Skin soothing and repairing agent based on hydroxyapatite microsphere composite material and preparation method of skin soothing and repairing agent

Abstract

The invention relates to the technical field of skin care products, and discloses a skin soothing and repairing agent based on a hydroxyapatite microsphere composite material and a preparation method thereof, the skin soothing and repairing agent comprises the following raw materials by weight: 0.75-1.95 parts of tetrahydromethylpyrimidine carboxylic acid; 0.25 to 0.75 part of bisabolol; 1 to 2.3 parts of nicotinamide; 5 to 15 parts of hydroxyapatite microspheres; the repairing agent is efficiently loaded and slowly released, the porous structure of the hydroxyapatite (HAP) microspheres can efficiently adsorb relieving active matter, long-acting slow release is achieved through physical adsorption, and instantaneous high-concentration stimulation is avoided.

Description

Technical Field

[0001] This invention relates to the field of skincare technology, and in particular to a skin soothing and repairing agent based on hydroxyapatite microsphere composite material and its preparation method. Background Technology

[0002] Soothing and repairing active ingredients are widely used in skincare products to address issues such as damaged skin barrier, sensitivity, and inflammation.

[0003] However, these active ingredients still face the following challenges in practical applications: 1. Low transdermal efficiency: Many soothing active ingredients (such as macromolecules or peptides) have difficulty effectively penetrating the stratum corneum, resulting in insufficient bioavailability; 2. Poor stability: Some components are easily degraded by environmental factors or become inactive during storage; 3. Risk of irritation: The rapid release of high concentrations of active ingredients may trigger skin intolerance and further cause adverse skin reactions.

[0004] Traditional transdermal enhancement technologies (such as liposomes, nanoemulsions, polymer microspheres, etc.) can partially improve the delivery efficiency of active ingredients, but they still have problems such as low loading rate, unstable sustained-release performance, or insufficient biocompatibility.

[0005] Therefore, there is an urgent need for a skin soothing and repairing agent based on hydroxyapatite microsphere composite materials and its preparation method to solve the above problems. Summary of the Invention

[0006] The purpose of this invention is to provide a skin soothing and repairing agent based on hydroxyapatite microsphere composite material and its preparation method.

[0007] The solution of the present invention is: A skin soothing and repairing agent based on hydroxyapatite microsphere composite material, comprising the following raw materials in parts by weight: 0.75–1.95 parts of tetrahydromethylpyrimidine carboxylic acid; Bisabolol 0.25–0.75 parts; Nicotinamide 1-2.3 parts; 5-15 parts of hydroxyapatite microspheres; The remainder is solvent.

[0008] As a preferred technical solution, the mass ratio of the hydroxyapatite microspheres, tetrahydromethylpyrimidine carboxylic acid, bisabolol and nicotinamide is 1-15:3-5:1-2:4-6.

[0009] As a preferred technical solution, the hydroxyapatite microspheres are porous hydroxyapatite microspheres with a particle size range of 25-50 μm, an average pore size of 63.18 Å, and a porosity controlled at 70%.

[0010] As a preferred technical solution, the mass ratio of tetrahydromethylpyrimidine carboxylic acid, bisabolol and nicotinamide is 4:1:5.

[0011] This invention also discloses a method for preparing a skin soothing and repairing agent based on hydroxyapatite microsphere composite material, comprising the following steps: 1) At 45°C, 0.25 to 0.75 parts by weight of bisabolol are dissolved in an organic solvent, wherein the organic solvent is cetearyl alcohol or cyclopentamethoxysiloxane, and the mass ratio of bisabolol to organic solvent is 1:10 to 20; to obtain a bisabolol solution; 2) Add 5-15 parts by weight of hydroxyapatite microspheres to the bisabolol solution, vortex mix for 1 min, shake in the dark for 6-15 h at a temperature of 35-39℃ and a shaking speed of 120-150 rpm / min to obtain loaded hydroxyapatite microspheres. 3) Dissolve 1-2.3 parts by weight of nicotinamide in PBS buffer, stir magnetically at 250-350 rpm for 8-12 min at 25-37°C until completely transparent to obtain a nicotinamide solution. Slowly add 0.75-1.95 parts by weight of tetrahydromethylpyrimidine carboxylic acid to the nicotinamide solution, and continue stirring at 180-220 rpm for 25-35 min. Protect from light, keep the ambient temperature ≤37°C, and maintain the pH at 6.5-7 to obtain a mixed solution. 4) Add the loaded hydroxyapatite microspheres to the mixed solution, vortex mix for 1 min, shake at 35-39°C in the dark at 100-150 rpm for 12 h, centrifuge at 8000 rpm for 10 min, remove the supernatant, and obtain the skin soothing and repairing agent based on the hydroxyapatite microsphere composite material.

[0012] As a preferred technical solution, in step 1), the organic solution is a mixture of anhydrous ethanol and propylene glycol, wherein the volume ratio of anhydrous ethanol to propylene glycol is 95:5, and the mass ratio of bisabolol to the organic solution is 1:15.

[0013] As a preferred technical solution, in step 2), the vibration is carried out in the dark for 12 hours at a temperature of 37°C and a rotation speed of 150 rpm / min.

[0014] As a preferred technical solution, in step 3), the magnetic stirring is performed at 300 rpm for 10 min until completely transparent to obtain a nicotinamide solution; 0.75 to 1.95 parts by weight of tetrahydromethylpyrimidine carboxylic acid is slowly added to the nicotinamide solution, and stirring is continued at 200 rpm for 30 min.

[0015] As a preferred technical solution, nicotinamide is used in PBS buffer at a concentration of 3-5% w / v, and tetrahydromethylpyrimidine carboxylic acid is used in PBS buffer at a concentration of 1-3% w / v.

[0016] This invention also discloses the application of a skin soothing and repairing agent based on hydroxyapatite microsphere composite material in skin care products and cosmetics.

[0017] Due to the adoption of the above technical solution, a skin soothing and repairing agent based on hydroxyapatite microsphere composite material comprises the following raw materials in parts by weight: 0.75-1.95 parts of tetrahydromethylpyrimidine carboxylic acid; 0.25-0.75 parts of bisabolol; 1-2.3 parts of nicotinamide; 5-15 parts of hydroxyapatite microspheres; and the balance being solvent.

[0018] Advantages of this invention: This invention provides a highly efficient loading and sustained-release repair agent. The porous structure of the hydroxyapatite microspheres efficiently adsorbs soothing active ingredients and achieves long-lasting sustained release through physical adsorption, avoiding instantaneous high-concentration irritation. When niacinamide is loaded onto the hydroxyapatite microspheres, its penetration efficiency can be increased by 2-3 times, while reducing the risk of redness caused by direct skin contact.

[0019] Hydroxyapatite enhances the stability of active ingredients by isolating photosensitive and oxygen-sensitive components (such as bisabolol) from their degradation, thus extending the shelf life of the formulation. It also slows down photodegradation and reduces the instantaneous irritation of chemical sunscreens through a sustained-release mechanism.

[0020] The synergistic repair mechanism: Hydroxyapatite itself is bioactive, and its calcium and phosphorus components can promote the migration of keratinocytes and accelerate barrier repair.

[0021] In this invention, hydroxyapatite microspheres, tetrahydromethylpyrimidine carboxylic acid, bisabolol and nicotinamide are used in combination to synergistically inhibit inflammatory factors and enhance the anti-allergic effect.

[0022] The hydroxyapatite microsphere-based soothing and repair system overcomes the limitations of traditional delivery technologies through a triple mechanism of "loading-slow release-synergistic repair," making it particularly suitable for long-term care of highly sensitive skin. This further expands its application prospects in anti-inflammatory and barrier repair fields. Detailed Implementation

[0023] To overcome the above deficiencies, the present invention provides a skin soothing and repairing agent based on hydroxyapatite microsphere composite material and its preparation method to solve the problems in the background art.

[0024] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below with reference to specific embodiments.

[0025] Example 1 A method for preparing a skin soothing and repairing agent based on hydroxyapatite microsphere composite material. 1) At 45℃, 0.25 parts by weight of bisabolol were dissolved in an organic solution, with a mass ratio of bisabolol to organic solution of 1:10; a bisabolol solution was obtained. 2) Add 5 parts by weight of hydroxyapatite microspheres to the bisabolol solution, vortex mix for 1 min, shake in the dark for 6 h at 35℃ and 120 rpm / min to obtain loaded hydroxyapatite microspheres. 3) Dissolve 1 part by weight of nicotinamide in PBS buffer, stir magnetically at 250 rpm for 8 min at 25°C until completely transparent to obtain a nicotinamide solution. Slowly add 0.75 parts by weight of tetrahydromethylpyrimidine carboxylic acid to the nicotinamide solution, continue stirring at 180 rpm for 25 min, protect from light, keep the ambient temperature ≤37°C, and the pH 6.5 to obtain a mixed solution. 4) Add the loaded hydroxyapatite microspheres to the mixed solution, vortex mix for 1 min, shake at 35°C in the dark at 100 rpm for 12 h, centrifuge at 8000 rpm for 10 min, remove the supernatant, and obtain the skin soothing and repairing agent based on the hydroxyapatite microsphere composite material.

[0026] The hydroxyapatite microspheres are porous hydroxyapatite microspheres with a particle size range of 25–50 μm, an average pore size of 63.18 Å, and a porosity controlled at 70%.

[0027] In step 1), the organic solution is anhydrous ethanol.

[0028] In step 2), the vibration is carried out in the dark for 12 hours at a temperature of 37°C and a rotation speed of 150 rpm / min.

[0029] Example 2 A method for preparing a skin soothing and repairing agent based on hydroxyapatite microsphere composite material: 1) At 45°C, 0.75 parts by weight of bisabolol were dissolved in an organic solution, with a mass ratio of bisabolol to organic solution of 1:20; a bisabolol solution was obtained. 2) Add 15 parts by weight of hydroxyapatite microspheres to the bisabolol solution, vortex mix for 1 min, shake in the dark for 15 h at 39℃ and 150 rpm / min to obtain loaded hydroxyapatite microspheres. 3) Dissolve 2.3 parts by weight of nicotinamide in PBS buffer, stir magnetically at 350 rpm for 12 min at 37°C until completely transparent to obtain a nicotinamide solution. Slowly add 1.95 parts by weight of tetrahydromethylpyrimidine carboxylic acid to the nicotinamide solution, continue stirring at 220 rpm for 35 min, protect from light, keep the ambient temperature ≤37°C, and the pH 7 to obtain a mixed solution. 4) Add the loaded hydroxyapatite microspheres to the mixed solution, vortex mix for 1 min, shake at 39°C in the dark at 150 rpm for 12 h, centrifuge at 8000 rpm for 10 min, remove the supernatant, and obtain the skin soothing and repairing agent based on the hydroxyapatite microsphere composite material.

[0030] The hydroxyapatite microspheres are porous hydroxyapatite microspheres with a particle size range of 25–50 μm, an average pore size of 63.18 Å, and a porosity controlled at 70%.

[0031] In step 1), the organic solution is anhydrous ethanol.

[0032] Example 3 A method for preparing a skin soothing and repairing agent based on hydroxyapatite microsphere composite material: 1) At 45°C, 0.5 parts by weight of bisabolol were dissolved in an organic solution, with a mass ratio of bisabolol to organic solution of 1:15; a bisabolol solution was obtained. 2) Add 10 parts by weight of hydroxyapatite microspheres to the bisabolol solution, vortex mix for 1 min, shake in the dark for 12 h at 37℃ and 150 rpm / min to obtain loaded hydroxyapatite microspheres. 3) Dissolve 2 parts by weight of nicotinamide in PBS buffer, stir magnetically at 300 rpm for 10 min at 35°C until completely transparent to obtain a nicotinamide solution. Slowly add 1 part by weight of tetrahydromethylpyrimidine carboxylic acid to the nicotinamide solution, continue stirring at 200 rpm for 30 min, protect from light, keep the ambient temperature ≤37°C, and the pH 6.5 to obtain a mixed solution. 4) Add the loaded hydroxyapatite microspheres to the mixed solution, vortex mix for 1 min, shake at 37°C in the dark for 12 rpm for 12 h, centrifuge at 8000 rpm for 10 min, remove the supernatant, and obtain the skin soothing and repairing agent based on the hydroxyapatite microsphere composite material.

[0033] In step 1), the organic solution is a mixture of anhydrous ethanol and propylene glycol, and the volume ratio of anhydrous ethanol to propylene glycol is 95:5.

[0034] The hydroxyapatite microspheres are porous hydroxyapatite microspheres with a particle size range of 25–50 μm, an average pore size of 63.18 Å, and a porosity controlled at 70%.

[0035] Example 4 1) At 45℃, bisabolol was dissolved in an organic solution at a mass ratio of 1:15 to bisabolol; a bisabolol solution was obtained. 2) Add the hydroxyapatite microspheres to the bisabolol solution, vortex mix for 1 min, shake in the dark for 12 h at 37℃ and 150 rpm / min to obtain the loaded hydroxyapatite microspheres. 3) Dissolve nicotinamide in PBS buffer, stir magnetically at 300 rpm for 10 min at 37°C until completely transparent to obtain a nicotinamide solution. Slowly add tetrahydromethylpyrimidine carboxylic acid to the nicotinamide solution, continue stirring at 200 rpm for 30 min, protect from light, keep the ambient temperature ≤37°C, and the pH 6.5 to obtain a mixed solution. 4) Add the loaded hydroxyapatite microspheres to the mixed solution, vortex mix for 1 min, shake at 37°C in the dark for 12 rpm for 12 h, centrifuge at 8000 rpm for 10 min, remove the supernatant, and obtain the skin soothing and repairing agent based on the hydroxyapatite microsphere composite material.

[0036] In step 1), the organic solution is a mixture of anhydrous ethanol and propylene glycol, and the volume ratio of anhydrous ethanol to propylene glycol is 95:5.

[0037] Nicotinamide was used at a concentration of 2% w / v in PBS buffer, and tetrahydromethylpyrimidine carboxylic acid was used at a concentration of 5% w / v in PBS buffer.

[0038] The mass ratio of the hydroxyapatite microspheres, tetrahydromethylpyrimidine carboxylic acid, bisabolol, and nicotinamide is 10:4:1:5.

[0039] The hydroxyapatite microspheres are porous hydroxyapatite microspheres with a particle size range of 25–50 μm, an average pore size of 63.18 Å, and a porosity controlled at 70%.

[0040] The product of Example 4 was subjected to skin soothing and skin irritation tests.

[0041] Soothing: If either the skin color (red-green) value (a*) or the lactic acid stinging score significantly decreased (P<0.050) before or after using the sample, the test sample is considered to have a soothing effect.

[0042] Skin color (red-green) value a* value test results

[0043] Compared to before sample use, after 28 days of sample use, the skin color (red-green) a* value of the 30 subjects showed a significant difference, with a change rate of -3.74% compared to the baseline value. This indicates that the test sample has a soothing effect after 28 days of use.

[0044] Repeated skin irritation: Apply approximately 0.5 mL of the test substance directly to one side of the skin, covering an area of ​​2.5 cm x 2.5 cm. When the test substance is prepared using a non-irritating solvent, apply the solvent to the other side as a control. Apply once daily for 14 consecutive days.

[0045] Lactic acid stinging score test results

[0046] Compared with before using the sample, after 28 days of use, the lactic acid stinging scores of the 30 subjects showed a significant difference, with a change rate of -29.17% compared with the baseline value. This indicates that the test sample has a soothing effect after 28 days of use.

[0047] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of this invention is defined by the appended claims and their equivalents.

Claims

1. A skin soothing and repairing agent based on hydroxyapatite microsphere composite material, characterized in that, The ingredients include the following parts by weight: 0.75–1.95 parts of tetrahydromethylpyrimidine carboxylic acid; Bisabolol 0.25–0.75 parts; Nicotinamide 1-2.3 parts; 5-15 parts of hydroxyapatite microspheres; The remainder is solvent.

2. The skin soothing and repairing agent based on hydroxyapatite microsphere composite material as described in claim 1, characterized in that: The mass ratio of the hydroxyapatite microspheres, tetrahydromethylpyrimidine carboxylic acid, bisabolol and nicotinamide is 1-15:3-5:1-2:4-6.

3. The skin soothing and repairing agent based on hydroxyapatite microsphere composite material as described in claim 1, characterized in that: The hydroxyapatite microspheres are porous hydroxyapatite microspheres with a particle size range of 25–50 μm, an average pore size of 63.18 Å, and a porosity controlled at 70%.

4. The skin soothing and repairing agent based on hydroxyapatite microsphere composite material as described in claim 2, characterized in that: The mass ratio of tetrahydromethylpyrimidine carboxylic acid, bisabolol, and nicotinamide is 4:1:

5.

5. A method for preparing a skin soothing and repairing agent based on hydroxyapatite microsphere composite material as described in any one of claims 1-4, characterized in that, Includes the following steps: 1) At 45°C, 0.25 to 0.75 parts by weight of bisabolol are dissolved in an organic solvent, wherein the organic solvent is cetearyl alcohol or cyclopentamethoxysiloxane, and the mass ratio of bisabolol to organic solvent is 1:10 to 20; to obtain a bisabolol solution; 2) Add 5-15 parts by weight of hydroxyapatite microspheres to the bisabolol solution, vortex mix for 1 min, shake in the dark for 6-15 h at a temperature of 35-39℃ and a shaking speed of 120-150 rpm / min to obtain loaded hydroxyapatite microspheres. 3) Dissolve 1-2.3 parts by weight of nicotinamide in PBS buffer, stir magnetically at 250-350 rpm for 8-12 min at 25-37°C until completely transparent to obtain a nicotinamide solution. Slowly add 0.75-1.95 parts by weight of tetrahydromethylpyrimidine carboxylic acid to the nicotinamide solution, and continue stirring at 180-220 rpm for 25-35 min. Protect from light, keep the ambient temperature ≤37°C, and maintain the pH at 6.5-7 to obtain a mixed solution. 4) Add the loaded hydroxyapatite microspheres to the mixed solution, vortex mix for 1 min, shake at 35-39°C in the dark at 100-150 rpm for 12 h, centrifuge at 8000 rpm for 10 min, remove the supernatant, and obtain the skin soothing and repairing agent based on the hydroxyapatite microsphere composite material.

6. The method for preparing a skin soothing and repairing agent based on hydroxyapatite microsphere composite material as described in claim 1, characterized in that: In step 1), the organic solution is a mixture of anhydrous ethanol and propylene glycol, with a volume ratio of 95:5 for anhydrous ethanol to propylene glycol and a mass ratio of 1:15 for bisabolol to the organic solution.

7. The preparation method of a skin soothing and repairing agent based on hydroxyapatite microsphere composite material as described in claim 1, characterized in that: In step 2), the vibration is carried out in the dark for 12 hours at a temperature of 37°C and a rotation speed of 150 rpm / min.

8. The method for preparing a skin soothing and repairing agent based on hydroxyapatite microsphere composite material as described in claim 1, characterized in that: In step 3), the magnetic stirring is performed at 300 rpm for 10 minutes until the solution becomes completely transparent, thus obtaining a nicotinamide solution. 0.75 to 1.95 parts by weight of tetrahydromethylpyrimidine carboxylic acid is then slowly added to the nicotinamide solution, and stirring is continued at 200 rpm for 30 minutes.

9. The method for preparing a skin soothing and repairing agent based on hydroxyapatite microsphere composite material as described in claim 1, characterized in that: Nicotinamide is used in PBS buffer at a concentration of 3–5% w / v, and tetrahydromethylpyrimidine carboxylic acid is used in PBS buffer at a concentration of 1–3% w / v.

10. The application of a skin soothing and repairing agent based on hydroxyapatite microsphere composite material as claimed in any one of claims 1-4 in skin care products and cosmetics.

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