Hydroxybutyl chitosan-based composite plant anti-inflammatory composite material and preparation method thereof

Abstract

The application discloses a hydroxybutyl chitosan-based composite plant anti-inflammatory composite material and a preparation method thereof. Relying on the unique temperature-sensitive phase change characteristics of HBCS, the phase change mechanism is triggered when contacting the skin, and sustained slow-release power is provided for anti-inflammatory repair components, so that the action time of the effective components is greatly prolonged. The application not only utilizes the direct anti-inflammatory signal inhibition effect of EGCG and spilanthes acmella, but also innovatively exerts the immunoregulatory activity of HBCS itself; HBCS can preliminarily modulate the receptor activity of macrophages and keratinocytes, and forms a complementary enhancement effect of 'pre-modulation and post-inhibition' with subsequent effective components, and finally realizes the strong anti-inflammatory and repair effect far beyond single component. The system realizes the synergistic anti-inflammatory effect of the carrier and the functional components through the removal of 'bad cells' by gynostemma pentaphyllum, the modification of 'good cells' by HBCS, the blockage of 'inflammatory signals' by EGCG combined with gynostemma pentaphyllum, and the maintenance of'system balance' by spilanthes acmella cooperated with gynostemma pentaphyllum.

Description

Technical Field

[0001] This invention belongs to the field of functional skincare technology, specifically relating to a hydroxybutyl chitosan-based composite plant anti-inflammatory material and its preparation method. Background Technology

[0002] As a highly effective localized skincare product, the formulation and carrier technology of facial masks directly impact the user experience and the effectiveness of their active ingredients. Thermosensitive hydrogels represent a cutting-edge drug delivery system, and their sol-gel transition properties can significantly enhance the product experience. Poloxamer is a commonly used synthetic thermosensitive material, but its biocompatibility, biodegradability, and tissue adhesion need improvement, and it primarily relies on physical encapsulation, limiting its interaction with active ingredients. The gels formed by such materials typically have weak mechanical strength and poor adhesion to skin and mucous membranes, making them prone to breakage or slippage during facial activities or in the presence of sweat, resulting in short-lasting occlusive effects and hindering the sustained penetration of active ingredients. Summary of the Invention

[0003] To address the technical bottlenecks in the application of existing thermosensitive hydrogels in skincare products, such as low phase transition temperature matching, insufficient mechanical stability, and limited biocompatibility, this application proposes a hydroxybutyl chitosan-based composite plant anti-inflammatory composite material and its preparation method.

[0004] This invention introduces hydroxybutyl chitosan (HBCS) into a temperature-sensitive composite material, and simultaneously constructs a ternary synergistic anti-inflammatory system with epigallocatechin gallate (EGCG), centella asiatica extract, and purslane extract. The product is a spreadable sol at room temperature, which rapidly transforms into a viscoelastic gel upon contact with the skin, adhering tightly and releasing active ingredients for a long time, achieving excellent soothing, redness-reducing, and barrier-repairing effects.

[0005] The HBCS and EGCG complex system achieves a significant enhancement in anti-inflammatory and repairing effects by constructing a full-link mechanism of "steady-state maintenance—efficient delivery—synergistic efficacy." Leveraging its unique temperature-sensitive phase transition properties, this system provides sustained-release power during application, not only extending the duration of action of active ingredients but also ensuring long-lasting release of the active components. Secondly, regarding the penetration-enhancing mechanism, HBCS's excellent adhesion and moisturizing properties soften the stratum corneum and assist in opening pores, significantly increasing skin permeability and forming a highly efficient "penetration-enhancing" channel. This greatly improves the transdermal delivery efficiency of effective components, ensuring that active ingredients reach the target site directly. Finally, in terms of enhanced anti-inflammatory effects, this system forms a unique intracellular complementary mechanism: First, Centella asiatica induces ferroptosis in M1 pro-inflammatory macrophages, directly reducing the number of inflammatory cells at the root. Then, HBCS drives immune microenvironment remodeling, guiding macrophages towards M2 anti-inflammatory epipolarization, optimizing local anti-inflammatory sensitivity, and creating a microenvironment conducive to repair. Simultaneously, EGCG and Centella asiatica synergistically block inflammatory signaling pathways; EGCG inhibits the NF-κB / p38 MAPK pathway and the NLRP3 inflammasome, while Centella asiatica targets the STAT3 / IL-23 / IL-17 axis and regulates the JAK2 / STAT3 pathway, thus interrupting key inflammatory cascade responses through a dual-pathway approach. Finally, Portulaca oleracea and Centella asiatica work together to regulate systemic immune homeostasis; Portulaca oleracea inhibits TNF-α / ICAM-1 expression to maintain the macrophage activation-inhibition balance, while Centella asiatica regulates the Th17 / Treg ratio, thereby restoring adaptive immune homeostasis and preventing inflammatory recurrence.

[0006] One of the technical solutions of the present invention is to provide a hydroxybutyl chitosan-based composite plant anti-inflammatory composite material, comprising hydroxybutyl chitosan, epigallocatechin gallate, centella asiatica extract, purslane extract, moisturizer, and skin barrier repair agent.

[0007] Furthermore, the mass ratio of the hydroxybutyl chitosan, moisturizer, and skin barrier repair agent is 1-10:5-12:1-4.

[0008] Furthermore, the mass ratio of epigallocatechin gallate, Centella asiatica extract, and Portulaca oleracea extract is (0.5-1.5):(1-3):(1-3).

[0009] Furthermore, the mass ratio of the epigallocatechin gallate, centella asiatica extract, and purslane extract is 1:2:2. Furthermore, the mass ratio of the hydroxybutyl chitosan to the total mass of epigallocatechin gallate, centella asiatica extract, and purslane extract is 1-10:2-7.

[0010] Furthermore, the degree of substitution of hydroxybutyl chitosan is 0.5-1.2.

[0011] Furthermore, it also includes a preservative, which is one or more of p-hydroxyacetophenone, 1,2-hexanediol, and octyl glycol.

[0012] Furthermore, the moisturizer is one or more of glycerin, dipropylene glycol, panthenol, and sodium hyaluronate.

[0013] Furthermore, the skin barrier repair agent is one or more of ceramide NP, squalane, bisabolol, and ectoine.

[0014] The second technical solution of the present invention is to provide a method for preparing the above-mentioned hydroxybutyl chitosan-based composite plant anti-inflammatory composite material, comprising the following steps: (1) Mix epigallocatechin gallate, centella asiatica extract, purslane extract, moisturizer, and skin barrier repair agent evenly, and stir in a water bath at 45°C for 30 minutes to obtain a uniform active phase A; (2) Add the uniform active phase A to the aqueous solution of hydroxybutyl chitosan and stir until homogeneous; (3) Add preservatives, homogenize and then vacuum degas for 30 minutes to obtain hydroxybutyl chitosan-based composite plant anti-inflammatory composite material.

[0015] In the hydroxybutyl chitosan-based composite plant anti-inflammatory material, epigallocatechin gallate, centella asiatica extract, and purslane extract account for 2-7% of the total mass, hydroxybutyl chitosan accounts for 1-10% of the total mass, moisturizer accounts for 5-12% of the total mass, skin barrier repair agent accounts for 1-4% of the total mass, preservative accounts for 0.1-0.5% of the total mass, and the balance is water; among them, the water in the aqueous solution of hydroxybutyl chitosan accounts for 80% of the total water content of the hydroxybutyl chitosan-based composite plant anti-inflammatory material.

[0016] The advantages of this invention are: This invention significantly improves the stability of active ingredients and achieves intelligent, long-lasting sustained release. The active ingredients are dissolved in water with hydroxybutyl chitosan to form a solution. Utilizing the thermosensitive properties of hydroxybutyl chitosan, the solution transforms into a gel state upon application to the face. Simultaneously, leveraging the unique thermosensitive phase change properties of HBCS, a phase change mechanism is triggered upon skin contact, providing sustained release power for the anti-inflammatory and repairing ingredients, thereby significantly extending the duration of action of the active ingredients.

[0017] This invention not only utilizes the direct anti-inflammatory signaling inhibition effects of EGCG and purslane, but also innovatively leverages the immunomodulatory activity of HBCS itself. HBCS can initially modulate the receptor activity of macrophages and keratinocytes, putting cells in a "sensitized" state that is more sensitive to inflammation suppression. This, in turn, creates a complementary and synergistic effect of "modulation followed by inhibition" with subsequent effective components, ultimately achieving a powerful anti-inflammatory and repairing effect far exceeding that of a single component. This system achieves synergistic anti-inflammatory effects through Centella asiatica clearing "bad cells," HBCS modifying "good cells," EGCG combined with Centella asiatica blocking "inflammatory signals," and purslane synergistically maintaining "system balance" with Centella asiatica. Attached Figure Description

[0018] Figure 1 This is a rheological test diagram of Example 1.

[0019] Figure 2 This is a diagram illustrating the anti-inflammatory effect of Example 1. Detailed Implementation

[0020] The following examples are provided to further illustrate the present invention and are intended to explain the invention, not to limit its scope. Unless otherwise specified, all figures are expressed in parts by weight and weight percentages.

[0021] Unless otherwise specified, the raw materials used in this invention are all conventional commercially available products; unless otherwise specified, the methods used in this invention are all conventional methods in the field.

[0022] The embodiments of the present invention will be further described below with reference to several examples.

[0023] It should be understood that the described embodiments are merely some, not all, of the embodiments in this application. All other embodiments obtained by those skilled in the art based on the embodiments in this application without inventive effort are within the scope of protection of this application.

[0024] The terminology used in the embodiments of this application is for the purpose of describing particular embodiments only and is not intended to be limiting of this application. The singular forms “a,” “the,” and “the” used in the embodiments of this application and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise.

[0025] Example 1 (1) Mix EGCG, Centella asiatica extract, Portulaca oleracea extract, glycerin, panthenol and ceramide NP, and stir in a water bath at 45°C for 30 minutes to obtain a uniform active phase A.

[0026] (2) Measure about 80% of the total amount of deionized water and slowly sprinkle HBCS powder into it while stirring at 800 rpm. After adding the powder, increase the speed to 1000 rpm and stir at room temperature until completely dissolved to obtain clear solution B.

[0027] (3) Slowly add active phase A to solution B and stir at 1000 rpm for 20 minutes at room temperature to make it evenly mixed.

[0028] (4) Add 1,2-hexanediol and make up the weight with the remaining deionized water. Homogenize at 1500 rpm for 3 minutes at <25°C.

[0029] (5) Degas the obtained sol under vacuum for 30 minutes, fill it into dark sample bottles, and store it in a cool place.

[0030] Its composition by weight percentage is as follows: Hydroxybutyl chitosan (HBCS, degree of substitution 0.8): 8% EGCG: 0.5% Centella asiatica extract (containing 30% asiaticoside): 1.0% Purslane extract: 1.0% Glycerin: 5.0% Panthenol: 2.0% Ceramide NP: 1% 1,2-Hexanediol: 0.5% Deionized water: Top up to 100%.

[0031] The gelation time and gelation condition (transformation into a non-flowing gel, which does not flow when inverted) of the product in Test Example 1 under water bath conditions of 30℃, 35℃, 40℃, 45℃, and 50℃ are shown in the table below.

[0032] Table 1. Gel formation time of Example 1 at different temperatures Example 2 (1) Mix EGCG, Centella asiatica extract, Portulaca oleracea extract, glycerin and ceramide NP, and stir in a water bath at 45°C for 30 minutes to obtain a uniform active phase A.

[0033] (2) Measure about 80% of the total amount of deionized water and slowly sprinkle HBCS powder into it while stirring at 800 rpm. After adding the powder, increase the speed to 1000 rpm and stir at room temperature until completely dissolved to obtain clear solution B.

[0034] (3) Slowly add active phase A to solution B and stir at 1000 rpm for 20 minutes at room temperature to make it evenly mixed.

[0035] (4) Add 1,2-hexanediol and make up the weight with the remaining deionized water. Homogenize at 1500 rpm for 3 minutes at <25°C.

[0036] (5) Degas the obtained sol under vacuum for 30 minutes, fill it into dark sample bottles, and store it in a cool place.

[0037] Its composition by weight percentage is as follows: Hydroxybutyl chitosan (HBCS, degree of substitution 0.8): 10% EGCG: 1% Centella asiatica extract (containing 30% asiaticoside): 3.0% Purslane extract: 3.0% Glycerin: 5.0% Ceramide NP: 4% 1,2-Hexanediol: 0.5% Deionized water: Top up to 100%.

[0038] Example 3 (1) Mix EGCG, Centella asiatica extract, Portulaca oleracea extract, glycerin and squalane, and stir in a water bath at 45°C for 30 minutes to obtain a uniform active phase A.

[0039] (2) Measure about 80% of the total amount of deionized water and slowly sprinkle HBCS powder into it while stirring at 800 rpm. After adding the powder, increase the speed to 1000 rpm and stir at room temperature until completely dissolved to obtain clear solution B.

[0040] (3) Slowly add active phase A to solution B and stir at 1000 rpm for 20 minutes at room temperature to make it evenly mixed.

[0041] (4) Add 1,2-hexanediol and make up the weight with the remaining deionized water. Homogenize at 1500 rpm for 3 minutes at <25°C.

[0042] (5) Degas the obtained sol under vacuum for 30 minutes, fill it into dark sample bottles, and store it in a cool place.

[0043] Its composition by weight percentage is as follows: Hydroxybutyl chitosan (HBCS, degree of substitution 1.2): 1% EGCG: 1% Centella asiatica extract (containing 30% asiaticoside): 1.0% Purslane extract: 1.0% Glycerin: 12.0% Squalane: 2% 1,2-Hexanediol: 0.1% Deionized water: Top up to 100%.

[0044] The composite plant anti-inflammatory material (HBCS+EGCG+Centella asiatica+Portulaca oleracea) provided by this invention achieves comprehensive anti-inflammatory repair from the cellular level to the systemic immune system through a four-layer synergistic mechanism: The first layer involves cell source clearance, primarily driven by Centella asiatica, which induces ferroptosis in M1 pro-inflammatory macrophages, directly reducing the number of inflammatory cells at the root. The second layer involves immune microenvironment remodeling, driven by HBCS, guiding macrophages towards M2 anti-inflammatory epipolarization, optimizing local "anti-inflammatory sensitivity," and creating a microenvironment conducive to repair. The third layer involves blocking inflammatory signaling pathways, synergistically achieved by EGCG and Centella asiatica—EGCG inhibits the NF-κB / p38 MAPK pathway and the NLRP3 inflammasome, while Centella asiatica targets the STAT3 / IL-23 / IL-17 axis and regulates the JAK2 / STAT3 pathway, thus blocking key inflammatory cascade reactions through dual pathways. The fourth layer involves systemic immune homeostasis regulation, jointly achieved by Portulaca oleracea and Centella asiatica—Portulaca oleracea inhibits TNF-α / ICAM-1 expression to maintain the "activation-inhibition" balance of macrophages, while Centella asiatica regulates the Th17 / Treg ratio, thereby restoring adaptive immune homeostasis and preventing inflammation recurrence.

[0045] This four-layer architecture is progressive and multi-targeted, which not only quickly controls acute inflammation, but also focuses on long-term immune balance and comprehensively improves the skin's anti-inflammatory and repair capabilities.

[0046] Comparative Example 1 The anti-inflammatory essence components, by weight percentage, are as follows: EGCG: 0.5% Centella asiatica extract (containing 30% asiaticoside): 1.0% Purslane extract: 1.0% Glycerin: 5.0% Panthenol: 2.0% Ceramide NP: 0.5% 1,2-Hexanediol: 0.6% Deionized water: Replenish to 100% Preparation method: (1) Mix EGCG, Centella asiatica extract, Portulaca oleracea extract, glycerin, panthenol and ceramide NP, and stir in a water bath at 45°C for 30 minutes; (2) Add 1,2-hexanediol and make up the weight with the remaining deionized water. Homogenize at 1500 rpm for 3 minutes at <25°C.

[0047] (3) Degas the obtained sol under vacuum for 30 minutes, fill it into dark sample bottles, and store it in a cool place.

[0048] Comparative Example 2 Thermosensitive matrix gel component, its composition by weight percentage is as follows: Hydroxybutyl chitosan (HBCS, degree of substitution 0.8): 8% Glycerin: 5.0% Panthenol: 2.0% Ceramide NP: 0.5% 1,2-Hexanediol: 0.6% Deionized water: Replenish to 100% Preparation method: (1) Mix glycerol, panthenol and ceramide NP, stir in a water bath at 45°C for 30 minutes to obtain a uniform active phase A.

[0049] (2) Measure about 80% of the total amount of deionized water and slowly sprinkle HBCS powder into it while stirring at 800 rpm. After adding the powder, increase the speed to 1000 rpm and stir at room temperature until completely dissolved to obtain clear solution B.

[0050] (3) Slowly add active phase A to solution B and stir at 1000 rpm for 20 minutes at room temperature to make it evenly mixed.

[0051] (4) Add 1,2-hexanediol and make up the weight with the remaining deionized water. Homogenize at 1500 rpm for 3 minutes at <25°C.

[0052] (5) Degas the obtained sol under vacuum for 30 minutes, fill it into dark sample bottles, and store it in a cool place.

[0053] The TNF-α inhibition rate of Comparative Example 1 (anti-inflammatory essence component) was 37.6%; The TNF-α inhibition rate of Comparative Example 2 (thermosensitive matrix gel component) was 5.6%; The inhibition rate of TNF-α in Example 1 was significantly increased (47.8%), and the anti-inflammatory effect was further enhanced by the synergy between the carrier and the active ingredient, which verified the "innovative synergistic mechanism of carrier and active ingredient in the technical breakthrough".

[0054] Comparative Example 3 The difference from Example 1 is that hydroxybutyl chitosan was replaced with hydroxypropyl chitosan. Experiments showed that the TNF-α inhibition rate of the prepared composite material was reduced to approximately 40%, indicating that hydroxypropyl chitosan could not achieve a synergistic effect.

[0055] The above embodiments describe in detail the structure, features, and effects of the present invention. The above description is only a preferred embodiment of the present invention. Any changes made in accordance with the concept of the present invention, or equivalent embodiments modified to have equivalent changes, shall still fall within the scope of protection of the present invention if they do not exceed the scope covered by the specification.

Claims

1. A hydroxybutyl chitosan-based composite plant anti-inflammatory material, characterized in that, Including hydroxybutyl chitosan, epigallocatechin gallate, centella asiatica extract, purslane extract, moisturizer, and skin barrier repair agent.

2. The hydroxybutyl chitosan-based composite plant anti-inflammatory composite material according to claim 1, characterized in that, The mass ratio of the hydroxybutyl chitosan, moisturizer, and skin barrier repair agent is (1-10):(5-12):(1-4).

3. The hydroxybutyl chitosan-based composite plant anti-inflammatory composite material according to claim 1, characterized in that, The mass ratio of the epigallocatechin gallate, Centella asiatica extract, and Portulaca oleracea extract is (0.5-1.5):(1-3):(1-3).

4. The hydroxybutyl chitosan-based composite plant anti-inflammatory composite material according to claim 1, characterized in that, The mass ratio of the epigallocatechin gallate, centella asiatica extract, and purslane extract is 1:2:

2.

5. The hydroxybutyl chitosan-based composite plant anti-inflammatory composite material according to claim 1, characterized in that, The mass ratio of the hydroxybutyl chitosan to the total mass of epigallocatechin gallate, centella asiatica extract, and purslane extract is (1-10):(2-7).

6. The hydroxybutyl chitosan-based composite plant anti-inflammatory composite material according to claim 1, characterized in that, The degree of substitution of hydroxybutyl chitosan is 0.5-1.

2.

7. The hydroxybutyl chitosan-based composite plant anti-inflammatory composite material according to claim 1, characterized in that, It also includes preservatives, which are one or more of p-hydroxyacetophenone, 1,2-hexanediol, and octyl glycol.

8. The hydroxybutyl chitosan-based composite plant anti-inflammatory composite material according to claim 1, characterized in that, The moisturizer is one or more of glycerin, dipropylene glycol, panthenol, and sodium hyaluronate; the skin barrier repair agent is one or more of ceramide NP, squalane, bisabolol, and ectoine.

9. A method for preparing the hydroxybutyl chitosan-based composite plant anti-inflammatory composite material as described in claim 1, characterized in that, It includes the following steps: (1) Mix epigallocatechin gallate, centella asiatica extract, purslane extract, moisturizer, and skin barrier repair agent evenly, and stir in a water bath at 45°C for 30 minutes to obtain a uniform active phase A; (2) Add the uniform active phase A to the aqueous solution of hydroxybutyl chitosan and stir until homogeneous; (3) Add preservatives, homogenize and then vacuum degas for 30 minutes to obtain hydroxybutyl chitosan-based composite plant anti-inflammatory composite material.

10. The method according to claim 9, characterized in that, In the hydroxybutyl chitosan-based composite plant anti-inflammatory material, epigallocatechin gallate, centella asiatica extract, and purslane extract account for 2-7% of the total mass, hydroxybutyl chitosan accounts for 1-10% of the total mass, moisturizer accounts for 5-12% of the total mass, skin barrier repair agent accounts for 1-4% of the total mass, preservative accounts for 0.1-0.5% of the total mass, and the balance is water; among them, the water in the aqueous solution of hydroxybutyl chitosan accounts for 80% of the total water content of the hydroxybutyl chitosan-based composite plant anti-inflammatory material.

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