Skin anti-allergic composition as well as preparation method and application thereof

Abstract

The invention relates to a skin antiallergic composition and a preparation method and application thereof, and the composition is prepared from the following raw materials: sodium cellulose, essence, propylene glycol, a coating solution, a nonionic surfactant and water, the coating solution is prepared by taking modified chitosan microspheres, ascophyllum nodosum extract, chamomile flower extract, centella asiatica extract, anthemis nobilis flower extract, glycerol and water as raw materials, and the modified chitosan microspheres are products obtained by grafting polylactic acid with chitosan. The modified chitosan microsphere can form a nano-micelle with a core-shell structure in a solvent, the ascophyllum nodosum extract, the chamomilla recutita extract, the centella asiatica extract and the anthemis nobilis extract are wrapped in the nano-micelle, the situation that the extracts are degraded or inactivated due to the external environment is avoided, a stable dispersion system can be formed in water, and the stability of the nano-micelle is improved. The plant extract is released after the body surface is coated, and the plant extract and other components synergistically improve the anti-allergic effect of the skin.

Description

Technical Field

[0001] The present invention relates to the technical field of skin care products, and in particular to a skin anti-allergic composition and a preparation method and application thereof. Background Art

[0002] At present, plant extracts are the most common core ingredients in common skin anti-allergic compositions. Their widespread application stems from their multi-effect anti-allergic mechanisms, safety advantages and market demand. Specifically, plant extracts with skin anti-allergic functions are usually widely used because they contain anti-inflammatory, antihistamine, antioxidant or barrier repair active ingredients (such as flavonoids, polyphenols, steroids, polysaccharides, etc.).

[0003] Among plant extracts, Ascophyllum nodosum extract, Chamomile extract, Centella asiatica extract, and Anthemis nodosum flower extract all have anti-allergic functions for the skin. Among them, Ascophyllum nodosum extract is mainly composed of fucoidan, which indirectly reduces the risk of sensitivity by regulating the skin microecology and enhancing the water-locking ability of the stratum corneum. Its antioxidant property can reduce the inflammatory response caused by environmental stimuli. Chamomile extract contains blue azulene (guaiacyl) and flavonoids, which can quickly relieve skin redness and stinging by inhibiting the release of histamine and blocking the production of inflammatory factors (such as interleukins and tumor necrosis factor). Centella asiatica extract contains triterpenoid saponins such as asiatica glycoside and madecassic acid, which promote collagen synthesis by activating the SMAD pathway, inhibit the release of inflammatory mediators (such as prostaglandins and nitric oxide), and reduce oxidative stress damage. Anthemis nodosum flower extract contains more than 27 anti-inflammatory triterpenoid compounds, which can inhibit inflammatory exudation by enhancing capillary toughness and reducing permeability, while scavenging free radicals and reducing oxidative damage.

[0004] However, the active ingredients such as polyphenols and flavonoids in Ascophyllum nodosum extract, Chamomile extract, Centella asiatica extract and Anthemis nobilis extract are easily degraded by external environmental factors such as light and oxygen, resulting in inactivation of ingredients, generation of irritants or phase separation, etc., which reduces the anti-allergic effect of the skin. The impact is even greater during long-term storage. Moreover, during long-term storage, the plant extracts may aggregate, and the particles formed by aggregation cannot penetrate the stratum corneum of the skin, causing the active ingredients to remain on the surface, resulting in reduced absorption efficiency and affecting the anti-allergic effect of the skin.

[0005] In summary, it is necessary to develop a new technical solution to solve the deficiencies in the existing technology. Summary of the Invention

[0006] The present invention provides an anti-allergic skin composition, its preparation method, and application. The anti-allergic skin composition is prepared using sodium cellulose, fragrance, propylene glycol, a coating solution, a nonionic surfactant, and water as raw materials. The coating solution is prepared using modified chitosan microspheres, Ascophyllum nodosum extract, Chamomile extract, Centella asiatica extract, Anthemis nobilis flower extract, glycerin, and water as raw materials. The modified chitosan microspheres are chitosan grafted onto polylactic acid. The anti-allergic skin composition of the present invention can form a stable dispersion system, can be stored for a long time, and exhibits excellent anti-allergic effects, thus having promising application prospects.

[0007] The object of the present invention is to provide an anti-allergic skin composition, comprising the following components in parts by mass:

[0008]

[0009] Wherein, the coating solution is composed of the following components in parts by mass:

[0010]

[0011] Wherein, the modified chitosan microspheres are products obtained by grafting chitosan with polylactic acid.

[0012] Furthermore, the sodium cellulose is selected from one or more of sodium carboxymethyl cellulose, sodium hydroxyethyl cellulose, and sodium hydroxypropyl cellulose.

[0013] Furthermore, the fragrance is selected from one or more of rose essential oil, lavender essential oil, and tea tree essential oil.

[0014] Another object of the present invention is to provide a method for preparing the above-mentioned anti-allergic skin composition, comprising the following steps:

[0015] S1, mixing chitosan, lactide, and a catalyst, heating and stirring to react, and purifying to obtain modified chitosan microspheres;

[0016] S2, blending the modified chitosan microspheres and glycerol, and ultrasonically treating the mixture to obtain a nanomicelle dispersion;

[0017] S3, mixing the nanomicelle dispersion, Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, Anthemis nobilis flower extract, and water, and dialyzing to obtain a coating solution;

[0018] S4. Blending the coating solution, sodium cellulose, essence, propylene glycol, nonionic surfactant and water to obtain an anti-allergic skin composition.

[0019] Furthermore, in step S1, the mass ratio of chitosan to lactide is 1:(4-6).

[0020] Furthermore, in step S1, the temperature of the heating and stirring reaction is 110-130°C.

[0021] Furthermore, in step S2, the ultrasonic treatment time is 20-40 minutes.

[0022] Furthermore, in step S3, the dialysis time is 2-4 days.

[0023] Another object of the present invention is to provide use of the above-mentioned skin anti-allergic composition in skin care products.

[0024] The present invention has the following beneficial effects:

[0025] The skin anti-allergic composition of the present invention is prepared using sodium cellulose, a coating solution, and the like as raw materials, wherein the coating solution comprises modified chitosan microspheres, a variety of plant extracts, and other components. The modified chitosan microspheres are obtained by first ring-opening polymerization of lactide under the catalysis of stannous octoate to form polylactic acid, and then grafting the polylactic acid with the amino and hydroxyl groups of chitosan. The chitosan in the modified chitosan microspheres of the present invention has a hydrophilic chain segment, and the polylactic acid has a hydrophobic chain segment. In a solvent, the hydrophilic chain segment and the hydrophobic chain segment work together to form nano micelles with a core-shell structure, and the Ascophyllum nodosum extract, the Chamomile flower extract, the Centella asiatica extract and the Anthemis nodosum flower extract are encapsulated inside the nano micelles, thereby avoiding degradation or loss of activity of the extracts caused by external environments such as light and oxygen. Secondly, the hydrophilic chain segment makes the nano micelles easily soluble in water, thereby forming a stable dispersion system in water. Moreover, after the modified chitosan microsphere nano micelles are mixed with sufficient water, the encapsulated plant extracts are released, and the components work synergistically to improve the anti-allergic effect of the skin. DETAILED DESCRIPTION

[0026] In order to more clearly illustrate the technical solutions of the present invention, the following examples are given. Unless otherwise stated, the raw materials, reactions and post-processing methods mentioned in the examples are common raw materials on the market and technical methods well known to those skilled in the art.

[0027] The terms "preferred," "preferably," "more preferred," and the like, used herein, refer to embodiments of the invention that may provide certain benefits under certain circumstances. However, other embodiments may also be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.

[0028] It should be understood that, except in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about." Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and appended claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.

[0029] The examples of the present invention use the following raw materials:

[0030] Sodium carboxymethyl cellulose, molecular weight 200,000, was purchased from Shanghai Jingchun Industrial Co., Ltd.;

[0031] Chitosan, molecular weight 1526.4539, degree of deacetylation greater than 90%, was purchased from Xi'an Jiahe Biotechnology Co., Ltd.;

[0032] Rose essential oil and fragrance were purchased from Guangzhou Hecheng Sanshen Biotechnology Co., Ltd.;

[0033] Glyceryl stearate, a nonionic surfactant, was purchased from Croda Chemicals (Shanghai) Co., Ltd.;

[0034] Ascophyllum nodosum extract was purchased from Lanzhou Waterless Biotechnology Co., Ltd.;

[0035] Chamomile flower extract was purchased from Lanzhou Waterless Biotechnology Co., Ltd.

[0036] Centella asiatica extract was purchased from Shanxi Lisheng Biotechnology Co., Ltd.;

[0037] Chamomile flower extract was purchased from Shaanxi Tianze Qiannuo Biotechnology Co., Ltd.

[0038] In the embodiment of the present invention, a dialysis bag with a molecular weight cut-off of 3500 Da was used for dialysis.

[0039] Example 1

[0040] A skin anti-allergic composition, comprising the following components in parts by weight:

[0041]

[0042] The coating solution is composed of the following components in parts by mass:

[0043]

[0044] The preparation method of the skin anti-allergic composition comprises the following steps:

[0045] S1. Under a nitrogen atmosphere, chitosan, lactide, stannous octoate, and 1-allyl-3-methylimidazole chloride were blended in a mass ratio of 1:5:0.4:10, heated to 120°C and stirred for 20 h. The reactants were precipitated with sufficient ethanol, filtered, washed, and Soxhlet extracted with acetone. After drying, modified chitosan microspheres were obtained.

[0046] S2. Blending the modified chitosan microspheres and glycerol according to the above mass fractions, and ultrasonically dispersing them for 30 minutes to obtain a nanomicelle dispersion;

[0047] S3. Adding the Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, and Anthemis nodosum flower extract, and water to the nanomicelle dispersion according to the above-mentioned parts by mass, mixing them evenly, and dialyzing them in sufficient water for 3 days, changing the water every 12 hours, to complete the encapsulation of the Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, and Anthemis nodosum flower extract by the nanomicelles to obtain a coating solution;

[0048] S4. Blend the coating solution, sodium carboxymethyl cellulose, rose essential oil, propylene glycol, glyceryl stearate and water according to the above-mentioned parts by mass to obtain an anti-allergic skin composition.

[0049] Example 2

[0050] A skin anti-allergic composition, comprising the following components in parts by weight:

[0051]

[0052] The coating solution is composed of the following components in parts by mass:

[0053]

[0054] The preparation method of the skin anti-allergic composition comprises the following steps:

[0055] S1. Under a nitrogen atmosphere, chitosan, lactide, stannous octoate, and 1-allyl-3-methylimidazole chloride were blended in a mass ratio of 1:5:0.4:10, heated to 115°C and stirred for 20 h. The reactants were precipitated with sufficient ethanol, filtered, washed, and Soxhlet extracted with acetone. After drying, modified chitosan microspheres were obtained.

[0056] S2. Blending the modified chitosan microspheres and glycerol according to the above mass fractions, and ultrasonically dispersing them for 30 minutes to obtain a nanomicelle dispersion;

[0057] S3. Adding the Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, and Anthemis nodosum flower extract, and water to the nanomicelle dispersion according to the above-mentioned parts by mass, mixing them evenly, and dialyzing them in sufficient water for 3 days, changing the water every 12 hours, to complete the encapsulation of the Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, and Anthemis nodosum flower extract by the nanomicelles to obtain a coating solution;

[0058] S4. Blend the coating solution, sodium carboxymethyl cellulose, rose essential oil, propylene glycol, glyceryl stearate and water according to the above-mentioned parts by mass to obtain an anti-allergic skin composition.

[0059] Example 3

[0060] A skin anti-allergic composition, comprising the following components in parts by weight:

[0061]

[0062]

[0063] The coating solution is composed of the following components in parts by mass:

[0064]

[0065] The preparation method of the skin anti-allergic composition comprises the following steps:

[0066] S1. Under a nitrogen atmosphere, chitosan, lactide, stannous octoate, and 1-allyl-3-methylimidazole chloride were blended in a mass ratio of 1:5:0.4:10, heated to 120°C and stirred for 20 h. The reactants were precipitated with sufficient ethanol, filtered, washed, and Soxhlet extracted with acetone. After drying, modified chitosan microspheres were obtained.

[0067] S2. Blending the modified chitosan microspheres and glycerol according to the above mass fractions, and ultrasonically dispersing them for 25 minutes to obtain a nanomicelle dispersion;

[0068] S3. Adding the Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, and Anthemis nodosum flower extract, and water to the nanomicelle dispersion according to the above-mentioned parts by mass, mixing them evenly, and dialyzing them in sufficient water for 3 days, changing the water every 12 hours, to complete the encapsulation of the Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, and Anthemis nodosum flower extract by the nanomicelles to obtain a coating solution;

[0069] S4. Blend the coating solution, sodium carboxymethyl cellulose, rose essential oil, propylene glycol, glyceryl stearate and water according to the above-mentioned parts by mass to obtain an anti-allergic skin composition.

[0070] Comparative Example 1

[0071] The difference between Comparative Example 1 and Example 1 is that step S1 is deleted, and chitosan is used instead of modified chitosan microspheres. The remaining components and preparation method are the same as those in Example 1.

[0072] Test Example 1

[0073] The anti-allergic skin compositions of Examples 1-3 and Comparative Example 1 were subjected to a hyaluronidase inhibition test.

[0074] Test method:

[0075] Long-term storage testing

[0076] Take 1mL CaCl2 solution (0.25mmol / L) and 5mL hyaluronidase solution (100U / mL) and incubate them in a water bath at 37℃ for 20min; add 5mL of the sample solution for testing that has been stored for 90 days and continue to incubate for 20min; then add 5mL sodium hyaluronate solution (0.5mg / mL), incubate them in a water bath at 37℃ for 30min, then take them out and place them at room temperature for 5min; add 1mL NaOH solution (0.4 mol / L) and 5 mL of acetylacetone solution (3.5 mL of acetylacetone dissolved in 50 mL of 1.0 mol / L sodium carbonate solution) were heated in a boiling water bath for 15 min and then immediately transferred to an ice water bath and cooled for 5 min; 10 mL of Ehrlich reagent (8 g of p-dimethylaminobenzaldehyde dissolved in 150 mL of concentrated hydrochloric acid and 150 mL of anhydrous ethanol) was added dropwise and diluted with 30 mL of anhydrous ethanol. The mixture was allowed to stand at room temperature for 20 min for color development and the absorbance at a wavelength of 540 nm was measured using a spectrophotometer.

[0077] The calculation formula for the inhibition rate of hyaluronidase by the sample is as follows:

[0078]

[0079] The letters in the formula mean: A: absorbance value of the control solution sample (acetic acid buffer solution replaces the sample solution); B: absorbance value of the control blank solution sample (acetic acid buffer solution replaces the sample solution and enzyme solution); C: absorbance value of the sample solution; D: absorbance value of the sample blank solution (acetic acid buffer solution replaces the enzyme solution). The sample solution is the anti-allergic skin composition of the present invention diluted with sufficient water after storage for 90 days (the mass ratio of the anti-allergic skin composition to water is 1:100) or Comparative Example 1 diluted with an equal amount of water after storage for 90 days.

[0080] The test results are shown in Table 1.

[0081] Table 1 Results of the hyaluronidase inhibition test on the skin anti-allergic composition

[0082]

[0083] As can be seen from Table 1, in the long-term storage test, the inhibition rate of hyaluronidase in Examples 1-3 was significantly higher than that in Comparative Example 1. This is because Comparative Example 1 used chitosan instead of modified chitosan microspheres, and did not introduce hydrophobic segments, so it was impossible to form micelles, and thus it was impossible to encapsulate the Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, and Anthemis nodosum flower extract, resulting in a significant decrease in the inhibition rate of hyaluronidase after long-term storage, which means that the anti-allergic effect of the skin was significantly reduced.

[0084] Test Example 2

[0085] A skin irritation repair experiment was conducted on the skin anti-allergic compositions of Examples 1-3 and Comparative Example 1.

[0086] Test method:

[0087] (1) Routine testing

[0088] The experiment was carried out according to the method described in Section 2.2.6 Skin irritation repair experiment in the literature (Wang Ling. Research on the preparation process, efficacy and action pathway of anti-allergic and antipruritic plant combination extracts [D]. 2015.).

[0089] 10 volunteers in good physical condition were selected, and the inner sides of the left and right arms of the volunteers were selected as the test sites, and a square area with a size of 2cm×2cm was circularly marked; the test area (the same area) was washed with clean water, and the subjects sat quietly for 10 minutes. The skin redness blank value was measured using the Mexamter MX18 (pigment test probe) of the German CK company, and then the smear experiment stage was entered; the test area was stimulated with a 50% mass fraction capsaicin aqueous solution (about 0.01mL); after continuous stimulation for 30 minutes, the numerical value was collected; 0.05mL of the test sample was smeared on the test area (wherein, the sample was the skin anti-allergic composition of the present invention diluted with sufficient water, the mass ratio of the skin anti-allergic composition to water was 1:100, or comparative example 1 diluted with an equal amount of water), and data was collected after 45 minutes; 0.05mL of pure water was smeared on the blank control; the numerical values ​​measured each time at the experimental site of the subject were counted, the average change rate was calculated, and the change in the redness value was analyzed.

[0090] The change in skin redness value reflects the change of skin redness in the experimental area over time during the test period. The larger the value, the greater the degree of skin redness.

[0091] The calculation formula is as follows:

[0092]

[0093] (2) Long-term storage test

[0094] The difference between this test method and the conventional test (1) is that the sample solution used has been stored for 90 days. The rest is the same as the conventional test (1).

[0095] The test results are shown in Table 2.

[0096] Table 2 Skin irritation repair test results

[0097]

[0098] As can be seen from Table 2, in conventional tests, the average rate of change of skin redness after applying the samples of Examples 1-3 was slightly lower than that of Comparative Example 1, while in long-term storage tests, the average rate of change of skin redness after applying the samples of Examples 1-3 was significantly lower than that of Comparative Example 1. This is because Comparative Example 1 uses chitosan instead of modified chitosan microspheres, does not introduce hydrophobic segments, and cannot form micelles, thereby failing to encapsulate the Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, and Anthemis nodosum flower extract. After long-term storage, the plant extracts are affected by the external environment, causing inactivation, degradation, and other adverse effects, resulting in a significant decrease in the anti-allergic effect of the skin. The modified chitosan microspheres of Examples 1-3 form micelles to encapsulate the plant extracts. After the encapsulated plant extracts are released, the adverse effects of the external environment on the encapsulated plant extracts during long-term storage are avoided, that is, the adverse effects described in Comparative Example 1 are avoided, so they can synergize with the other components to achieve a good anti-allergic effect on the skin.

[0099] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0100] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A skin anti-allergic composition, characterized in that, The skin anti-allergic composition comprises the following components in parts by weight: Wherein, the coating solution is composed of the following components in parts by mass: Wherein, the modified chitosan microspheres are products obtained by grafting chitosan with polylactic acid.

2. The anti-allergic skin composition according to claim 1, characterized in that: The sodium cellulose is selected from one or more of sodium carboxymethyl cellulose, sodium hydroxyethyl cellulose, and sodium hydroxypropyl cellulose.

3. The anti-allergic skin composition according to claim 1, characterized in that: The fragrance is selected from one or more of rose essential oil, lavender essential oil and tea tree essential oil.

4. The method for preparing the antiallergic skin composition according to any one of claims 1 to 3, characterized in that: The preparation method of the skin anti-allergic composition comprises the following steps: S1, mixing chitosan, lactide, and a catalyst, heating and stirring to react, and purifying to obtain modified chitosan microspheres; S2, blending the modified chitosan microspheres and glycerol, and ultrasonically treating the mixture to obtain a nanomicelle dispersion; S3, mixing the nanomicelle dispersion, Ascophyllum nodosum extract, Chamomile flower extract, Centella asiatica extract, Anthemis nobilis flower extract, and water, and dialyzing to obtain a coating solution; S4. Blending the coating solution, sodium cellulose, essence, propylene glycol, nonionic surfactant and water to obtain an anti-allergic skin composition.

5. The method for preparing the anti-allergic skin composition according to claim 4, characterized in that: In step S1, the mass ratio of chitosan to lactide is 1:(4-6).

6. The method for preparing the anti-allergic skin composition according to claim 4, characterized in that: In step S1, the temperature of the heating and stirring reaction is 110-130°C.

7. The method for preparing the anti-allergic skin composition according to claim 4, characterized in that: In step S2, the ultrasonic treatment time is 20-40 minutes.

8. The method for preparing the anti-allergic skin composition according to claim 4, characterized in that: In step S3, the dialysis time is 2-4 days.

9. Use of the anti-allergic skin composition according to any one of claims 1 to 3 in skin care products.

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