A targeted anti-aging microemulsion skin care preparation containing procyanidine C1 and a preparation method thereof

Abstract

This invention discloses a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 and its preparation method, comprising the following components by weight percentage: oil phase: 12%–22%; nonionic surfactant: 18%–28%; co-surfactant: 6%–12%; proanthocyanidin C1: 0.8%–4.5%; marine collagen oligopeptides: 2%–7%; targeted modification component: 0.2%–0.8%; deionized water: balance; the formulation is an oil-in-water microemulsion with a particle size of 10–50 nm and a polydispersity index ≤0.2; the purity of the proanthocyanidin C1 is ≥95%; this invention relates to the field of anti-aging technology. This targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 and its preparation method involve compounding an oil phase, nonionic surfactant, and co-surfactant in a specific ratio, combined with a two-stage high-pressure microfluidic homogenization process, to prepare an oil-in-water nanoscale microemulsion with a particle size strictly controlled within the range of 10–40 nm and a polydispersity index ≤0.15. The system is uniform and delicate, without stratification, flocculation, or oil droplet aggregation.

Description

Technical Field

[0001] This invention relates to the field of anti-aging technology, specifically to a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 and its preparation method. Background Technology

[0002] As research on skin aging continues to deepen, oxidative stress damage, collagen loss, and low transdermal absorption efficiency of active ingredients have become major technical bottlenecks for anti-aging skincare products. Proanthocyanidins C1 possess extremely strong free radical scavenging ability and antioxidant activity, but their poor stability and susceptibility to damage from light and oxygen, coupled with the difficulty in achieving deep-layer targeted delivery to the skin when simply added, limit their efficacy.

[0003] Marine collagen oligopeptides have small molecular weights and are easily absorbed, which can replenish skin collagen and improve skin elasticity. However, when combined with antioxidant ingredients, they are prone to problems such as system instability and poor compatibility. Existing anti-aging microemulsion formulations generally have defects such as large particle size, poor dispersibility, insufficient stability, and low transdermal efficiency, making it difficult to achieve the synergistic effects of high antioxidant capacity, high collagen replenishment, high targeted absorption, and high storage stability at the same time.

[0004] Furthermore, traditional microemulsion preparation processes do not strictly control light and oxygen levels, which can easily lead to the degradation of active ingredients such as proanthocyanidin C1, reducing product efficacy and shelf life. Currently, there is a lack of targeted anti-aging microemulsion skincare formulations that are scientifically formulated, have controllable particle size, strong targeting, and high stability, and can efficiently combine proanthocyanidin C1 with marine collagen oligopeptides. This fails to meet the market's demand for highly effective, safe, and stable anti-aging skincare products.

[0005] To address these issues, this invention proposes a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 and its preparation method. Summary of the Invention

[0006] (a) Technical problems to be solved To address the shortcomings of existing technologies, this invention provides a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 and its preparation method, thus solving the problems mentioned in the background section.

[0007] (II) Technical Solution To achieve the above objectives, the present invention provides the following technical solution: a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1, comprising the following components by weight percentage: Oil phase: 12%~22%; Nonionic surfactants: 18%–28%; Co-surfactant: 6%–12%; Proanthocyanidins C1: 0.8%–4.5%; Marine collagen oligopeptides: 2%–7%; Targeted modification components: 0.2%–0.8%; Deionized water: Balance; The formulation is an oil-in-water microemulsion with a particle size of 10–50 nm and a polydispersity index ≤0.2; the purity of the proanthocyanidin C1 is ≥95%; the molecular weight of the marine collagen oligopeptides is ≤800 Da, and ≥70% of the peptides have a molecular weight between 300 and 600 Da.

[0008] Preferably, the oil phase is composed of two or three of the following components in a specific mass ratio: Squalane: 30%–60%; Jojoba oil: 20%–40%; Caprylic / capric triglyceride: 10%–30%; and the viscosity of the oil phase at 25°C is 20–100 mPa·s.

[0009] Preferably, the nonionic surfactant is a compound system of Tween 80 and Span 60 with a mass ratio of 2:1 to 5:1; the co-surfactant is a compound system of 1,2-propanediol and polyethylene glycol-400 with a mass ratio of 1:1 to 3:1.

[0010] Preferably, the marine collagen oligopeptides are derived from salmon skin and prepared using an enzymatic hydrolysis-ultrafiltration process. The total content of glycine, proline, and hydroxyproline in their amino acid composition is ≥45%, and the proportion of peptides with glycine at the N-terminus is ≥60%.

[0011] Preferably, the targeted modification component is a chitosan quaternary ammonium salt with a degree of deacetylation ≥90%, a degree of quaternization substitution ≥60%, and a molecular weight of 5-50 kDa; or the targeted modification component is a collagen affinity peptide whose amino acid sequence contains Gly-XY repeating units and the number of repeating units is ≥6.

[0012] Preferably, the formulation further comprises 0.1% to 2% of a plant-derived antioxidant adjuvant, wherein the plant-derived antioxidant adjuvant is selected from one or more of rosemary extract, green tea polyphenols, and grape seed extract, and its total polyphenol content is ≥50mg / g.

[0013] A method for preparing a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 includes the following steps: Step 1: Preparation of oil phase: Weigh the oil phase, nonionic surfactant, and co-surfactant according to the proportion, place them in a jacketed reactor, and stir in a water bath at 45-60℃ at 200-400r / min for 15-30min until uniform and transparent to obtain an oil phase mixture. Step 2, Aqueous phase preparation: Proanthocyanidin C1, marine collagen oligopeptides, targeted modification components and plant-derived antioxidants are dissolved in deionized water in sequence, the dissolution temperature is controlled at 25-40℃, and the mixture is stirred at 100-300 r / min for 20-40 min until completely dissolved to obtain an aqueous phase mixture. The pH of the aqueous phase is adjusted to 5.5-6.5. Step 3, Pre-emulsification: Under stirring conditions of 40-55℃ and 400-600r / min, the aqueous phase mixture is added dropwise to the oil phase mixture at a rate of 2-10mL / min. After the addition is completed, stirring is continued for 30-60min to obtain the pre-emulsion. Step 4, High-pressure homogenization: Transfer the pre-emulsion to a high-pressure microfluidic homogenizer and homogenize it 2 to 5 times at a pressure of 300 to 800 bar, with the homogenization temperature controlled at 25 to 45°C. Step 5, Post-processing: The homogenized emulsion is cooled to room temperature under light-protected conditions and filtered through a 0.22μm filter membrane to obtain the microemulsion skin care formulation; Steps one through five are performed entirely under yellow light (wavelength 580–600 nm) or red light (wavelength 620–750 nm) conditions, with an illuminance ≤ 50 lux. Preferably, in step four, the high-pressure homogenization adopts a two-stage homogenization process: the first-stage homogenization pressure is 500-800 bar, and the second-stage homogenization pressure is 100-300 bar; the microemulsion particle size after homogenization is 10-40 nm, the polydispersity index is ≤0.15, and the absolute value of the Zeta potential is ≥30 mV.

[0014] Preferably, the preparation method further includes step six: filling the obtained microemulsion skin care preparation into an opaque container under nitrogen protection at a filling temperature of 20-30°C, and filling the top space of the container with nitrogen until the residual oxygen content is ≤2%.

[0015] (III) Beneficial Effects This invention provides a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 and its preparation method. Compared with the prior art, it has the following beneficial effects: (1) The targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 and its preparation method are disclosed. A water-in-oil nanoscale microemulsion is prepared by compounding an oil phase, nonionic surfactant, and co-surfactant in a specific ratio, combined with a two-stage high-pressure microfluidic homogenization process. The particle size is strictly controlled within the range of 10–40 nm, with a polydispersity index ≤0.15. The system is uniform and delicate, without stratification, flocculation, or oil droplet aggregation. Compared with conventional microemulsions, the microemulsion of this invention has a smaller particle size and narrower distribution, which can significantly reduce interfacial tension, improve the appearance transparency and skin comfort of the formulation, and meet the high requirements of high-end skincare products for dosage form appearance and user experience.

[0016] (2) The targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 and its preparation method optimize the emulsification system and targeted modification components, so that the absolute value of the microemulsion zeta potential is ≥30mV, the electrostatic repulsion between particles is sufficient, and the dispersion stability can be maintained for a long time, and it is not easy to have phenomena such as layering, demulsification, and sedimentation. At the same time, the entire preparation process is carried out under low-illuminance yellow or red light conditions, and nitrogen protection and light-proof filling are used to ensure that the oxygen residue at the top of the container is ≤2%, which significantly reduces the oxidative degradation of proanthocyanidin C1 by oxygen and light, greatly improves the retention rate of active ingredients and product shelf life, and solves the industry pain points of traditional antioxidant skincare products being easy to deactivate and not resistant to storage.

[0017] (3) The targeted anti-aging microemulsion skin care preparation containing proanthocyanidin C1 and its preparation method use proanthocyanidin C1 with a purity of ≥95% as the core antioxidant ingredient, combined with plant-derived antioxidant auxiliaries such as rosemary extract, green tea polyphenols, and grape seed extract to form a multi-level antioxidant system. The DPPH free radical scavenging rate is as high as 81.3%~95.8%, which can effectively remove excess free radicals in the skin, inhibit lipid peroxidation, reduce oxidative stress damage caused by external factors such as ultraviolet rays and environmental pollution, delay collagen cross-linking and fiber aging at the cellular level, lighten fine lines, improve dullness, and achieve long-lasting antioxidant and anti-aging effects.

[0018] (4) This targeted anti-aging microemulsion skincare preparation containing proanthocyanidin C1 and its preparation method, by adding marine collagen oligopeptides derived from salmon skin with a molecular weight ≤800Da, of which more than 70% of the peptides have a molecular weight of 300-600Da and are rich in glycine, proline, and hydroxyproline, can be directly absorbed and utilized by the skin to quickly replenish lost collagen, promote the regeneration and remodeling of collagen fibers in the dermis, and enhance skin support and elasticity. Synergistically working with proanthocyanidin C1, it achieves the dual effects of "antioxidant and damage prevention + collagen replenishment," significantly improving aging problems such as skin laxity, roughness, and fine lines, resulting in a more comprehensive and lasting anti-aging effect. Attached Figure Description

[0019] Figure 1 Comparison of Zata potential test results for the microemulsion skin care formulation provided by the present invention; Figure 2 Comparison chart of DPPH free radical scavenging rate test of the microemulsion skin care formulation provided by the present invention. Detailed Implementation

[0020] 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. Example 1

[0021] Component composition (weight percentage) Oil phase: 18%; Nonionic surfactant: 23%; Co-surfactant: 9%; Proanthocyanidin C1: 2.0%; Marine collagen oligopeptides: 4.5%; Targeted modification components: 0.5%; Plant-derived antioxidant adjuvants: 0.8%; Deionized water: Balance.

[0022] Oil phase composition: 50% squalane, 30% jojoba oil, 20% caprylic / capric triglycerides Nonionic surfactant: Tween 80: Span 60 = 3:1 Co-surfactant: 1,2-propanediol: polyethylene glycol-400 = 2:1 Plant-derived antioxidant adjuvant: Rosemary extract (total polyphenol content ≥50mg / g) Preparation method Step 1: Oil phase preparation: Weigh the oil phase, nonionic surfactant, and co-surfactant according to the proportion, and stir in a 50℃ water bath at 300r / min for 20min until uniform and transparent.

[0023] Step 2, Aqueous phase preparation: Dissolve proanthocyanidin C1, marine collagen oligopeptides, chitosan quaternary ammonium salt, and rosemary extract in deionized water, stir at 30℃ and 200r / min for 30min until completely dissolved, and adjust the pH to 6.0.

[0024] Step 3, Pre-emulsification: At 45℃ and 500r / min, the aqueous phase is added dropwise to the oil phase at a rate of 5mL / min, and the mixture is stirred for 45min after the addition is complete.

[0025] Step 4, High-pressure homogenization: Two-stage homogenization, first stage 600 bar, second stage 200 bar, homogenization 3 times, temperature 35℃.

[0026] Step 5, Post-processing: Cool to room temperature in the dark, filter with a 0.22μm filter membrane, and operate under yellow light (590nm) at an illuminance of 40 lux throughout.

[0027] Step 6, Filling: Fill into opaque containers under nitrogen protection, with the oxygen residue at the top ≤2%. Example 2

[0028] Component composition (weight percentage) Oil phase: 12%; Nonionic surfactant: 18%; Co-surfactant: 6%; Proanthocyanidin C1: 0.8%; Marine collagen oligopeptides: 2%; Targeted modification components: 0.2%; Plant-derived antioxidant adjuvants: 0.1%; Deionized water: Balance.

[0029] Oil phase composition: 60% squalane, 40% jojoba oil Nonionic surfactant: Tween 80: Span 60 = 2:1 Co-surfactant: 1,2-propanediol: polyethylene glycol-400 = 1:1 Plant-derived antioxidant adjuvant: Green tea polyphenols (total polyphenol content ≥50mg / g) Preparation method Same as Example 1, homogenization parameters: 500 bar for the first stage, 100 bar for the second stage, homogenized twice. Example 3

[0030] Component composition (weight percentage) Oil phase: 22%; Nonionic surfactant: 28%; Co-surfactant: 12%; Proanthocyanidin C1: 4.5%; Marine collagen oligopeptides: 7%; Targeted modification components: 0.8%; Plant-derived antioxidant auxiliaries: 2%; Deionized water: Balance.

[0031] Oil phase composition: 30% squalane, 20% jojoba oil, 30% caprylic / capric triglycerides Nonionic surfactant: Tween 80: Span 60 = 5:1 Co-surfactant: 1,2-propanediol: polyethylene glycol-400 = 3:1 Plant-derived antioxidant adjuvant: Grape seed extract (total polyphenol content ≥50mg / g) Preparation method Same as Example 1, homogenization parameters: 800 bar for the first stage, 300 bar for the second stage, homogenized 5 times.

[0032] Comparative Example 1 Compared with Example 1, this one does not contain proanthocyanidin C1, but the other components, proportions, and preparation methods are exactly the same.

[0033] Comparative Example 2 Compared to Example 1, this one does not contain marine collagen oligopeptides, but all other components, proportions, and preparation methods are exactly the same.

[0034] Comparative Example 3 Compared with Example 1, this one does not contain the targeted modification component, but the remaining components, proportions, and preparation methods are exactly the same.

[0035]

[0036] From the table above and Figure 1 It can be known that: (1) The average particle size of Examples 1-3 was 22-35 nm, and the polydispersity index was 0.10-0.14. The system was uniform and fine. The particle size and PDI of Comparative Example 1 (without proanthocyanidin C1) increased slightly; the uniformity of Comparative Example 2 (without marine collagen oligopeptides) decreased; the particle size of Comparative Example 3 (without targeting components) increased to 41 nm and the PDI reached 0.22, and the microemulsion state deteriorated significantly.

[0037] (2) Examples 1-3 showed excellent stability with a Zeta potential of -32 to -42 mV. Comparative Examples 1 and 2 showed a slight decrease in stability; Comparative Example 3 showed a significantly reduced stability with a Zeta potential of only -18 mV, and was prone to aggregation and stratification.

[0038] (3) Examples 1-3 showed DPPH scavenging rates of 81.3% to 95.8%, with outstanding antioxidant effects. Comparative Example 1 (without proanthocyanidin C1) saw a sharp drop to 42.6%; Comparative Example 2 saw a drop to 70.2%; and Comparative Example 3 saw a slight drop to 85.1%.

[0039] Furthermore, any content not described in detail in this specification is existing technology known to those skilled in the art.

[0040] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0041] 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 targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1, characterized in that, Composed of the following components by weight percentage composition: Oil phase: 12%~22%; Nonionic surfactants: 18%–28%; Co-surfactant: 6%–12%; Proanthocyanidins C1: 0.8%–4.5%; Marine collagen oligopeptides: 2%–7%; Targeted modification components: 0.2%–0.8%; Deionized water: Balance; The formulation is an oil-in-water microemulsion with a particle size of 10–50 nm and a polydispersity index ≤0.2; the purity of the proanthocyanidin C1 is ≥95%; the molecular weight of the marine collagen oligopeptides is ≤800 Da, and ≥70% of the peptides have a molecular weight between 300 and 600 Da.

2. The targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 according to claim 1, characterized in that: The oil phase is composed of two or three components in a mass ratio: Squalane: 30%–60%; Jojoba oil: 20%–40%; Caprylic / capric triglyceride: 10%–30%; and the viscosity of the oil phase at 25°C is 20–100 mPa·s.

3. The targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 according to claim 1, characterized in that: The nonionic surfactant is a compound system of Tween 80 and Span 60 with a mass ratio of 2:1 to 5:1; the co-surfactant is a compound system of 1,2-propanediol and polyethylene glycol-400 with a mass ratio of 1:1 to 3:

1.

4. The targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 according to claim 1, characterized in that: The marine collagen oligopeptides are derived from salmon skin and prepared using an enzymatic hydrolysis-ultrafiltration process. The total content of glycine, proline, and hydroxyproline in their amino acid composition is ≥45%, and the proportion of peptides with glycine at the N-terminus is ≥60%.

5. The targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 according to claim 1, characterized in that: The targeted modification component is a chitosan quaternary ammonium salt with a degree of deacetylation ≥90%, a degree of quaternization substitution ≥60%, and a molecular weight of 5–50 kDa; or the targeted modification component is a collagen affinity peptide whose amino acid sequence contains Gly-XY repeating units with a repeating unit number ≥6.

6. The targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 according to claim 1, characterized in that: The formulation also contains 0.1% to 2% of plant-derived antioxidant adjuvants, which are selected from one or more of rosemary extract, green tea polyphenols, and grape seed extract, and have a total polyphenol content ≥50mg / g.

7. A method for preparing a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 according to claim 1, characterized in that, Includes the following steps: Step 1: Preparation of oil phase: Weigh the oil phase, nonionic surfactant, and co-surfactant according to the proportion, place them in a jacketed reactor, and stir in a water bath at 45-60℃ at 200-400r / min for 15-30min until uniform and transparent to obtain an oil phase mixture. Step 2, Aqueous phase preparation: Proanthocyanidin C1, marine collagen oligopeptides, targeted modification components and plant-derived antioxidants are dissolved in deionized water in sequence, the dissolution temperature is controlled at 25-40℃, and the mixture is stirred at 100-300 r / min for 20-40 min until completely dissolved to obtain an aqueous phase mixture. The pH of the aqueous phase is adjusted to 5.5-6.

5. Step 3, Pre-emulsification: Under stirring conditions of 40-55℃ and 400-600r / min, the aqueous phase mixture is added dropwise to the oil phase mixture at a rate of 2-10mL / min. After the addition is completed, stirring is continued for 30-60min to obtain the pre-emulsion. Step 4, High-pressure homogenization: Transfer the pre-emulsion to a high-pressure microfluidic homogenizer and homogenize it 2 to 5 times at a pressure of 300 to 800 bar, with the homogenization temperature controlled at 25 to 45°C. Step 5, Post-processing: The homogenized emulsion is cooled to room temperature under light-protected conditions and filtered through a 0.22μm filter membrane to obtain the microemulsion skin care formulation; Steps one through five are performed entirely under yellow light (wavelength 580–600 nm) or red light (wavelength 620–750 nm) conditions, with an illuminance of ≤50 lux.

8. The method for preparing a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 according to claim 7, characterized in that: In step four, the high-pressure homogenization adopts a two-stage homogenization process: the first-stage homogenization pressure is 500-800 bar, and the second-stage homogenization pressure is 100-300 bar; the microemulsion particle size after homogenization is 10-40 nm, the polydispersity index is ≤0.15, and the absolute value of the Zeta potential is ≥30 mV.

9. The method for preparing a targeted anti-aging microemulsion skincare formulation containing proanthocyanidin C1 according to claim 7, characterized in that: The preparation method further includes step six: filling the obtained microemulsion skin care preparation into an opaque container under nitrogen protection at a filling temperature of 20-30°C, and filling the top space of the container with nitrogen until the residual oxygen content is ≤2%.

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