Composition with oil control effect as well as preparation method and application thereof

Abstract

The invention discloses a composition with an oil control effect as well as a preparation method and application thereof, the composition comprises carboxymethyl porous starch, chitosan oligosaccharide and sarcosine, the composition takes the carboxymethyl porous starch as a carrier, and the chitosan oligosaccharide and the sarcosine are loaded through the porous structure, hydrogen bond and ion action of the carboxymethyl porous starch to form the composition. According to the composition with the oil control effect disclosed by the invention, the stability of the chitosan oligosaccharide is improved while the amino irritation is reduced; through the synergistic effect of chitosan oligosaccharide and sarcosine, the oil control effect of the composition is improved from multiple targets, the application range of chitosan oligosaccharide in oil control products is widened, and the chitosan oligosaccharide oil control composition has the advantages of being good in stability, high in safety and good in oil control effect; the preparation method is simple to operate, mild in process condition and good in application prospect.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and relates to a composition with oil control effect, a preparation method and application thereof, and in particular to a composition capable of taking into account stability, safety and multi-target oil control, a preparation method and application thereof. Background Art

[0002] When oil accumulates on the skin surface, it affects the breathability and health of the skin, causing problems such as clogged pores, and even skin diseases such as acne and seborrheic dermatitis. By effectively controlling sebum secretion, the occurrence of these skin problems can be reduced, which helps maintain the normal physiological function of the skin, protect the skin from external environmental damage, and improve the overall health of the skin. Therefore, people's demand for oil control products is also increasing.

[0003] At present, there are few studies on the inhibition of skin lipids by chitosan oligosaccharides, but the inhibition of skin lipids is also achieved by regulating lipid metabolism pathways. Studies have shown that chitosan oligosaccharides reduce lipid accumulation in non-alcoholic fatty liver cell models by regulating fatty acid absorption and triglyceride synthesis pathways. Specifically, chitosan oligosaccharides can significantly downregulate the expression levels of genes and proteins such as peroxisome proliferator-activated receptor γ (PPArpmγ) and fatty acid transferase (CD36); they can also reduce lipid accumulation by inhibiting the expression of inflammatory factors such as IL-8 and TNF-α, and the phosphorylation of the p38 mitogen-activated protein kinase (p38MAPK) signaling pathway. In addition, chitosan oligosaccharides can also inhibit the activity of 5α-reductase; this provides a theoretical basis for the development of new oil control products. At the same time, studies have shown that sarcosine has the effect of inhibiting the activity of 5α-reductase.

[0004] Due to the presence of amino groups in chitosan oligosaccharides, they are very susceptible to oxidation or other chemical reactions under light and heat conditions, which not only destroys their molecular structure but may also be irritating to the skin, greatly limiting their application in cosmetics.

[0005] Therefore, it is of great practical significance to develop a chitosan oligosaccharide composition with good safety, good stability and good oil control effect. Summary of the invention

[0006] Due to the above-mentioned defects in the prior art, the present invention provides a chitosan oligosaccharide composition with good safety, good stability and good oil control effect, specifically a composition and a preparation method thereof that can take into account stability, safety and multi-target oil control at the same time, so as to overcome the defects of poor stability and safety of the current chitosan oligosaccharide used in oil control.

[0007] In order to achieve the above object, the present invention provides the following technical solutions:

[0008] A composition with oil-controlling effect comprises carboxymethyl porous starch, chitosan oligosaccharide and sarcosine.

[0009] The composition uses carboxymethyl porous starch as a carrier, and loads chitosan oligosaccharide and sarcosine through porous structure, hydrogen bond and ion action to form a composition. The composition reduces amino irritation while improving the stability of chitosan oligosaccharide; through the synergistic effect of chitosan oligosaccharide and sarcosine, the oil control effect of the composition is improved from multiple targets, broadening the application of chitosan oligosaccharide in oil control products. The above composition has multiple advantages such as good stability, high safety, good oil control effect, etc., and has broad application prospects in the fields of cosmetics.

[0010] As the preferred technical solution:

[0011] In the composition with oil-control effect as described above, the mass ratio of the carboxymethyl porous starch, chitosan oligosaccharide and sarcosine is 10-20:1:0.1-0.5.

[0012] As described above, the composition with oil-control effect, wherein the carboxymethyl porous starch utilizes porous structure, hydrogen bonds and ionic effects to load chitosan oligosaccharides and sarcosine, is stable and safe and specifically controls oil through multiple targets.

[0013] The present invention also provides a method for preparing the composition with oil-control effect as described above, comprising dissolving carboxymethyl porous starch in water to obtain a carboxymethyl porous starch aqueous solution, and adjusting the pH value thereof to 5.5-7.0; stirring the carboxymethyl porous starch aqueous solution, and adding chitosan oligosaccharide and sarcosine to the stirred carboxymethyl porous starch aqueous solution, and maintaining stirring for a certain time; standing for a certain time, and then drying and crushing to obtain the composition with oil-control effect.

[0014] The preparation method is simple to operate, has mild process conditions and has good application prospects.

[0015] As the preferred technical solution:

[0016] In the method as described above, the carboxymethyl porous starch is dissolved in water under stirring at 25-80° C., and the concentration of the carboxymethyl porous starch aqueous solution is 100 g / L.

[0017] In the method described above, the carboxymethyl porous starch aqueous solution under stirring refers to a carboxymethyl porous starch aqueous solution at 25° C. and a stirring speed of 200-800 rpm, and maintaining stirring for a certain period of time refers to maintaining stirring for 1-4 hours.

[0018] In the method as described above, the certain period of time refers to 1 to 3 hours of standing.

[0019] In the method described above, the drying refers to freeze drying, specifically freeze drying at -80°C for 48 to 72 hours.

[0020] According to the method described above, the composition is mechanically pulverized for 10 to 20 minutes after drying.

[0021] In addition, the present invention also provides use of the above-mentioned composition with oil-control effect in preparing cosmetics.

[0022] The above technical solution is only a feasible technical solution of the present invention, and the protection scope of the present invention is not limited thereto. Those skilled in the art can reasonably adjust the specific design according to actual needs.

[0023] The above invention has the following advantages or beneficial effects:

[0024] (1) The composition with oil control effect of the present invention uses carboxymethyl porous starch as a carrier, and loads chitosan oligosaccharide and sarcosine to form a composition through porous structure, hydrogen bonding and ionic action. The composition reduces amino irritation and improves the stability of chitosan oligosaccharide, which helps to improve its overall performance and efficacy in cosmetics, making it play a more lasting and stable role, thereby bringing better skin care effects to consumers;

[0025] (2) In the composition with oil control effect of the present invention, chitosan oligosaccharide and sarcosine act synergistically to improve the oil control effect of the composition through multi-target oil control, thus broadening the application of chitosan oligosaccharide in oil control products and having good application prospects. DETAILED DESCRIPTION

[0026] The structure of the present invention is further described below in conjunction with specific embodiments, but is not intended to be a limitation of the present invention.

[0027] Example 1

[0028] A method for preparing a composition having oil control effect comprises the following steps:

[0029] (1) Preparing a carboxymethyl porous starch solution: at room temperature, accurately weigh carboxymethyl porous starch according to a mass ratio of carboxymethyl porous starch, chitosan oligosaccharide, and sarcosine of 10:1:0.1, and add water and stir until the solution is completely dissolved;

[0030] (2) Adjust the pH value: adjust the pH value of the solution to 5.5;

[0031] (3) Loading chitosan oligosaccharide and sarcosine: Stir the carboxymethyl porous starch solution at a speed of 200 rpm / min at room temperature. Accurately weigh chitosan oligosaccharide and sarcosine according to the mass ratio of carboxymethyl porous starch, chitosan oligosaccharide and sarcosine of 10:1:0.1, and add them to the carboxymethyl porous starch solution with adjusted pH value, and continue stirring for 4 h.

[0032] (4) Standing: The mixture was allowed to stand at room temperature for 1 h to ensure that chitosan oligosaccharide and sarcosine were fully loaded on the carboxymethyl porous starch;

[0033] (5) Freeze drying: pre-freeze the solution obtained in (4) in an ultra-low temperature refrigerator for 48 h, then place it on the shelf of a freeze dryer and freeze-dry it at -80 °C for 48 h;

[0034] (6) Pulverizing: The freeze-dried object is pulverized mechanically for 10 minutes to obtain a composition.

[0035] Example 2

[0036] A method for preparing a composition having oil control effect comprises the following steps:

[0037] (1) Preparing a carboxymethyl porous starch solution: at 50° C., accurately weigh carboxymethyl porous starch according to a mass ratio of carboxymethyl porous starch, chitosan oligosaccharide, and sarcosine of 15:1:0.25, and add water and stir until the solution is completely dissolved;

[0038] (2) Adjusting pH value: Adjust the pH value of the solution to 6.5;

[0039] (3) Loading chitosan oligosaccharide and sarcosine: Stir the carboxymethyl porous starch solution at a speed of 500 rpm / min at room temperature. Accurately weigh chitosan oligosaccharide and sarcosine according to the mass ratio of carboxymethyl porous starch, chitosan oligosaccharide and sarcosine of 15:1:0.25, and add them to the carboxymethyl porous starch solution with adjusted pH value, and continue stirring for 2.5 h.

[0040] (4) Standing: The mixture was allowed to stand at room temperature for 2 h to ensure that chitosan oligosaccharide and sarcosine were fully loaded on the carboxymethyl porous starch;

[0041] (5) Freeze drying: pre-freeze the solution obtained in (4) in an ultra-low temperature refrigerator for 48 h, then place it on the shelf of a freeze dryer and freeze-dry it at -80 °C for 60 h;

[0042] (6) Pulverizing: The freeze-dried object is pulverized mechanically for 15 minutes to obtain a composition.

[0043] Example 3

[0044] A method for preparing a composition having oil control effect comprises the following steps:

[0045] (1) Preparing a carboxymethyl porous starch solution: at 80° C., accurately weigh carboxymethyl porous starch according to a mass ratio of carboxymethyl porous starch, chitosan oligosaccharide, and sarcosine of 20:1:0.5, and add water and stir until the solution is completely dissolved;

[0046] (2) Adjusting pH: Adjust the pH value of the solution to 7.0;

[0047] (3) Loading chitosan oligosaccharide and sarcosine: Stir the carboxymethyl porous starch solution at a speed of 800 rpm / min at room temperature. Accurately weigh chitosan oligosaccharide and sarcosine according to the mass ratio of carboxymethyl porous starch, chitosan oligosaccharide and sarcosine of 20:1:0.5, and add them to the carboxymethyl porous starch solution with adjusted pH value, and continue stirring for 1 h.

[0048] (4) Standing: The mixture was allowed to stand at room temperature for 3 h to ensure that chitosan oligosaccharide and sarcosine were fully loaded on the carboxymethyl porous starch;

[0049] (5) Freeze drying: pre-freeze the solution in (4) in an ultra-low temperature refrigerator for 48 h, then place it on the shelf of a freeze dryer and freeze-dry it at -80 °C for 72 h;

[0050] (6) Pulverizing: The freeze-dried object is pulverized mechanically for 20 minutes to obtain a composition.

[0051] Comparative Example 1

[0052] This comparative example is a 1wt% chitosan oligosaccharide aqueous solution.

[0053] Comparative Example 2

[0054] This comparative example is a mixed solution of chitosan oligosaccharide and sarcosine, wherein the final concentration of chitosan oligosaccharide is 1wt%, and the final concentration of sarcosine is 0.25wt%.

[0055] Comparative Example 3

[0056] This comparative example is a 0.2wt% chitosan oligosaccharide aqueous solution.

[0057] Comparative Example 4

[0058] This comparative example is a 3wt% chitosan oligosaccharide aqueous solution.

[0059] Comparative Example 5

[0060] This comparative example is a 1wt% sarcosine aqueous solution.

[0061] In order to prove the technical advantages of the technical solution provided by this application, the following is an experimental test experiment of the technical solution provided by this application:

[0062] 1. Stability test

[0063] 1.1 Composition of stability test samples

[0064] Table 1. Composition of stability test samples

[0065]

[0066] 1.2 Test conditions and methods

[0067] Table 2. Stability test conditions and methods

[0068]

[0069] 1.3 Results and observations

[0070] The test results are shown in Table 3 (√ indicates that the sample is stable)

[0071] Table 3. Stability test results

[0072]

[0073] As shown in Table 3, sample groups 1 to 3 showed better stability than control groups 1 to 2, indicating that the oil control composition prepared by the present invention indeed improves the stability of chitosan oligosaccharide.

[0074] 2. Evaluation of oil control efficacy

[0075] 2.1 Inhibition of 5α-reductase activity:

[0076] 2.1.1 Operation steps

[0077] (1) Sample loading in 96-well microplate: The test sets up standard well group, sample well group and blank control well group (the blank control well group does not contain sample and HrpmP enzyme labeling reagent, and the rest of the steps are the same). Each test group has 3 parallel wells. Add 50μL of standard with different 5Arpm enzyme activity concentrations to the standard well group (the enzyme activity is 0U, 5U, 10U, 20U, 40U and 80U respectively). First add 25μL of the sample to be tested to the sample well group, and then add 25μL of 40U standard (the final enzyme activity concentration in the sample well is 20U). Add 50μL of buffer to the blank control well group. During the loading process, carefully add the solution to the bottom of the 96-well microplate, try to avoid the pipette tip touching the wall or bottom of the well plate, and finally shake gently to mix.

[0078] (2) Incubation at 37°C: After adding the sample to the 96-well microplate, seal the opening of the well plate with a sealing film to prevent water evaporation and foreign matter from dripping in. Then place the microplate in a constant temperature water bath oscillator (speed 0), keep the liquid level just above the liquid addition level of the well plate, and incubate at 37°C for 30 minutes.

[0079] (3) Plate washing: After the plate is incubated at 37°C for 30 minutes, carefully remove the sealing film, discard the liquid, and gently shake dry. Dilute the 30-fold concentrated washing solution with 30-fold distilled water as the washing solution for the plate. Fill each well with washing solution, let it stand for 30 seconds, then discard the liquid and gently shake dry. Repeat this process 5 times and gently pat dry with a dry towel.

[0080] (4) Add enzyme: Add 100 μL of HrpmP enzyme-labeled reagent to each well, except for the blank well.

[0081] (5) Incubation at 37°C: Same steps as (2).

[0082] (6) Plate washing: The operation steps are the same as (4).

[0083] (7) TMB color development: First add 50 μL of TMB color developer A solution to each well, then add 50 μL of TMB color developer B solution, gently shake to mix, and incubate at 37°C in the dark for 10 minutes.

[0084] (8) Stop color development: Add 50 μL of stop solution to each well to terminate the TMB color development reaction (the blue color immediately turns to yellow).

[0085] (9) Absorbance determination: Set the test wavelength of the microplate reader to 450nm and measure the absorbance (OD value) of each well in sequence. The determination should be completed within 15 minutes after adding the stop color development.

[0086] 2.1.2 Composition of 5α-reductase activity inhibition test samples

[0087] Table 4. Composition of 5α-reductase activity inhibition test samples

[0088]

[0089] 2.1.3 Samples’ inhibition test on 5α-reductase activity

[0090] After completing the test of the OD450nm values ​​of each standard well, sample well and blank well, first calculate the standard curve of different enzyme activity concentrations and OD450nm values ​​of the standard wells, then calculate the OD450nm value corresponding to the theoretical enzyme activity concentration (20U) of the sample well according to the curve as the OD540nm value of the standard well for the sample test concentration, and calculate the OD450nm value corresponding to the theoretical enzyme activity concentration (0U) of the blank well according to the curve as the OD450nm value of the blank well. The inhibition rate of the sample on 5α-reductase (%) = (OD450nm standard well-OD450nm sample well) / (OD450nm standard well-OD450nm blank well) × 100%.

[0091] 2.1.4 Results of the sample inhibition test on 5α-reductase activity

[0092] The test results are shown in Table 5.

[0093] Table 5. 5α-reductase inhibition rate test results

[0094]

[0095] As shown in Table 5, the content of chitosan oligosaccharide in the aqueous solution of the sample obtained in Example 2 (1.625 wt%) is half of that in Comparative Example 3, but the effect of the composition in inhibiting 5α-reductase is very similar to that in Comparative Example 3.

[0096] 2.2 Human body oil control efficacy test:

[0097] 2.2.1 Test details, steps and precautions

[0098] (1) Test population: Recruit 20 experimental volunteers aged 20 to 35 years old, in good health, without skin diseases, not pregnant or breastfeeding, and not allergic to product ingredients.

[0099] (2) Test site: The test site is the forehead. The sample application area and the control area are randomly distributed on the left and right sides of the forehead. The sample application area and the control area are the same in area, each area is 3 cm × 3 cm, and the area interval is 1 cm.

[0100] (3) Test instrument: Sebumeter SM815 or one with the same principle.

[0101] (4) Test conditions: The test environment temperature is 20℃~22℃; the test environment relative humidity is 40%~60%; the test conditions during the test should remain consistent, such as: tester, location, instrument, etc.

[0102] (5) Test period: 8h;

[0103] (6) Test method:

[0104] Twenty test subjects were selected for this test. A 3cm×3cm area was marked symmetrically on the left and right sides of each person's forehead, with the left side being the sample area and the right side being the blank control area. 0.5 ml was applied to each area, and the skin oil content 2, 4, and 8 hours after using the sample was tested using the skin oil tester Sebumeter SM815. Three points were randomly selected from each area for testing, and the average values ​​were taken, recorded as T2, T4, and T8, respectively. The oil control efficacy was evaluated by calculating the rate of change of oil content.

[0105] (7) Change rate of skin oil content (%) = [(T n sample-T0 sample)-(T n control-T0 control)] / (T n Control-T0 control)*100%;

[0106] T0 is the skin sebum content at the initial moment, T n is the skin sebum content after n hours

[0107] 2.2.2 Composition of human oil control efficacy test samples

[0108] Table 6. Composition of samples tested for human oil control efficacy

[0109]

[0110] The test results are shown in Table 7:

[0111] Table 7. Change rate of skin sebum content (%)

[0112]

[0113] As shown in Table 7, compared with the blank control area, the skin oil secretion of the subjects decreased by 35.58%, 32.93% and 31.17% after using Example 2 for 2h, 4h and 8h, respectively, indicating that the composition of Example 2 can significantly reduce the oil content on the skin surface. Compared with Comparative Examples 4 and 5, Example 2 can have a similar or even stronger effect of inhibiting skin oil while reducing the addition amount of chitosan oligosaccharide and sarcosine. It can be seen that the composition of the present invention can significantly reduce the oil content on the skin surface, and chitosan oligosaccharide and sarcosine have a synergistic effect.

[0114] Those skilled in the art should understand that those skilled in the art can implement variations by combining the prior art and the above embodiments, which will not be described in detail here. Such variations do not affect the essential content of the present invention, and will not be described in detail here.

[0115] The above describes the preferred embodiments of the present invention. It should be understood that the present invention is not limited to the above-mentioned specific embodiments, and the devices and structures that are not described in detail should be understood to be implemented in a common manner in the art; any technician familiar with the art can use the above-disclosed methods and technical contents to make many possible changes and modifications to the technical solutions of the present invention without departing from the scope of the technical solutions of the present invention, or modify them into equivalent embodiments of equivalent changes, which does not affect the essential content of the present invention. Therefore, any simple modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solutions of the present invention are still within the scope of protection of the technical solutions of the present invention.

Claims

1. A composition with oil control effect, characterized in that: Including carboxymethyl porous starch, chitosan oligosaccharide and sarcosine.

2. The composition with oil control effect according to claim 1, characterized in that: The mass ratio of the carboxymethyl porous starch, chitosan oligosaccharide and sarcosine is 10-20:1:0.1-0.

5.

3. The composition with oil control effect according to claim 1, characterized in that: The carboxymethyl porous starch utilizes porous structure, hydrogen bond and ion action to load chitosan oligosaccharide and sarcosine.

4. A method for preparing a composition with oil control effect as claimed in any one of claims 1 to 3, characterized in that: The carboxymethyl porous starch is dissolved in water to obtain a carboxymethyl porous starch aqueous solution, and the pH value thereof is adjusted to 5.5-7.0; the carboxymethyl porous starch aqueous solution is stirred, and chitosan oligosaccharide and sarcosine are added to the stirred carboxymethyl porous starch aqueous solution, and the stirring is maintained for a certain time; after standing for a certain time, the solution is dried and crushed to obtain the composition with oil control effect.

5. The method according to claim 4, characterized in that The carboxymethyl porous starch is dissolved in water under stirring at 25-80° C., and the concentration of the carboxymethyl porous starch aqueous solution is 100 g / L.

6. The method according to claim 4, characterized in that The carboxymethyl porous starch aqueous solution under stirring refers to a carboxymethyl porous starch aqueous solution at 25° C. and a stirring speed of 200 to 800 rpm, and maintaining stirring for a certain time refers to maintaining stirring for 1 to 4 hours.

7. The method according to claim 4, characterized in that The said standing for a certain period of time refers to standing for 1 to 3 hours.

8. The method according to claim 4, characterized in that The drying refers to freeze drying, specifically freeze drying at -80°C for 48 to 72 hours.

9. The method according to claim 4, characterized in that After drying, the composition is mechanically pulverized for 10 to 20 minutes.

10. Use of the composition with oil control effect as claimed in any one of claims 1 to 3 in the preparation of cosmetics.

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