Moisture-locking, film-forming and multi-channel relieving and repairing compound, preparation method therefor, and use thereof

By using a composite membrane structure of sodium hyaluronate, budding short stem enzyme polysaccharide, and polyquaternium salt, combined with the use of specific ingredients, the problems of insufficient water-locking capacity and skin irritation in moisturizing skin care products are solved, achieving long-lasting moisturizing and soothing effects.

WO2026026851A1PCT designated stage Publication Date: 2026-02-05SICHUAN ZERUN JIAMEI COSMETICS CO LTD
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Patent Information

Application Number
PCT/CN2025/111486
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-08-02
Filing Date
2025-07-30
Publication Date
2026-02-05

AI Technical Summary

Technical Problem

Existing moisturizing skincare products have insufficient water-locking ability, leading to rapid moisture loss, and high molecular polymers can easily clog containers and irritate the skin.

Method used

A membrane structure is formed by combining sodium hyaluronate, budding short stem enzyme polysaccharide and polyquaternium salt, and combined with ingredients such as disodium EDTA, menthol, hydrogenated castor oil and European sour cherry blossom extract to form a complex that locks in moisture, forms a film, and provides multi-pathway soothing and repair. The stability and safety of the ingredients are improved by controlling the degree of acetyl substitution and using specific catalysts.

Benefits of technology

It achieves long-lasting moisture retention, inhibits moisture evaporation, reduces skin irritation, provides a continuous cooling and soothing sensation, improves skin absorption, and enhances user comfort and moisturizing effects.

✦ Generated by Eureka AI based on patent content.

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    Figure PCTCN2025111486-FTAPPB-I100003
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Abstract

A moisture-locking, film-forming, and multi-channel relieving and repairing compound, a preparation method therefor, and use thereof. The compound comprises: 0.1-15% of glycerin, 0.1-25% of a humectant, 0.01-0.5% of disodium ethylenediaminetetraacetic acid, 0.01-0.5% of polyquaternium, 0.01-0.5% of menthol, 0.01-2% of hydrogenated castor oil, 0.01-2% of a preservative, 0.01-0.1% of a European sour cherry flower extract, 0.01-0.1% of a bitter orange flower hydrolat, with the balance being deionized water; the humectant comprises 10-20 parts of sodium hyaluronate, 5-15 parts of aureobasidium pullulans polysaccharide, 5-10 parts of serine, and 1-5 parts of sodium alginate. The compound can be used for preparing skin care products such as sprays, creams, emulsions, and essences, and it features fast absorption and long-lasting moisturizing effects. At the same time, the product will not block the nozzle of a packaging container during long-term use.
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Description

Water-locking film-forming and multi-channel soothing repair composite, preparation method and application thereof TECHNICAL FIELD

[0001] The present application relates to the field of cosmetics, more particularly, it relates to a water-locking film-forming and multi-channel soothing repair composite, preparation method and application thereof. BACKGROUND

[0002] Moisturizing skin care products are cosmetic products with moisturizing and soothing effects. The product formula mostly contains mineral water, polyols and moisturizing agents, etc. It can be made into products in various forms such as spray, cream, emulsion and essence. Consumers can achieve the effects of rapid skin moisturizing and soothing after use.

[0003] Many moisturizing skin care products contain small molecule polyols. Due to their small molecular structure, small molecule polyols can be quickly absorbed by the skin, providing an immediate sense of hydration. However, the water retention capacity of small molecule polyols is relatively weak. They mainly increase the water content of the skin by combining with water molecules, but cannot form a long-lasting moisturizing barrier on the skin surface. Therefore, when the environmental humidity decreases or the skin's own water evaporates, these water molecules are easily lost, resulting in the short-term nature of the moisturizing effect and the inability to provide long-term hydration to the skin. Moreover, the rapid absorption and loss of water often cause uneven makeup and makeup removal after makeup.

[0004] In order to solve the problem of long-term moisturizing, some existing products have begun to use high molecular polymers. This type of polymer can form a protective film on the skin surface, effectively locking in moisture and providing long-term hydration to the skin. However, at the same time, this high molecular polymer also brings new problems in the use process. Due to its viscous texture, on the one hand, it is easy to block the spray nozzle of the packaging container, affecting the user experience, and on the other hand, it can cause discomfort to some consumers with sensitive skin.

[0005] Therefore, there is a need for a moisturizing product that is fast-absorbing and has long-lasting moisturizing effects, while also being non-clogging and soothing to the skin during long-term use. SUMMARY

[0006] To solve the above problems, the present application provides a water-locking film-forming and multi-channel soothing repair composite, preparation method and application thereof.

[0007] In a first aspect, the water-locking film-forming and multi-channel soothing repair composite provided by the present application adopts the following technical solution:

[0008] A compound with water-locking film-forming and multi-channel soothing repair, comprising the following components by mass percentage: 0.1-15% glycerol, 0.1-25% humectant, 0.01-0.5% disodium ethylenediaminetetraacetate, 0.01-0.5% polyquaternary ammonium salt, 0.01-0.5% menthol, 0.01-2% hydrogenated castor oil, 0.01-2% preservative, 0.01-0.1% European sour cherry flower extract and 0.01-0.1% bitter orange flower hydrolat, and the rest is deionized water, wherein the humectant comprises 10-20 parts of sodium hyaluronate, 5-15 parts of pullulan, 5-10 parts of serine and 1-5 parts of sodium alginate by weight.

[0009] By adopting the above technical scheme, since sodium hyaluronate, pullulan and polyquaternary ammonium salt are compounded to form a film structure, the water in the skin can be locked, the evaporation and loss of skin moisture can be effectively inhibited, long-term continuous moisturizing can be provided for the skin, and the long-acting moisturizing effect of the product is ensured. The addition of disodium ethylenediaminetetraacetate can stabilize the polyquaternary ammonium salt, reduce the agglomeration and precipitation of the polyquaternary ammonium salt in the compound, and prevent uneven distribution of the polyquaternary ammonium salt in the compound from causing poor film-forming effect. Menthol can bring a cooling feeling and has the effects of soothing skin irritation and reducing swelling. The lubricity and moisturizing property of hydrogenated castor oil can improve the absorption capacity of the skin, so that menthol can better penetrate into the deep layer of the skin and play its soothing role. The combination of the lubricating property of hydrogenated castor oil and the cooling feeling of menthol can continuously stimulate the cooling effect and will not cause stinging and discomfort, reducing the discomfort of the skin. The European sour cherry flower extract is rich in various antioxidant components such as vitamin C and polyphenols. These components can neutralize free radicals and reduce the damage of oxidative stress to the skin. The bitter orange flower hydrolat also contains antioxidant components, which can reduce the damage of oxidative stress to the skin, help to delay skin aging, and have the effects of moisturizing, anti-inflammatory, brightening and plant fragrance.

[0010] Optionally, the humectant further comprises 5-15 parts of acetylated sodium hyaluronate by weight, and the preparation method of the acetylated sodium hyaluronate is as follows:

[0011] Prepare hyaluronic acid with a molecular weight of 500-2000 kDa, a mixed solvent of acetic acid and acetic anhydride in a mass ratio of 1:(1.5-3.5), a catalyst, and a 5% sodium bicarbonate solution;

[0012] Put the hyaluronic acid in the mixed solvent, and the mass ratio of hyaluronic acid to mixed solvent is 1:(20-40). Under the temperature condition of 5-40℃, add 1-3% of the total mass of the reaction solution of the catalyst, and carry out acylation reaction. When the reaction solution is completely transparent, the reaction is completed;

[0013] The completely transparent reaction solution is added into water to precipitate, the fibrous precipitate is collected, and the precipitate is washed with deionized water to obtain acetylated hyaluronic acid;

[0014] After the pH value of the acetylated hyaluronic acid is adjusted to neutral by using a sodium bicarbonate solution, the acetylated hyaluronic acid is filtered, diluted with deionized water to a concentration of 10-50 mL / g, and then filtered, and spray drying is performed by using a spray drying device, wherein the inlet air temperature is 100-200 DEG C, and the outlet air temperature is 70-120 DEG C.

[0015] Optionally, the average degree of substitution of acetyl groups in the acetylated sodium hyaluronate is 3.0-3.3, and the catalyst comprises triethylamine and 4-dimethylaminopyridine in a mass ratio of 1:(3-5).

[0016] By using the above technical solution, the acetylated sodium hyaluronate has a stronger moisturizing effect when the average degree of substitution of acetyl groups is 3.0-3.3, and the above reaction is carried out at a lower temperature, which helps to reduce the occurrence of side reactions and improve the purity and quality of the product. At the same time, the use of triethylamine and 4-dimethylaminopyridine can accelerate the reaction process and improve the reaction efficiency. Compared with the conventional use of sulfuric acid as a catalyst, the present method can efficiently react at a lower temperature, and the harmful impurities in the product are lower, and the skin will not be stimulated. By adjusting with a sodium bicarbonate solution, the pH value of the acetylated sodium hyaluronate reaches neutral, which helps to reduce the irritability of the product to the skin and improve the comfort of use.

[0017] Optionally, the moisturizing agent further comprises trehalose and carrageenan oligosaccharide, the carrageenan oligosaccharide is compounded with the acetylated sodium hyaluronate in a mass ratio of 1:(3.5-6.5), and the carrageenan oligosaccharide is compounded with the trehalose in a mass ratio of 1:(2-4).

[0018] By using the above technical solution, trehalose has good water retention and can effectively lock water when applied to the skin surface, improving the water content while allowing the skin to remain moist continuously. Trehalose can also reduce the damage of irritants to the skin, promote epidermal cell regeneration, and enhance the stability of the stratum corneum, which helps to repair damaged tissues. Carrageenan oligosaccharide can absorb a large amount of water to form a gel, thereby improving the moisturizing property of the skin. The combination of carrageenan oligosaccharide and trehalose in a mass ratio of 1:(2-4) can achieve higher moisturizing effect, thereby providing long-term nourishment and moisturizing for the skin. The combination of acetylated sodium hyaluronate and carrageenan oligosaccharide can provide long-lasting moisturizing for the skin. At the same time, the combination of acetylated sodium hyaluronate and carrageenan oligosaccharide can further promote the repair and regeneration of the skin.

[0019] Optionally, the preservative comprises one or more of decanoic acid triglyceride, phenoxyethanol, and potassium sorbate.

[0020] By adopting the technical scheme, the decanoic acid triglyceride has the dual effects of antibiosis and moisturization, can inhibit the growth of microorganisms to a certain extent, maintain the moisture of the product, prevent the product from deteriorating, has little skin irritation, and is suitable for sensitive skin.

[0021] Optionally, the compound having water-locking film-forming and multi-channel soothing repair further comprises 1-3% of microencapsulated calcium sulfate by mass percentage, and the preparation method of the microencapsulated calcium sulfate is as follows:

[0022] 30-50 parts of nano calcium sulfate powder by weight is added into 150 parts of a 20-40 wt% polylactic acid solution, mixed by using ultrasonic vibration, the mixed solution is transferred to an emulsification device, stirred at 60-80 r / min at 75-85°C, and emulsified for 40-60 min, the emulsified microcapsule suspension is placed in acetone, the solidification time is controlled, and after solidification, the microencapsulated calcium sulfate is obtained by centrifugal separation, and the microencapsulated calcium sulfate is washed with deionized water.

[0023] By adopting the technical scheme, the microencapsulated calcium sulfate can keep the calcium sulfate particles in the compound in a relatively stable state, and does not increase the viscosity of the compound during storage, so that when the user uses the compound on the skin surface by rubbing, applying or the like, the microencapsulated coating wall material of the microencapsulated calcium sulfate in the compound is damaged, so that the nano calcium sulfate directly contacts the moisturizing agent, the nano calcium sulfate can increase the viscosity and adhesion of the moisturizing agent, play a role in accelerating the promotion of gelation, so that the moisturizing agent can quickly form a film, not only can lock the water in the skin, effectively inhibit the evaporation and loss of skin moisture, but also can prevent the drying effect of the external environment on the skin, and by controlling the addition amount of the microencapsulated calcium sulfate to be 1-3%, the film-forming effect can be ensured, and the skin will not feel sticky.

[0024] In a second aspect, the application provides a preparation method of a compound having water-locking film-forming and multi-channel soothing repair, which adopts the following technical scheme:

[0025] A preparation method of a compound having water-locking film-forming and multi-channel soothing repair, comprising the following steps:

[0026] Deionized water, glycerol, a moisturizing agent, disodium ethylenediaminetetraacetate, and a polyquaternary ammonium salt are mixed, heated to 80-85°C and stirred until completely dissolved to obtain component A;

[0027] Cooling component A to 40-45℃, adding component B, component C to component A in turn, and stirring uniformly to obtain a mixed solution, component B includes a mixture of menthol, hydrogenated castor oil, European sour cherry flower extract and bitter orange flower hydrolat, and component C includes a preservative;

[0028] Cooling the mixed solution to below 35℃ and discharging to obtain a compound with water-locking film-forming and multi-channel soothing repair.

[0029] Optionally, component C further includes microencapsulated calcium sulfate.

[0030] By mixing and heating deionized water, glycerol, a humectant, disodium ethylenediaminetetraacetate and a polyquaternary ammonium salt to 80-85℃, it can be ensured that these ingredients are fully dissolved and uniformly distributed, and this step ensures that the moisturizing effect of glycerol and the humectant and the film-forming effect of the polyquaternary ammonium salt can be maximized. Adding a mixture of menthol, hydrogenated castor oil, European sour cherry flower extract and bitter orange flower hydrolat at 40-45℃ helps to uniformly disperse the ingredients at a lower temperature and prevents degradation of heat-sensitive ingredients. Hydrogenated castor oil maintains its film-forming properties at a lower temperature, further enhancing the water-locking effect. Adding a preservative at a lower temperature ensures the activity and stability of the preservative while reducing its impact on other active ingredients. The effectiveness of the preservative ensures the safety and shelf life of the product.

[0031] In a third aspect, the present application provides an application of a compound with water-locking film-forming and multi-channel soothing repair, which adopts the following technical solution:

[0032] An application of a compound with water-locking film-forming and multi-channel soothing repair, the compound with water-locking film-forming and multi-channel soothing repair is used for preparing a skin care product, and the skin care product includes a skin care product such as a spray, a cream, a lotion or an essence.

[0033] In summary, the present application has the following beneficial effects

[0034] 1. Since the present application combines glycerol, a humectant, a polyquaternary ammonium salt, disodium ethylenediaminetetraacetate, menthol and hydrogenated castor oil, glycerol provides a water-rubbing feeling to the skin, and the composite film formed by the humectant and the polyquaternary ammonium salt can lock in skin moisture for a long time, effectively preventing water loss and the influence of the external dry environment. Disodium ethylenediaminetetraacetate stabilizes the polyquaternary ammonium salt and has anti-inflammatory soothing effect, and menthol and hydrogenated castor oil together provide a cooling and soothing experience, while improving the skin's ability to absorb, ensuring that the cooling effect is sustained and gentle, and bringing a long-lasting moisturizing and comfortable experience to the user.

[0035] 2, The specific catalyst combination of triethylamine and 4-dimethylaminopyridine is preferred in the application, which not only accelerates the reaction and improves the efficiency, but also significantly reduces the harmful impurities in the acetylated sodium hyaluronate product, ensuring the mildness of the acetylated sodium hyaluronate to the skin. Finally, by adjusting the sodium bicarbonate solution, the pH value of the acetylated sodium hyaluronate is neutralized, further reducing the irritation to the skin and improving the comfort of use.

[0036] 3, The preferred method in the application is to compound carrageenan oligosaccharide with trehalose at a ratio of 1:2 to 1:4, which significantly improves the moisturizing effect and brings long-term moisturizing and moisturizing to the skin, thereby improving the touch of the skin and making it softer and smoother. When acetylated sodium hyaluronate is used with carrageenan oligosaccharide, the two work together to not only strengthen the moisturizing effect and bring long-lasting moisturizing to the skin, but also further promote the repair and regeneration process of the skin.

[0037] 4, The preferred method in the application is to use microencapsulated calcium sulfate technology to keep calcium sulfate particles stable in the complex, avoiding an increase in viscosity. When used, the microcapsule membrane is destroyed by rubbing or applying, releasing nano calcium sulfate, which can increase the viscosity and adhesion of the moisturizer, promote the gelation process, and make the moisturizer form a protective film quickly. This technology not only effectively locks in skin moisture and inhibits its evaporation and loss, but also resists the drying effects of the external environment on the skin. By controlling the addition amount of microencapsulated calcium sulfate to be 1-3%, the ideal film-forming effect is ensured while avoiding a sticky feeling on the skin. DETAILED DESCRIPTION

[0038] The application is further described in conjunction with the following examples, and it is particularly noted that: in the following examples, the specific conditions are not specified, and the conventional conditions or the conditions recommended by the manufacturer are used. The raw materials used in the following examples can be obtained from ordinary commercial sources unless otherwise specified.

[0039] Preparation Example 1

[0040] The preparation method of acetylated sodium hyaluronate is as follows:

[0041] Prepare 1000 kDa hyaluronic acid, a mixed solvent of acetic acid and acetic anhydride in a mass ratio of 1:2.5, a catalyst of triethylamine and 4-dimethylaminopyridine in a mass ratio of 1:4, and a 5% sodium bicarbonate solution;

[0042] Add 10 kg of hyaluronic acid to 300 kg of mixed solvent and mix by stirring equipment. At a temperature of 25°C, add 6.2 kg of catalyst and perform acylation reaction. When the reaction solution is completely transparent, the reaction is complete.

[0043] The completely transparent reaction liquid was added to 500 kg of deionized water for standing precipitation, and the fibrous precipitate was collected by filter screen, and the precipitate was washed with deionized water to obtain acetylated hyaluronic acid;

[0044] The pH value of the obtained acetylated hyaluronic acid was adjusted using a sodium bicarbonate solution to make the pH value of the acetylated hyaluronic acid neutral, and the acetylated hyaluronic acid sodium was diluted to a concentration of 30 mL / g with deionized water and then filtered through a filter screen to remove large particles of 0.5 mm or more. Spray drying was performed using a spray drying device with an inlet temperature of 150°C and an outlet temperature of 100°C.

[0045] Preparation Example 2

[0046] The preparation method of acetylated hyaluronic acid is different from that of Preparation Example 1 in that 10 kg of hyaluronic acid is added to 200 kg of mixed solvent.

[0047] Preparation Example 3

[0048] The preparation method of acetylated hyaluronic acid is different from that of Preparation Example 1 in that 10 kg of hyaluronic acid is added to 400 kg of mixed solvent.

[0049] Preparation Example 4

[0050] The preparation method of acetylated hyaluronic acid is different from that of Preparation Example 1 in that 10 kg of hyaluronic acid is added to 100 kg of mixed solvent.

[0051] Preparation Example 5

[0052] The preparation method of acetylated hyaluronic acid is different from that of Preparation Example 1 in that 10 kg of hyaluronic acid is added to 500 kg of mixed solvent.

[0053] Preparation Example 6

[0054] The preparation method of microencapsulated calcium sulfate is as follows:

[0055] 4 kg of nano calcium sulfate powder was added to 15 kg of 30 wt% polylactic acid solution, mixed using 28 KHz ultrasonic vibration for 5 min, transferred to an emulsification reaction kettle, stirred at 80°C at 70 r / min, emulsified for 50 min, and the emulsified microcapsule suspension was placed in 20 kg of acetone, and the solidification time was controlled at 2 h. After solidification, microencapsulated calcium sulfate was separated by centrifuge, and the microencapsulated calcium sulfate was washed with deionized water.

[0056] Preparation Example 7

[0057] The preparation method of the microencapsulated calcium sulfate is: different from the preparation example 6, 4kg of nano calcium sulfate powder is added into 15kg of 20wt% polylactic acid solution.

[0058] Preparation example 8

[0059] The preparation method of the microencapsulated calcium sulfate is: different from the preparation example 6, 4kg of nano calcium sulfate powder is added into 15kg of 40wt% polylactic acid solution.

[0060] Preparation example 9

[0061] The preparation method of the microencapsulated calcium sulfate is: different from the preparation example 6, 4kg of nano calcium sulfate powder is added into 15kg of 10wt% polylactic acid solution.

[0062] Preparation example 10

[0063] The preparation method of the microencapsulated calcium sulfate is: different from the preparation example 6, 4kg of nano calcium sulfate powder is added into 15kg of 50wt% polylactic acid solution.

[0064] Example 1

[0065] A preparation method of a composite with water-locking film-forming and multi-channel soothing repair:

[0066] After 84.25kg of deionized water, 5kg of glycerol, 10kg of moisturizing agent, 0.2kg of disodium ethylenediaminetetraacetate, and 0.2kg of polyquaternium-51 are mixed in a reaction kettle, heating to 82℃ and continuously stirring at 80r / min until completely dissolved to obtain component A;

[0067] Cool the component A in the reaction kettle to 42℃, and then add component B, component C into component A in sequence and fully stir by a stirrer at 60r / min to obtain a mixed solution, component B includes 0.1kg of menthol, 0.1kg of hydrogenated castor oil, 0.05kg of sour cherry blossom extract and 0.05kg of bitter orange blossom hydrolat, and component C includes 0.05kg of preservative;

[0068] Discharge when the mixed solution is cooled to 30℃ to obtain a composite with water-locking film-forming and multi-channel soothing repair; wherein the moisturizing agent includes 4.3kg of sodium hyaluronate, 2.8kg of pullulan, 2kg of serine, and 0.9kg of sodium alginate; the preservative is selected from decanoic acid triglyceride.

[0069] Example 2

[0070] A method for preparing a complex having water-locking film-forming and multi-channel soothing repair: different from example 1 is that the humectant includes sodium hyaluronate 3.3 kg, pullulan 2.2 kg, serine 1.5 kg, 0.6 kg sodium alginate, acetylated sodium hyaluronate 2.4 kg, acetylated sodium hyaluronate is prepared from preparation example 1.

[0071] Example 3

[0072] A method for preparing a complex having water-locking film-forming and multi-channel soothing repair: different from example 2 is that the humectant includes sodium hyaluronate 3.3 kg, pullulan 2.2 kg, serine 1.5 kg, 0.6 kg sodium alginate, acetylated sodium hyaluronate 2.4 kg, acetylated sodium hyaluronate is prepared from preparation example 2.

[0073] Example 4

[0074] A method for preparing a complex having water-locking film-forming and multi-channel soothing repair: different from example 2 is that the humectant includes sodium hyaluronate 3.3 kg, pullulan 2.2 kg, serine 1.5 kg, 0.6 kg sodium alginate, acetylated sodium hyaluronate 2.4 kg, acetylated sodium hyaluronate is prepared from preparation example 3.

[0075] Example 5

[0076] A method for preparing a complex having water-locking film-forming and multi-channel soothing repair: different from example 2 is that the humectant includes sodium hyaluronate 3 kg, pullulan 2 kg, serine 1 kg, 0.4 kg sodium alginate, acetylated sodium hyaluronate 2 kg, trehalose 1.2 kg and carrageenan oligosaccharide 0.4 kg.

[0077] Example 6

[0078] A method for preparing a complex having water-locking film-forming and multi-channel soothing repair:

[0079] After mixing 82.35 kg of deionized water, 5 kg of glycerol, 10 kg of humectant, 0.2 kg of disodium ethylenediaminetetraacetate, and 0.2 kg of polyquaternary salt-51 in a reaction kettle, heat to 82°C and continue to stir at a speed of 80 r / min until completely dissolved to obtain component A;

[0080] Cool component A in the reaction kettle to 42°C, and then add component B and component C to component A in sequence and fully stir through a stirrer at a speed of 60 r / min to obtain a mixed solution, component B includes 0.1 kg of menthol, 0.1 kg of hydrogenated castor oil, 0.05 kg of sour cherry blossom extract and 0.05 kg of bitter orange blossom hydrolat, and component C includes 0.05 kg of preservative and 2 kg of microencapsulated calcium sulfate;

[0081] The mixture is cooled to 30℃ and discharged to obtain a complex with water-locking film-forming and multi-channel soothing repair. Among them, the humectant includes sodium hyaluronate 3 kg, pullulan 2 kg, serine 1 kg, 0.4 kg sodium alginate, acetylated sodium hyaluronate 2 kg, trehalose 1.2 kg and carrageenan oligosaccharide 0.4 kg, acetylated sodium hyaluronate is prepared from Preparation Example 1, microencapsulated calcium sulfate is prepared from Preparation Example 6, and the preservative is selected from decanoic acid triglyceride.

[0082] Example 7

[0083] A method for preparing a complex with water-locking film-forming and multi-channel soothing repair: different from Example 6 is that the microencapsulated calcium sulfate is prepared from Preparation Example 7.

[0084] Example 8

[0085] A method for preparing a complex with water-locking film-forming and multi-channel soothing repair: different from Example 6 is that the microencapsulated calcium sulfate is prepared from Preparation Example 8.

[0086] Comparative Example 1

[0087] A method for preparing a complex with water-locking film-forming and multi-channel soothing repair: different from Example 1 is that polyquaternium-51 is not added.

[0088] Comparative Example 2

[0089] A method for preparing a complex with water-locking film-forming and multi-channel soothing repair: different from Example 1 is that disodium ethylenediaminetetraacetate is not added.

[0090] Comparative Example 3

[0091] A method for preparing a complex with water-locking film-forming and multi-channel soothing repair: different from Example 5 is that the humectant includes sodium hyaluronate 3 kg, pullulan 2 kg, serine 1 kg, 0.4 kg sodium alginate, acetylated sodium hyaluronate 2 kg, 0.4 kg trehalose and carrageenan oligosaccharide 1.2 kg.

[0092] Comparative Example 4

[0093] A method for preparing a complex with water-locking film-forming and multi-channel soothing repair: different from Example 6 is that acetylated sodium hyaluronate is prepared from Preparation Example 4.

[0094] Comparative Example 5

[0095] A method for preparing a complex with water-locking film-forming and multi-channel soothing repair: different from Example 6 is that acetylated sodium hyaluronate is prepared from Preparation Example 5.

[0096] Comparative Example 6

[0097] A method for preparing a complex with water-locking film formation and multi- pass soothing repair: the difference from Example 6 is that the microencapsulated calcium sulfate is prepared from Preparation Example 9.

[0098] Comparative Example 7

[0099] A method for preparing a complex with water-locking film formation and multi- pass soothing repair: the difference from Example 6 is that the microencapsulated calcium sulfate is prepared from Preparation Example 10.

[0100] Comparative Example 8

[0101] A method for preparing a complex with water-locking film formation and multi- pass soothing repair: the difference from Example 6 is that menthol and hydrogenated castor oil are not added.

[0102] Comparative Example 9

[0103] A method for preparing a complex with water-locking film formation and multi- pass soothing repair: the difference from Example 6 is that Prunus cerasus flower extract is not added.

[0104] Comparative Example 10

[0105] A method for preparing a complex with water-locking film formation and multi- pass soothing repair: the difference from Example 6 is that bitter orange flower hydrolate is not added.

[0106] Detection method

[0107] A total of 30 volunteers with dry skin on the flexor side of the forearm were randomly selected to participate in the test. The samples prepared in the examples and comparative examples were used on the same skin area in turns, and the skin moisture content of the flexor side of the forearm test area was tested before and 0.5h, 1h, 2h, 4h after the sample was used. The interval time for testing the next sample was 24h.

[0108] Table 1 Water content test

[0109] A 10% lactic acid solution was applied to the nasolabial folds of the volunteers on both sides. After the irritation score reached 2 points (moderate), the staff applied the sample to the same position. The discomfort score was recorded at 0min (immediately after application), 2min, 5min, 8min and 10min after the sample was applied.

[0110] Table 2 Itching test

[0111] Table 3 Pricking test

[0112] After using the product, the cooling sensation was self-evaluated at 0 min, 5 min, 10 min, and 20 min, with a score of 1-5 points. The higher the score, the more obvious the cooling sensation.

[0113] Table 4 Cooling sensation test

[0114] Human keratinocytes were co-cultured with the compositions obtained in Example 6 and Comparative Examples 9-10 for 2 hours, and then irradiated with 410-470 nm blue light for 30 minutes at 20 mW / cm2. Then the damaged condition of DNA was exhibited by microelectrophoresis.

[0115] Table 5 Anti-photoaging test

[0116] As can be seen from the combination of Example 1 and Comparative Examples 1-2 and Tables 1-4, the moisturizing agent can be complexed with the polyquaternary ammonium salt on the surface of the skin to form a complex film, which not only locks the water in the skin and effectively inhibits the evaporation and loss of skin moisture, but also prevents the drying effect of the external environment on the skin. The addition of disodium ethylenediaminetetraacetate can stabilize the polyquaternary ammonium salt, reduce its agglomeration and precipitation, and prevent the complex from causing container blockage during use, while also having a slight anti-inflammatory and soothing effect.

[0117] As can be seen from the combination of Example 5 and Comparative Example 3 and Table 1, after carrageenan oligosaccharide and trehalose are compounded at a mass ratio of 1:(2-4), a higher moisturizing effect can be achieved to provide long-term moisturizing and hydration to the skin. After acetylated hyaluronic acid is compounded with carrageenan oligosaccharide, both will play a moisturizing role together to provide long-lasting moisturizing to the skin.

[0118] As can be seen from the combination of Examples 3, 4, 7, 8 and Comparative Examples 4-7 and Table 1, the sodium acetylated hyaluronic acid prepared in Preparation Example 1 has the best moisturizing effect when added to the composition. The microencapsulated calcium sulfate prepared in Preparation Example 6 has the best film-forming and moisturizing effect when added to the composition.

[0119] As can be seen from the combination of Example 6 and Comparative Example 8 and Table 4, menthol can bring a cooling sensation and has the effect of soothing skin irritation and reducing redness. The lubricity and moisturizing property of hydrogenated castor oil can improve the skin's absorption capacity, allowing menthol to penetrate deeper into the skin and exert its soothing effect. The combination of the lubricating and moisturizing properties of hydrogenated castor oil and the cooling sensation of menthol allows the cooling effect to be continuously stimulated without causing a stinging or uncomfortable sensation.

[0120] It can be seen from the combination of Example 6 and Comparative Examples 9-10 and Table 5 that by adding the European sour cherry flower extract and bitter orange flower hydrolat, the antioxidant ingredients in the European sour cherry flower extract can scavenge free radicals, reduce the negative effects of light damage on the skin, and protect the skin from blue light damage. The bitter orange flower hydrolat is rich in various antioxidants such as flavonoids. These antioxidants can scavenge free radicals and reduce the damage of external factors such as ultraviolet light to the skin, thereby resisting photoaging.

[0121] The specific embodiments are merely illustrative of the present application, and are not intended to limit the present application. Those skilled in the art can make modifications to the embodiments according to the needs without creative contribution, as long as the modifications are within the scope of the claims of the present application.

Claims

1. A complex having water-lock film formation and multi-passage soothing repair, characterized by: 0.1-15% glycerin, 0.1-25% humectant, 0.01-0.5% disodium ethylenediaminetetraacetate, 0.01-0.5% polyquaternary ammonium salt, 0.01-0.5% menthol, 0.01-2% hydrogenated castor oil, 0.01-2% preservative, 0.01-0.1% Prunus cerasus flower extract, and 0.01-0.1% bitter orange flower hydrolat, the rest being deionized water; the humectant comprises 10-20 parts by weight of sodium hyaluronate, 5-15 parts of pullulan, 5-10 parts of serine, and 1-5 parts of sodium alginate.

2. The compound having water-lock film-forming and multi-passage soothing repair according to claim 1, characterized in that: The humectant further comprises 5-15 parts by weight of acetylated sodium hyaluronate, and the preparation method of the acetylated sodium hyaluronate is as follows: The hyaluronic acid is added into a mixed solvent of acetic acid and acetic anhydride, stirred uniformly to obtain a reaction solution, 1-3% of a catalyst based on the total mass of the reaction solution is added at 5-40°C, and an acylation reaction is performed, and the reaction is ended when the reaction solution is completely transparent; the mass ratio of the hyaluronic acid to the mixed solvent of acetic acid and acetic anhydride is 1:(20-40), and the mass ratio of acetic acid to acetic anhydride is 1:(1.5-3.5); The completely transparent reaction solution is added into water for precipitation, the fibrous precipitate is collected and washed to obtain acetylated hyaluronic acid; The pH value of the acetylated hyaluronic acid is adjusted to neutral by using a 5% sodium bicarbonate solution, then the acetylated sodium hyaluronate is diluted to a concentration of 10-50 mL / g with deionized water, filtered, and then spray dried, with an inlet air temperature of 100-200°C and an outlet air temperature of 70-120°C.

3. The compound having water-lock film-forming and multi-passage soothing repair according to claim 2, characterized in that: The average degree of substitution of acetyl groups in the acetylated sodium hyaluronate is 3.0-3.3, and the catalyst comprises triethylamine and 4-dimethylaminopyridine at a mass ratio of 1:(3-5).

4. The compound having water-lock film formation and multi-pass comfort repair according to claim 2, characterized by: The humectant further comprises trehalose and carrageenan oligosaccharide, the mass ratio of the carrageenan oligosaccharide to the acetylated sodium hyaluronate is 1:(3.5-6.5), and the mass ratio of the carrageenan oligosaccharide to the trehalose is 1:(2-4).

5. The compound having water-lock film formation and multi-pass comfort repair according to claim 2, characterized by: The molecular weight of the hyaluronic acid is 500-2000 kDa.

6. The compound having water-lock film-forming and multi-passage soothing repair according to claim 1, characterized in that: Further comprising 1-3% of microencapsulated calcium sulfate by mass percentage, and the preparation method of the microencapsulated calcium sulfate is as follows: 30-50 parts by weight of nano calcium sulfate powder is added into 150 parts of a 20-40 wt% polylactic acid solution, mixed by using ultrasonic vibration, the mixed solution is transferred into an emulsification device, stirred at 75-85°C at a speed of 60-80 r / min, and emulsified for 40-60 min, the emulsified microcapsule suspension is solidified in acetone, after solidification, the microencapsulated calcium sulfate is obtained by centrifugal separation, and the microencapsulated calcium sulfate is washed with deionized water.

7. The compound having water-lock film-forming and multi-passage soothing repair according to claim 1, characterized in that: The preservative comprises one or more of decanoyl triglyceride, phenoxyethanol, and potassium sorbate.

8. Process for the preparation of a complex having water-locking film-forming and multi- passage soothing repair according to any one of claims 1 to 7, characterized in that: The method comprises the following steps: The deionized water, glycerin, humectant, disodium ethylenediaminetetraacetate, and polyquaternary ammonium salt are mixed, heated to 80-85°C, and stirred until completely dissolved to obtain component A; Cooling component A to 40-45℃, adding component B, component C into component A in turn, and stirring well to obtain a mixture, component B includes menthol, hydrogenated castor oil, Prunus cerasifera extract and bitter orange flower hydrolat, component C includes preservatives; Cooling the mixture to 35℃ or below to discharge, to obtain a complex with water-locking film-forming and multi-channel soothing repair.

9. The method for preparing the complex with water-locking film-forming and multi-pathway soothing and repairing properties according to claim 8, characterized in that: The component C further includes microencapsulated calcium sulfate.

10. Use of a complex having water-locking film-forming and multi-path soothing repair according to any one of claims 1 to 7, characterized in that: The complex with water-locking film-forming and multi-channel soothing repair is used for preparing skin care products, which are sprays, creams, lotions or serums.

Citation Information

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