deep lip lines and high requirements for wrinkle-reducing efficiency, providing a highly effective solution for severe wrinkle reduction needs.

[0041] Comparative Example This comparative example employs a traditional high-temperature melting process and generalized compound formulation found in existing technologies. The core active ingredients are compounded in a non-targeted 1:1:1:1 ratio. It does not utilize the low-temperature ultrasonic-high-pressure homogenization process of this invention, but instead uses traditional oil-based and aqueous matrices and synthetic auxiliary ingredients. This is intended to create a stark contrast with the embodiments of this invention, highlighting the significant advantages of this invention's technical solution in terms of wrinkle-reducing effect, ingredient stability, and gentleness. The technical solution is as follows: Raw material preparation: The core active ingredients were weighed according to a mass ratio of recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol in a 1:1:1:1 ratio, accounting for 4% of the total mass of the lipstick. The complex oil phase was composed of petrolatum and lanolin mixed in a 2:1 mass ratio, and the aqueous matrix was prepared by mixing deionized water and propylene glycol in a 5:1 mass ratio, with a total oil phase to aqueous matrix mass ratio of 3:2. The auxiliary ingredients were ethylparaben and synthetic fragrance combined in a 2:1 mass ratio, accounting for 0.6% of the total mass of the lipstick. All active ingredients were stored at room temperature without any special sealing or light protection measures, and were directly added without any warming treatment before use.

[0042] Preparation of the oil phase: The composite oil phase was added to the reactor, and the heating device was turned on to raise the temperature to 80°C to completely melt the oil phase. The weighed super-retinol was added, and the stirring rate was controlled at 500 r / min. The stirring was continued for 20 minutes. No ultrasonic treatment was performed; the components were mixed only by stirring. The final dispersed particle size was approximately 300 nm.

[0043] Aqueous phase preparation: The aqueous matrix was added to another reactor and heated to 80°C. The core active ingredient of the polypeptide was added and stirred at a stirring rate of 300 r / min to dissolve it. No high-pressure homogenization was performed. The aqueous phase was obtained by direct filtration through a filter membrane with a pore size of 0.45 μm to remove obvious impurities.

[0044] Emulsification and blending: The molten oil phase was rapidly poured into the aqueous phase, and the system temperature was maintained at 80°C. Emulsification was carried out by continuous stirring for 30 minutes without the use of ultrasonic emulsification equipment. After emulsification, the heating device was turned off, and the system was allowed to cool naturally to 50°C.

[0045] Molding process: Add auxiliary ingredients to the cooled mixture and stir for 10 minutes until the system is initially homogeneous. Then pour it into a regular plastic mold and allow it to cool and solidify naturally at room temperature for 60 minutes. Demold the mixture to obtain the comparison sample lipstick.

[0046] In summary, this comparative example, employing a traditional high-temperature melting process and a generalized compound formulation, suffers from multiple technical defects. The 80℃ high temperature resulted in a 25% degradation rate of retinol and approximately 30% loss of peptide activity, significantly reducing the utilization rate of active ingredients. The lack of ultrasonic and high-pressure homogenization processes led to poor compatibility between water-soluble peptides and lipid-soluble retinol, resulting in uneven dispersion and easy aggregation. The dispersed particle size far exceeded the requirements of this invention, leading to extremely low transdermal absorption of active ingredients. After 28 days of continuous use by 100 participants, only 10% reported slight improvement in lip lines, 90% reported no significant effect, and 5% experienced discomfort such as dry and peeling lips. After one month of storage, the product exhibited stratification, with oil precipitating on top and sediment forming at the bottom, indicating extremely poor system stability. Its overall performance was far inferior to the three embodiments of this invention, fully demonstrating the technical advantages of the targeted formulation and low-temperature ultrasonic-high-pressure homogenization process of this invention.

[0047]

[0048] The comparison in the table above clearly shows that the three embodiments of the present invention are significantly superior to the comparative example in all performance indicators. The core advantage stems from the synergistic effect of targeted formulation design and low-temperature ultrasonic-high-pressure homogenization process. Embodiment 2, with a core active ingredient ratio of 6.5%, a standard targeted compounding ratio, and a complete process, achieves optimal overall performance in terms of wrinkle-reducing effect, ingredient stability, transdermal absorption rate, gentleness, and product uniformity, making it the best overall implementation scheme. Embodiment 3, with a high concentration of active ingredients (8%), has the strongest wrinkle-reducing effect, but its gentleness is slightly reduced, making it suitable for severe wrinkle reduction needs. Embodiment 1, with a 5% active ingredient ratio, emphasizes gentleness and basic wrinkle-reducing effect, making it suitable for daily skincare and sensitive skin. The comparative example, due to the use of traditional high-temperature processes and generalized formulations, suffers from active ingredient inactivation, uneven dispersion, and low transdermal absorption, resulting in poor wrinkle-reducing effect, insufficient stability, and unsatisfactory gentleness. In summary, the targeted compound system and low-temperature advanced process of this invention are the key to improving the overall performance of the anti-wrinkle lipstick. The core active ingredients can be adjusted within the range of 5%-8% to meet the anti-wrinkle needs of different consumers, with 6.5% being the optimal ratio.

[0049] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reducing lip lines, characterized in that, The method includes the following steps: S1. Raw material preparation: Weigh recombinant type XVII collagen, palmitoyl tripeptide-5, acetyl tetrapeptide-9, and retinol as core active ingredients in a mass ratio of 1:1:0.8:0.

5. At the same time, prepare a complex oil phase, an aqueous matrix, and auxiliary ingredients. The total mass of the core active ingredients accounts for 5%-8% of the total mass of the lipstick. The mass ratio of the complex oil phase to the aqueous matrix is ​​3:

2. The total mass of the auxiliary ingredients accounts for 0.3%-0.5% of the total mass of the lipstick. S2. Preparation of active oil phase: Add super A alcohol to the composite oil phase, place it in a 45℃ constant temperature reactor, turn on a 300W ultrasonic device for 15min, and continuously stir during the process to control the dispersed particle size ≤100nm to obtain the active oil phase. S3. Preparation of active aqueous phase: Recombinant type XVII collagen, palmitoyl tripeptide-5, and acetyl tetrapeptide-9 were added to the aqueous matrix in sequence and stirred at 35°C until the system was homogeneous and transparent. Then, the mixture was passed through a high-pressure homogenizer and homogenized at 80 MPa to obtain the active aqueous phase. S4. Ultrasonic emulsification and fusion: The active oil phase is slowly injected into the active aqueous phase, the system temperature is maintained at 45℃, and the system is treated with an ultrasonic emulsification device at a frequency of 20kHz for 20 minutes to form a stable emulsion system. S5. Molding process: Add auxiliary ingredients to the emulsified mixture and continue stirring for 10 minutes until the system is homogeneous. Then pour it into the lipstick mold and allow it to cool and solidify naturally at room temperature of 25°C for 30 minutes. Demolding will then yield the target lipstick.

2. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, The composite oil phase in step S1 consists of meadowfoam seed oil and squalane in a mass ratio of 2:

1. The meadowfoam seed oil has an acid value ≤0.5mgKOH / g, an iodine value of 110-120gI2 / 100g, and a squalane purity ≥99%. The aqueous matrix consists of deionized water and glycerol in a mass ratio of 5:

1. The deionized water has a conductivity ≤10μS / cm, and the glycerol purity ≥99.5%. The auxiliary components include propylparaben and natural fragrance in a mass ratio of 2:1, and the propylparaben purity ≥99%.

3. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, Step S2, in preparing the active oil phase, includes the following steps: First, add the composite oil phase into the constant temperature reactor, turn on the heating device to raise the system temperature to 45℃ and keep it at that temperature for 10 minutes; Slowly add the weighed super A alcohol to the composite oil phase, turn on the stirring device, control the stirring speed to 300 r / min, and stir for 5 min to allow the super A alcohol to be initially dispersed. Turn on the 300W ultrasonic device, keep the stirring rate constant during the ultrasonic treatment, take a sample every 5 minutes, and detect the dispersed particle size using a laser particle size analyzer. When the particle size is detected to be ≤100nm and the deviation between two consecutive sampling results is ≤5%, the ultrasonic equipment and stirring device are turned off to obtain the active oil phase.

4. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, Step S3 includes the following steps in preparing the active aqueous phase: Add the aqueous matrix to the mixing tank, turn on the heating device to raise the system temperature to 35°C, and keep it at that temperature for 5 minutes; Add recombinant type XVII collagen, palmitoyl tripeptide-5, and acetyl tetrapeptide-9 to the aqueous matrix in that order. After each addition of one component, stir at a stirring rate of 250 r / min for 8 min until the component is completely dissolved before adding the next component. Once all the core active ingredients have dissolved and the system is homogeneous and transparent, the mixture is passed into a high-pressure homogenizer and homogenized three times continuously at a pressure of 80 MPa, with each homogenization lasting 2 minutes and an interval of 3 minutes between adjacent homogenizations. After homogenization, the active aqueous phase is obtained.

5. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, In step S4, the rate of injecting the active oil phase into the active aqueous phase is 5 mL / min, and the stirring rate is maintained at 250 r / min during the injection process. During ultrasonic emulsification, the probe of the ultrasonic device is inserted into the system to a depth of 2-3 cm below the liquid surface, and the distance between the probe and the container wall is ≥5 cm. The probe position is adjusted every 4 minutes during the ultrasonic process, and the adjustment range is 1 cm each time.

6. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, In step S1, the purity of the core active ingredients is ≥98%, wherein the molecular weight of recombinant type XVII collagen is 150-200kDa, the molecular weight of palmitoyl tripeptide-5 is 497.6Da, the molecular weight of acetyl tetrapeptide-9 is 411.5Da, and the molecular weight of retinol is 328.5Da.

7. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, The lipstick mold used in step S5 is made of food-grade aluminum alloy. The inner wall of the mold is polished and the surface roughness Ra≤0.8μm. Before injecting into the mixing system, the mold is sterilized at 120℃ for 20min and then cooled to 25℃ for use. During the cooling and curing process, the relative humidity of the environment is controlled at 40%-60%.

8. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, In step S2, the ultrasonic frequency of the ultrasonic device is 20kHz, and the ultrasonic mode is intermittent ultrasonic, that is, working for 3 seconds, pausing for 1 second, and continuing for 15 minutes. In step S4, the ultrasonic emulsification device uses continuous ultrasonic mode, and the system temperature is monitored in real time during the ultrasonic process. When the temperature exceeds 45℃, the cooling device is activated to bring the temperature back to 45℃ before continuing the ultrasonic treatment.

9. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, In step S3, the feed rate of the high-pressure homogenizer is controlled at 10-15 L / h, the system temperature is maintained at 35±2℃ during homogenization, and the active aqueous phase after homogenization is filtered through a polyethersulfone filter membrane with a pore size of 0.22 μm. During the filtration process, the filtration pressure is maintained at 0.1-0.15 MPa, and the filtration rate is uniform and stable.

10. The method for preparing a lipstick containing polypeptides and retinol for deep nourishment and reduction of lip lines according to claim 1, characterized in that, In step S1, the core active ingredient is placed in a sealed, light-proof container before storage and use. The storage environment temperature is controlled at 2-8℃, the relative humidity is ≤60%, and the storage time does not exceed 6 months. Before use, the core active ingredient is placed in a constant temperature environment of 35℃ for 12 hours to warm up. The ingredient temperature is added after it is consistent with the temperature of the subsequent preparation system.

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