Preparation method and application of soluble fiber dried product, color-staying water-gloss lip gloss and preparation method

By extracting and processing soluble fiber dry products from pistachios and preparing color-stained water-gloss lip gloss with other raw materials, the existing lip gloss' antioxidant performance and insufficient anti-photo-oxidation performance are solved, and efficient UVB damage repair effect and long-lasting lip makeup effect are achieved.

CN119868200AInactive Publication Date: 2025-04-25저장 아얀 바이오텍 컴퍼니 리미티드
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Patent Information

Application Number
CN202510370669.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-27
Publication Date
2025-04-25
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

Existing lip glosses are difficult to achieve high antioxidant performance, anti-photooxidation performance and stability at the same time, and are not effective in repairing DNA and nuclear damage to human keratinocytes induced by UVB.

Method used

By extracting soluble fiber drying products from pistachios and combining other raw materials, soluble fiber drying products with high antioxidant and water-soluble are prepared by specific enzymatic decomposition and drying methods for the preparation of static water gloss lip gloss.

Benefits of technology

It improves the antioxidant performance, anti-photooxidation performance and stability of lip gloss, and has the effect of repairing the damage of human keratinocytes induced by UVB. It has high color rendering, stable color and strong water and light feeling, extending the durability of lip makeup.

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Abstract

The invention relates to the technical field of lip gloss, in particular to a preparation method and application of a soluble fiber dry product, color-staying water-gloss lip gloss and a preparation method thereof. The color-staying water-gloss lip gloss provided by the invention is prepared by adding the soluble fiber dried product extracted from pistachio nuts as a raw material, so that not only can the oxidation resistance of the lip gloss be improved, but also the photooxidation resistance and the stability of the lip gloss can be improved. Besides, the soluble fiber dry product is combined with other raw materials, so that the soluble fiber dry product in the lip gloss prepared by the method is loaded and wrapped by other raw material components, the photooxidation resistance and the stability of the lip gloss are improved, and the lip gloss can act for a long time. By combining the soluble fiber dried product with other raw materials, the lip gloss sample prepared by the method disclosed by the invention also has the effects of resisting UVB-induced human keratinocyte DNA and repairing cell nucleus damage.
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Description

Technical Field

[0001] The invention relates to the technical field of lip gloss, and in particular to a preparation method and application of a soluble fiber dried product, a color-retaining water-glossy lip gloss and a preparation method thereof. Background Art

[0002] Lip gloss is a type of lipstick. Its paste is soft and rich in texture, in the form of a viscous liquid or a thin paste. Lip gloss is rich in various highly moisturizing oils and glitter factors, and is crystal clear. After application, it has a moisturizing effect on the lips, and at the same time can make the lips crystal clear, bright and eye-catching, increase the three-dimensional sense of the lips, play the role of decorating the lips, and make people look more complex. Compared with lip gloss, lip gloss is thicker, has stronger covering power, and is richer in color; compared with lipstick, it is more moisturizing, not easy to dry, and keeps the lips moist and light.

[0003] Patent document CN109248113A discloses an emulsified lip gloss, which includes the following components by weight: 65-85 parts of oil phase; 1.0-10 parts of emulsifier; 10-20 parts of water phase; 0.1-5.0 parts of cosmetic pigments. The present invention uses oil-in-water emulsification technology to combine emulsifiers of specific compound types and compound ratios with specific contents of oil phase, water phase and cosmetic pigments. On the one hand, it can directly replenish water to the lips and instantly soften the surface of the lips; on the other hand, through the compound combination of specific types and specific proportions of emulsifiers, it can achieve the unique skin feel of lip gloss that quickly melts. In addition, the formula also contains a specific amount of moisturizer (1,2-hexanediol, butanediol, glycerin in the water phase), which can provide a more lasting moisturizing effect than the general full-oil formula system lip gloss, and can achieve a specific makeup effect of full, bright and lasting lips. Summary of the invention

[0004] In view of this, the present invention provides a preparation method and application of a soluble fiber dried product, a color-retaining water-gloss lip gloss and a preparation method. The color-retaining water-gloss lip gloss is made by adding a soluble fiber dried product extracted from pistachios as a raw material, which can not only improve the antioxidant properties of the lip gloss, but also improve its anti-photooxidation performance and stability. In addition, the soluble fiber dried product is combined with other raw materials, and the method of the present invention is notified so that the soluble fiber dried product used in the preparation of the lip gloss is loaded and wrapped by other raw material components, so that its anti-photooxidation performance and stability are improved and can have a lasting effect. By combining the soluble fiber dried product with other raw materials, the lip gloss sample prepared by the method of the present invention also has the effect of repairing human keratinocyte DNA and cell nucleus damage induced by UVB.

[0005] One of the purposes of the present invention is to provide a method for preparing a soluble fiber dry product. The method comprises: defatting pistachios to obtain defatted pistachio powder; After using alkaline protease to ultrasonically hydrolyze defatted pistachio powder, adding high temperature resistant α-amylase to perform ultrasonic hydrolysis to inactivate the enzyme, thereby obtaining a first enzyme-inactivating solution; Adding cellulase to the first enzyme-killing solution to perform ultrasonic enzymolysis to kill the enzyme, thereby obtaining a second enzyme-killing solution; The second enzyme-inactivated solution is centrifuged, the supernatant is taken, concentrated, treated with 95% ethanol, centrifuged and dried, and the precipitate is the soluble fiber dry product.

[0006] Specifically, the amount of alkaline protease added was 6% of the weight of defatted pistachio powder, and ultrasonic enzymolysis was performed in a water bath at 55°C and 500W for 30 min.

[0007] Specifically, after alkaline protease hydrolysis, the pH of the solution was adjusted to 4.8 with 3M glacial acetic acid, the amount of thermostable α-amylase added was 8% of the weight of defatted pistachio powder, and ultrasonic enzymolysis was carried out in a water bath at 90°C and 500W for 45 minutes.

[0008] Specifically, the amount of cellulase added was 5% of the weight of the defatted pistachio powder, and ultrasonic enzymolysis was performed at 60° C. and 350 W for 40 min.

[0009] One of the purposes of the present invention is to provide a color-retaining water-glossy lip gloss, wherein the raw materials thereof include, by weight, 800-1500 parts of the soluble fiber dried product prepared in the above steps, 400-600 parts of jojoba oil, 80-120 parts of beeswax, 30-60 parts of candelilla wax, 80-120 parts of polydimethylsiloxane, 100-300 parts of chitosan, 10-30 parts of sodium hyaluronate, 5-15 parts of cochineal red, 20-40 parts of mica powder, 2-8 parts of strawberry essence and 2-8 parts of ethyl paraben.

[0010] Specifically, the raw materials of the color-staying glossy lip gloss include, by weight, 800 parts of soluble fiber dry product, 600 parts of jojoba oil, 120 parts of beeswax, 30 parts of candelilla wax, 120 parts of polydimethylsiloxane, 100 parts of chitosan, 30 parts of sodium hyaluronate, 15 parts of cochineal red, 20 parts of mica powder, 2 parts of strawberry essence and 2 parts of ethyl paraben.

[0011] Specifically, the raw materials of the color-staying glossy lip gloss include, by weight, 1500 parts of dried soluble fiber, 400 parts of jojoba oil, 80 parts of beeswax, 60 parts of candelilla wax, 80 parts of polydimethylsiloxane, 300 parts of chitosan, 10 parts of sodium hyaluronate, 5 parts of cochineal red, 40 parts of mica powder, 8 parts of strawberry essence and 8 parts of ethyl paraben.

[0012] Specifically, the raw materials of the color-staying glossy lip gloss include, by weight, 1000 parts of soluble fiber dry product, 500 parts of jojoba oil, 100 parts of beeswax, 50 parts of candelilla wax, 100 parts of polydimethylsiloxane, 200 parts of chitosan, 20 parts of sodium hyaluronate, 10 parts of cochineal red, 30 parts of mica powder, 5 parts of strawberry essence and 3 parts of ethyl paraben.

[0013] Specifically, parts by weight refers to any weight and is a relative proportion by weight.

[0014] Specifically, the soluble fiber dry product was prepared from pistachios, and its average solubility was 91.08%, and the average content of flavan-3-ol was 205.51 μg / g.

[0015] One of the purposes of the present invention is to provide a method for preparing a color-retaining water-gloss lip gloss, comprising: 3) preparing a dry soluble fiber product; 4) Provide 800-1500 parts of dry soluble fiber, 400-600 parts of jojoba oil, 80-120 parts of beeswax, 30-60 parts of candelilla wax, 80-120 parts of polydimethylsiloxane, 100-300 parts of chitosan, 10-30 parts of sodium hyaluronate, 5-15 parts of cochineal, 20-40 parts of mica powder, 2-8 parts of strawberry flavor and 2-8 parts of ethylparaben.

[0016] 3) Mix and melt the formulated amounts of jojoba oil, beeswax and candelilla wax at 70-80°C to obtain an oil phase liquid.

[0017] 4) Add the formulated amount of polydimethylsiloxane and sodium hyaluronate to the oil phase liquid whose temperature has dropped to 60°C, and fully dissolve them in the mixed oil phase liquid.

[0018] 5) Add the formulated amount of dried soluble fiber and chitosan into a deionized water solution containing 1% glacial acetic acid and fully dissolve them; dissolve the anhydrous ethanol used for cochineal red and evenly disperse the pigment to obtain an aqueous phase liquid.

[0019] 6) While stirring, first slowly drop the aqueous phase into the obtained mixed oil phase, then add mica powder, strawberry essence and ethyl paraben. After the addition is complete, continue stirring to fully blend all the ingredients to obtain lip gloss liquid.

[0020] 7) Pour the stirred lip gloss liquid into the lip gloss tube and let it cool naturally.

[0021] The third object of the present invention is to provide the use of a dried soluble fiber product in the preparation of a lip gloss or lipstick having antioxidant properties and anti-photorepair properties.

[0022] Beneficial effects of the present invention: The soluble fiber dried product provided by the present invention can have water solubility and antioxidant functions, as well as anti-photooxidation performance and stability, and can be used to prepare color-retaining water-glossy lip gloss.

[0023] In addition, the soluble fiber dried product is combined with other raw materials, and the method of the present invention allows the soluble fiber dried product in the lip gloss to be loaded and wrapped by other raw material components, so that its anti-photooxidation performance and stability are improved and can have a long-lasting effect. By combining the soluble fiber dried product with other raw materials, the lip gloss sample prepared by the method of the present invention also has the effect of repairing human keratinocyte DNA and cell nucleus damage induced by ultraviolet radiation.

[0024] In addition, the color-retaining water-gloss lip gloss provided by the present invention has high color rendering, stable color, and strong water-gloss feeling. It can form a layer of fine reflective film on the surface of the lips to reflect light, creating a crystal clear, moist and full gloss, making the lips look more three-dimensional and fuller, as if a layer of crystal water film has just been applied, adding to the charm and attractiveness of the lips.

[0025] In addition, the color-retaining water-gloss lip gloss provided by the present invention can partially wrap the soluble fiber in it and release it continuously by adding the soluble fiber dried product and the preparation method provided by the present invention, so that the lips can maintain a charming water-gloss luster for a long time.

[0026] In addition, the color-retaining water-gloss lip gloss provided by the present invention can nourish and repair the skin, repair skin cell nucleus and DNA damage induced by ultraviolet radiation, improve the microcirculation of the lip skin, promote cell metabolism, repair damaged lip skin, enhance the resistance of the lip skin, reduce the damage of the external environment to the lips, and make the lip skin healthier and more elastic by adding the soluble fiber dried product and the preparation method provided by the present invention.

[0027] In addition, the protective film formed on the lips by adding polydimethylsiloxane to the color-retaining water-glossy lip gloss provided by the present invention has good adhesion and durability, and can be closely attached to the lip surface to prevent the lip gloss from easily falling off. Even when eating, drinking water or when the lips are more active, the lip gloss can remain relatively intact, and it is not easy to fade or smudge on a large area, thereby extending the durability of the lip makeup.

[0028] In addition, the color-retaining water-gloss lip gloss provided by the present invention can synergize with other ingredients by adding soluble fiber dried products, polydimethylsiloxane and chitosan, so that the lip gloss can be better attached to the lip skin and form a long-lasting color-retaining effect. At the same time, under the protection of the film-forming agent, the pigment is not easily affected by external factors and falls off, further enhancing the color-retaining ability of the lip gloss, so that users can maintain beautiful lip makeup all day without frequent makeup touch-ups.

[0029] In addition, the raw materials used in the color-retaining water-glossy lip gloss provided by the present invention are all safe raw materials of food grade or cosmetic grade, such as jojoba oil, beeswax, sodium hyaluronate, cochineal red, mica powder, etc. These raw materials have been strictly screened and tested, have less irritation to human skin, and are relatively safe. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 The peanut oil peroxide value of defatted pistachios, the dried soluble fiber product provided in Example 1, and the dried soluble fiber product provided in Comparative Example 1.

[0031] Figure 2 The flavan-3-ol content of defatted pistachios, the dried soluble fiber product provided in Example 1, and the dried soluble fiber product provided in Comparative Example 1.

[0032] Figure 3 The 30-day DPPH removal rates of the color-retaining water-glossy lip glosses provided in Example 2, Comparative Example 2, Comparative Example 3 and Comparative Example 4, respectively.

[0033] Figure 4 The 30-day ABTS clearance rates of the color-retaining glossy lip glosses provided in Example 2, Comparative Example 2, Comparative Example 3 and Comparative Example 4, respectively.

[0034] Figure 5 The percentage of comet tail DNA in HaCaT cells induced by UVB in the blank group, UVB group, Example 2 group, Comparative Example 2 group, Comparative Example 3 group and Comparative Example 4 group.

[0035] Figure 6 The fluorescence intensity of γH2Ax of HaCaT cells induced by UVB in the blank group, UVB group, Example 2 group, Comparative Example 2 group, Comparative Example 3 group and Comparative Example 4 group. DETAILED DESCRIPTION

[0036] In order to make the purpose, technical scheme and advantages of the present invention more clear, the present invention is further described in detail below in combination with the groups. It should be understood that the specific groups described herein are only used to explain the present invention and are not used to limit the present invention. The reagents not described in detail in the present invention are all conventional reagents and can be obtained from commercial channels; the methods not described in detail are all conventional experimental methods and can be obtained from the prior art.

[0037] Embodiment 1: 1) After washing and drying the pistachios, the pistachios are squeezed to obtain defatted pistachio residue, which is then ground to obtain defatted pistachio powder.

[0038] 2) Add defatted pistachio powder to an aqueous solution of alkaline protease (food grade, Shandong Longkote) containing 6% of the weight of defatted pistachio powder, and perform enzymatic hydrolysis in a water bath at 55°C and 500W for 30 min; 3) Adjust the pH of the solution to 4.8 with 3M glacial acetic acid, add thermostable α-amylase (food grade, Shandong Xinxiong Biological) at a final concentration of 8% of the weight of defatted pistachio powder, and perform ultrasonic enzymolysis in a water bath at 90°C and 500W for 45 minutes; 4) Boil in water for 10 min to obtain the first enzyme inactivation solution; 5) After cooling, add 5% of the weight of defatted pistachio powder to the first enzyme-killing solution, cellulase (food grade, Shandong Longkote), and perform ultrasonic enzymolysis at 60°C and 350W for 40 minutes; 6) Boil in water for 10 min to obtain the second enzyme inactivation solution; 7) After cooling, centrifuge the second enzyme inactivation solution at 6000 rpm for 10 min and take the supernatant; 8) Concentrate, add 4 times the volume of 95 ethanol preheated to 60°C, treat for 1 hour, centrifuge at 6000rpm for 10 minutes, and dry at 50°C to obtain the soluble fiber dry product.

[0039] Comparative Example 1: 1) After washing and drying the pistachios, the pistachios are squeezed to obtain defatted pistachio residue, which is then ground to obtain defatted pistachio powder.

[0040] 2) Add defatted pistachio powder into boiling water and soak at 100℃ for 2h; 3) Filter and take the filtrate; 4) Concentrate, add 4 times the volume of 95 ethanol preheated to 60°C, treat for 1 hour, centrifuge at 6000rpm for 10 minutes, and dry at 50°C to obtain the soluble fiber dry product.

[0041] Property determination: 1. Solubility Weigh 0.5 g (m1) sample into a beaker, add 50 mL distilled water, stir well, incubate at 75 °C in a water bath for 1 h, centrifuge at 5500 r / min for 15 min, collect the supernatant and dry in a 105 °C oven to constant weight, weigh the residue mass (m2), and calculate the solubility (%) = (m2 / m1) × 100%.

[0042] As a result, the average solubility of the defatted pistachio powder was 28.65%, the average solubility of the dried soluble fiber provided in Example 1 was 91.08%, and the average solubility of the dried soluble fiber provided in Comparative Example 1 was 59.63%, which indicates that the dried soluble fiber obtained by the method provided in Example 1 has stronger solubility.

[0043] 2. Antioxidant test of peanut oil Accurately weigh 10g of peanut oil and put it into a 50mL conical flask. Then accurately weigh 1mg of defatted pistachio powder, the dried soluble fiber provided in Example 1, or the dried soluble fiber provided in Comparative Example 1 and add them to the peanut oil. Slightly heat to dissolve and disperse the antioxidant, and then put it into a constant temperature oven at 28°C. After 50 minutes, take a sample to measure the peroxide value (POV) of the peanut oil. Perform the same operation on a conical flask with only peanut oil as a blank control.

[0044] like Figure 1 As shown, the POV of the defatted pistachio powder is comparable to that of the blank control, while the average POV value of the dried soluble fiber provided in Example 1 is significantly lower than that of the blank control and the defatted pistachio powder, indicating that the dried soluble fiber obtained by the method provided in Example 1 has stronger antioxidant properties against peanut oil.

[0045] 3. Detection of flavan-3-ols Sample treatment: 1.2 g of the dried soluble fiber provided in Example 1 or Comparative Example 1 was extracted three times with petroleum ether to remove impurities, and the solution was fixed to 5 mL with methanol to obtain a sample solution. 1.2 g of defatted pistachios were mixed into 5 mL of 75% ethanol solution, ultrasonically extracted at 200 W and 25 ° C for 20 min, centrifuged at 4 ° C and 1000 rpm for 20 min, and the extraction was repeated three times. The supernatant was repeatedly extracted with petroleum ether for three times to remove impurities. Take 0.5 mL of the solution after impurities removal, add methanol to the volume to 5 mL, and obtain a sample solution.

[0046] Detection: 1 mL of sample solution or standard solution of flavan-3-ol (10, 20, 50, 100, 500, 1000 ng / mL) was filtered and loaded onto an Extend C18 column (2.1 mm × 50 mm, 1.9 μm). Mobile phase A was 0.1% formic acid solution, mobile phase B was 100% methanol, column temperature was 30 °C, flow rate was 0.2 mL / min, and injection volume was 2 μL. The standard curve was drawn with the chromatographic peak area of ​​the standard solution as the ordinate and the mass concentration of the standard solution as the abscissa to obtain the linear regression equation. The concentration of flavan-3-ol in the sample solution was calculated based on the linear regression equation and the chromatographic peak area of ​​the sample solution, and then the content of flavan-3-ol in the sample was calculated.

[0047] like Figure 2 As shown, the average content of flavan-3-ol in the defatted pistachio powder is 25.36 μg / g, the average content of flavan-3-ol in the dried soluble fiber provided in Example 1 is 205.51 μg / g, and the average content of flavan-3-ol in the dried soluble fiber provided in Comparative Example 1 is 41.25 μg / g, which indicates that the dried soluble fiber obtained by the method provided in Example 1 has a higher content of flavan-3-ol.

[0048] Preparation of color-retaining water-gloss lip gloss Embodiment 2: Preparation of raw materials for color-fixing water-gloss lip gloss: 10 g of dried soluble fiber: provided in Example 1.

[0049] 5g jojoba oil (food grade, Wuhan Jiyesheng Chemical): has good moisturizing and stability, and can provide basic moisturizing effect for lip gloss.

[0050] 1g beeswax (food grade, Wuhan Jiyesheng Chemical): can increase the consistency of lip gloss and make it easier to shape.

[0051] 0.5g candelilla wax (food grade, Wuhan Jiyesheng Chemical): helps to improve the gloss and hardness of lip gloss.

[0052] 1g polydimethylsiloxane (MW 63,000, food grade, Alfa Aesar (China) Chemical Co., Ltd.): It can form a thin protective film on the lips, which can prevent the lip gloss from coming off easily.

[0053] 2g Chitosan: Chitosan (powder, low viscosity: <200 mPa.s, food grade, Shanghai Aladdin) is a natural high molecular weight polysaccharide with good biocompatibility, film-forming and antibacterial properties. It can form a protective film around the soluble fiber dry product to enhance the protection of the fiber, and its positively charged characteristics can interact with negatively charged substances to further stabilize the encapsulation structure.

[0054] 0.2g sodium hyaluronate, sodium hyaluronate (USP grade, Nanjing Romaimei Biological) has strong moisturizing ability, can absorb and lock a large amount of moisture, keeping the lips hydrated.

[0055] 0.1g cochineal red (food grade, Shaanxi Panier Biotechnology): The amount can be adjusted according to personal preference for color depth to achieve the ideal color effect.

[0056] 0.3g mica powder (food grade, Shanghai Jiader): Adding mica powder can give the lip gloss a unique gloss and create a watery effect.

[0057] 0.05g strawberry flavor (food grade, Jiangxi Zhonghuan Biological): increases the pleasure during use.

[0058] 0.03g ethyl paraben (food grade, Nanjing Kaifusi Chemical): prevents the lip gloss from deteriorating during storage.

[0059] Preparation steps: 1) Place jojoba oil, beeswax and candelilla wax in a clean glass container, heat in a water bath at 70-80°C, and stir continuously with a glass rod until the waxes are completely melted and the oil phase and waxes are fully mixed to obtain an oil phase liquid.

[0060] 2) Add polydimethylsiloxane and sodium hyaluronate to the oil phase liquid whose temperature has dropped to 60°C, and continue stirring to allow them to fully dissolve in the mixed oil phase liquid.

[0061] 3) Add the dried soluble fiber and chitosan to 50 mL of deionized water containing 1% glacial acetic acid, stir evenly to fully dissolve; dissolve cochineal red in 50 mL of anhydrous ethanol, and slowly add it to the aqueous solution containing the dried soluble fiber and chitosan, stirring while adding to ensure that the pigment is evenly dispersed to achieve the desired color, thereby obtaining an aqueous phase liquid.

[0062] 4) Under stirring, first slowly add the aqueous phase liquid to the obtained mixed oil phase liquid, the dropping process lasts for about 30 minutes, then add mica powder, strawberry essence and ethyl paraben. After the dropping is completed, continue stirring for 2 hours to allow all the ingredients to fully blend to obtain lip gloss liquid.

[0063] 5) Pour the stirred lip gloss liquid into the lip gloss tube and let it cool naturally.

[0064] In this way, a homemade color-staying water-gloss lip gloss is ready. When using it, gently apply it on the lips to show a charming lip makeup effect with long-lasting color and water-gloss. It should be noted that homemade lip gloss should be stored in a cool and dry place, avoid direct sunlight, and use it as soon as possible to ensure its quality and safety.

[0065] Comparative Example 2: 10 g of the dried soluble fiber provided in Comparative Example 1 was added, and the other raw materials of the color-fixing watery lip gloss were the same as those in Example 2.

[0066] Comparative Example 3: The raw materials of the color-retaining glossy lip gloss provided in Comparative Example 3 are: 10g of the dried soluble fiber provided in Example 1, 5g of jojoba oil, 1g of beeswax, 0.5g of candelilla wax, 1g of polydimethylsiloxane, 0.1g of cochineal red, 0.3g of mica powder, 0.05g of strawberry essence, and 0.03g of ethyl paraben. The preparation steps are: The preparation steps are: 1) Place jojoba oil, beeswax and candelilla wax in a clean glass container, heat in a water bath at 70-80℃, and stir continuously with a glass rod until the waxes are completely melted and the oil phase and waxes are fully mixed to obtain an oil phase liquid.

[0067] 2) Add the dried soluble fiber, polydimethylsiloxane and sodium hyaluronate to the oil phase liquid whose temperature has dropped to 60°C, and continue stirring to fully dissolve them in the mixed liquid.

[0068] 3) Prepare carmine solution: Dissolve carmine in 100 mL of anhydrous ethanol and slowly add it to the above mixture while stirring to ensure that the pigment is evenly dispersed to achieve the desired color.

[0069] 4) While stirring, slowly add mica powder, strawberry essence and ethyl paraben to the mixed system obtained in step 3) dropwise for about 30 minutes. After the addition is completed, continue stirring for 2 hours to allow all ingredients to fully blend to obtain lip gloss liquid.

[0070] 5) Pour the stirred lip gloss liquid into a clean lip gloss tube while it is still hot, taking care to avoid creating bubbles. After filling, allow the lip gloss to cool naturally to room temperature.

[0071] Comparative Example 4: The raw materials of the color-retaining water-glossy lip gloss provided in Comparative Example 4 are: 10g squalane, 5g jojoba oil, 1g beeswax, 0.5g candelilla wax, 1g polydimethylsiloxane, 0.2g sodium hyaluronate, 0.1g cochineal red, 0.3g mica powder, 0.05g strawberry essence, and 0.03g ethyl paraben. The preparation steps are: 1) Place squalane, jojoba oil, beeswax and candelilla wax in a clean glass container, heat in a water bath at 70-80°C, and stir continuously with a glass rod until the waxes are completely melted and the oil phase and waxes are fully mixed to obtain an oil phase liquid.

[0072] 2) Add polydimethylsiloxane and sodium hyaluronate to the oil phase liquid whose temperature has dropped to 60°C, and continue stirring to allow them to fully dissolve in the mixed liquid.

[0073] 3) Prepare carmine solution: Dissolve carmine in 100 mL of anhydrous ethanol and slowly add it to the above mixture while stirring to ensure that the pigment is evenly dispersed to achieve the desired color.

[0074] 4) While stirring, slowly add mica powder, strawberry essence and ethyl paraben to the mixed system obtained in step 3) dropwise for about 30 minutes. After the addition is completed, continue stirring for 2 hours to allow all ingredients to fully blend to obtain lip gloss liquid.

[0075] 5) Pour the stirred lip gloss liquid into a clean lip gloss tube while it is still hot, taking care to avoid creating bubbles. After filling, allow the lip gloss to cool naturally to room temperature.

[0076] Test of lip gloss antioxidant properties: The lip glosses provided in Example 2 and Comparative Examples 2 to 4 were placed in a light incubator under a light intensity of 3500 LX for 30 days. Samples were taken on the 1st, 5th, 10th, 20th and 30th days to detect the scavenging rates of DPPH free radicals and ABTS cation free radicals, and to explore the effect of light on the stability of polyphenols and polyphenol-chitosan nanoparticles.

[0077] Accurately weigh 10 mg of DPPH, add it to a 250 mL volumetric flask, dissolve it in anhydrous ethanol and make up to 1×10 -4 M DPPH reaction solution, stored in the dark. Use 3.8 mL of DPPH reaction solution to dissolve 0.2 mL of lip gloss sample solution, and keep it sealed at room temperature. After 30 min, measure the absorbance at 517 nm. DPPH free radical scavenging rate = (1 −(A1 − A2) / A0) × 100%; where: A1—0.2 mL sample solution + 3.8 mL DPPH solution absorbance; A2—0.2 mL sample solution + 3.8 mL anhydrous ethanol absorbance; A0—0.2 mL anhydrous ethanol + 3.8 mL DPPH solution absorbance.

[0078] Take 10 μL of lip gloss sample solution and mix it with 200 μL of ABTS reaction solution, react in the dark, and measure the absorbance at 734 nm after 6 minutes. ABTS free radical scavenging rate = (A0 − A1) / A0 × 100%; where: A0—200 μL ABTS working solution + 10 μL anhydrous ethanol absorbance; A1—200 μL ABTS working solution + 10 μL sample absorbance.

[0079] like Figure 3 and 4 As shown, the lip gloss provided in Example 2 maintained very high DPPH and ABTS clearance rates within 30 days. Although the lip gloss provided in Comparative Example 3 had high DPPH and ABTS clearance rates on the first day, its DPPH and ABTS clearance rates continued to decline within 30 days, and its anti-photooxidation performance stability was poor. Although the lip gloss provided in Comparative Example 2 maintained relatively stable DPPH and ABTS clearance rates within 30 days, they were significantly lower than those in Example 2. The lip gloss provided in Comparative Example 4 not only had difficulty in maintaining stable DPPH and ABTS clearance rates, but its DPPH and ABTS clearance rates were also significantly lower than those in Example 2.

[0080] Compared with Example 2, the only difference in Comparative Example 2 is that the raw material used is the dried soluble fiber provided in Comparative Example 1, which not only has lower solubility and antioxidant properties than the dried soluble fiber provided in Example 1, but also has a lower flavan-3-ol content than Example 1. As a result, although the lip gloss provided in Comparative Example 2 maintains a relatively stable DPPH clearance rate and ABTS clearance rate within 30 days, they are significantly lower than those in Example 2.

[0081] Compared with Example 2, although Comparative Example 3 uses the soluble fiber dried product provided in Example 1, the other raw materials and preparation steps of its lip gloss are different, resulting in a continuous decrease in its DPPH removal rate and ABTS removal rate within 30 days, and its anti-photooxidation performance stability is poor.

[0082] Compared with Example 2, Comparative Example 4 did not use the soluble fiber dry product and other ingredients provided in Example 1 as raw materials, resulting in low and continuously decreasing DPPH removal rates and ABTS removal rates within 30 days, and poor stability of its anti-photooxidation performance.

[0083] This shows that the color-retaining water-glossy lip gloss prepared by using the raw materials and method provided by the present invention not only has excellent anti-photooxidation performance, but also has very high stability.

[0084] Cell Testing: 1. DNA damage repair effect on human keratinocytes (HaCaT) 1) Lay the first layer of gel: Use PBS to prepare 25 ml of normal melting point 0.5% agarose (5 mg / ml), cover with plastic wrap, poke a few holes, and heat repeatedly in a microwave oven for 10 seconds each time until it is clear. Put the frosted end of the slide into the agarose, remove it and wipe the bottom clean, put it in a 60°C oven after solidification, and leave it for 1 day; 2) HaCaT cells were seeded in 6-well plates, with 10 cells per well. 5 cells, and the plate was placed in an incubator at 37°C and 5% CO2 for 24 h, and divided into a control group, a UVB group, an example 2 group, a comparative example 2 group, a comparative example 3 group, and a comparative example 4 group. The lip glosses of example 2, comparative example 2, comparative example 3, and comparative example 4 placed under a light intensity of 3500 LX for 15 days were respectively coated on a glass slide that can penetrate UVB, and the coating thickness was about 0.1 mm. The control group and the UVB group were not coated.

[0085] 3) The HaCaT cells in each group were exposed to 60 mJ / cm 2 UVB made the cell survival rate of the UVB group reach 60%; the control group was not exposed.

[0086] 4) Collect cells from each group and resuspend them in PBS to a density of 10 6 Pieces / ml; 5) Lay the second layer of gel: prepare 0.7% low melting point agarose (7mg / ml), cover with plastic wrap, poke a few holes, and heat repeatedly in a microwave oven for 10 seconds each time. After it is completely dissolved, transfer to a 37℃ oven for later use. Mix 10μL of cells and 75ul of 0.7% low melting point agarose evenly, spread on the first layer of gel, cover with a coverslip, and put in a 4℃ refrigerator for 10 minutes to solidify the second layer of agarose. 6) Cell lysis: Remove the coverslip horizontally, place the slide in a plate, pour in pre-cooled cell lysis buffer (add 1 ml of DMSO to every 9 ml before use), lyse at 4°C for 2 h, remove the slide and rinse with PBS; 7) DNA alkaline unwinding: Place the slide in a horizontal electrophoresis tank. Pour in the newly prepared alkaline electrophoresis buffer, covering the slide surface by about 0.25 cm, and place at room temperature for 20 min, so that the DNA can unwind under alkaline conditions and produce alkaline denaturable segments, making it easier for DNA breaks to migrate in the electric field; 8) Single cell electrophoresis: voltage 25V, current 200mA for 30 min. The voltage and current can be adjusted by changing the buffer level. 9) Neutralize the staining solution: After electrophoresis, place the slide in a plate, add 0.4 mM Tris-HCL (pH=7.5) buffer, immerse the slide, neutralize at 4℃ for 3 times, 10 minutes each time, and discard the Tris-HCL buffer; 10) Add 40 μL PI to each slide for staining, cover it with a thin film glove to prevent evaporation and spread the liquid evenly, and stain for 10 minutes away from light; 11) After fluorescent staining, photos were taken under a fluorescent microscope at 545 nm and the percentage of comet tail DNA content was evaluated using CASP1.2.3 (Casplab, Poland). The comet tail DNA% was used as an indicator of DNA damage. The experiment was repeated 3 times.

[0087] Comet assay was used to reflect the damage of UVB to HaCaT cells. Cells with red tail fluorescence were observed under a fluorescence microscope. Red tail cells represent cells that are positive for comet assay, which means DNA damage of HaCaT cells. CASP was used to quantitatively analyze the red tail cells in the image. The statistical results of comet tail DNA% are shown in the figure. Figure 5As shown. Compared with the control group, the cell DNA damage in the UVB group increased significantly, indicating that ultraviolet radiation caused damage to the DNA of HaCaT cells, and the lip gloss provided in Example 2 can reduce the comet tail DNA% ratio, indicating that the lip gloss provided in Example 2 can resist the DNA damage induced by UVB. However, the lip gloss provided in Comparative Examples 2 to 4 is not as effective as Example 2 in resisting UVB-induced DNA damage.

[0088] This shows that the color-retaining water-glossy lip gloss prepared by the raw materials and method provided by the present invention can improve the effect of the lip gloss in resisting UVB-induced DNA damage.

[0089] 2. Repair effect on nuclear damage of human keratinocytes (HaCaT) 1) HaCaT cells were seeded in 6-well plates, with 10 cells per well. 5 cells, and the plate was placed in an incubator at 37°C and 5% CO2 for 24 h, and divided into a control group, a UVB group, an example 2 group, a comparative example 2 group, a comparative example 3 group, and a comparative example 4 group. The lip glosses of example 2, comparative example 2, comparative example 3, and comparative example 4 placed under a light intensity of 3500 LX for 15 days were respectively coated on a glass slide that can penetrate UVB, and the coating thickness was about 0.1 mm. The control group and the UVB group were not coated.

[0090] 3) The HaCaT cells in each group were exposed to 60 mJ / cm 2 UVB made the cell survival rate of the UVB group reach 60%; the control group was not exposed.

[0091] 4) Fix HaCaT cells with paraformaldehyde for 20 min and dry at room temperature for 10 min; 5) Wash with PBS three times, 3 min each time, and then immerse in 1% Triton for 30 min; 6) Wash with PBS five times for 2 min each time, incubate with sheep serum at 37°C for 20 min, add primary antibody γH2Ax (Abcam, UK) and incubate at 4°C overnight; 7) Wash with PBS at 4°C for 5 times, 3 min each time, and then add secondary antibody anti-rabbit IgG H&L (Alexa Fluor 488) Abcam, UK) and incubate at 37°C for 50 min; 8) Wash with PBS 5 times, 3 minutes each time, add DAPI, and finally record the fluorescence image with a fluorescence inverted microscope. Blue fluorescence represents DAPI, and green fluorescence represents γH2Ax-positive cells. Image J 7.0 was used to calculate the green fluorescence intensity.

[0092] γH2Ax was used to reflect the damage of the cell nucleus. After fluorescent staining, the cells with positive γH2Ax staining were observed under a fluorescent microscope. The blue color was DAPI staining, which located all HaCaT cells. The green-stained cells represented the cells with positive γH2Ax staining, which represented the damage of the HaCaT cell nucleus. Figure 6 As shown, compared with the control group, the nuclear damage of HaCaT cells in the UVB group increased significantly, indicating that ultraviolet radiation caused damage to the HaCaT cell nucleus, and the lip gloss provided in Example 2 can reduce the fluorescence intensity of γH2Ax, indicating that the lip gloss provided in Example 2 can resist the nuclear damage induced by UVB. However, the lip gloss provided in Comparative Examples 2 to 4 is not as effective as Example 2 in resisting UVB-induced DNA damage.

[0093] Compared with Example 2, the only difference in Comparative Example 2 is that the raw material used is the dried soluble fiber product provided in Comparative Example 1, which not only has lower solubility and antioxidant properties than the dried soluble fiber product provided in Example 1, but also has a lower flavan-3-ol content than Example 1. As a result, the lip gloss provided in Comparative Example 2 is not as effective as Example 2 in repairing UVB-induced DNA and nuclear damage in human keratinocytes.

[0094] Compared with Example 2, although Comparative Example 3 uses the dried soluble fiber product provided in Example 1, the other raw materials and preparation steps of the lip gloss are different, resulting in that the lip gloss provided in Comparative Example 3 is not as effective as that in Example 2 in repairing UVB-induced human keratinocyte DNA and cell nucleus damage.

[0095] Compared with Example 2, Comparative Example 4 does not use the soluble fiber dry product and other ingredients provided in Example 1 as raw materials, resulting in that the lip gloss provided in Comparative Example 4 has less repair effects on human keratinocyte DNA and cell nucleus damage induced by UVB than that in Example 2.

[0096] This shows that the color-retaining water-gloss lip gloss prepared by the raw materials and method provided by the present invention can improve the UVB-induced human keratinocyte DNA and cell nucleus damage repair effect of the lip gloss.

[0097] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by any technician familiar with the technical field within the technical scope disclosed by the present invention should be covered within the protection scope of the present invention.

Claims

1. A method for preparing a soluble fiber dry product, characterized in that: include: defatting pistachios to obtain defatted pistachio powder; After using alkaline protease to ultrasonically hydrolyze defatted pistachio powder, adding high temperature resistant α-amylase to perform ultrasonic hydrolysis to inactivate the enzyme, thereby obtaining a first enzyme-inactivating solution; Adding cellulase to the first enzyme-killing solution to perform ultrasonic enzymolysis to kill the enzyme, thereby obtaining a second enzyme-killing solution; The second enzyme-inactivated solution is centrifuged, the supernatant is taken, concentrated, treated with 95% ethanol, centrifuged and dried, and the precipitate is the soluble fiber dry product.

2. The preparation method according to claim 1, characterized in that: The amount of alkaline protease added was 6% of the weight of defatted pistachio powder, and ultrasonic enzymatic hydrolysis was carried out in a water bath at 55 °C and 500 W for 30 min; After alkaline protease hydrolysis, the solution pH was adjusted to 4.8 with 3M glacial acetic acid, and the amount of thermostable α-amylase added was 8% of the weight of defatted pistachio powder. Ultrasonic enzymatic hydrolysis was carried out in a water bath at 90°C and 500W for 45min. The amount of cellulase added was 5% of the weight of defatted pistachio powder, and ultrasonic enzymolysis was performed at 60°C and 350W for 40 minutes.

3. A color-retaining water-gloss lip gloss, characterized in that: The raw materials include, by weight, 800-1500 parts of a dried soluble fiber product prepared by the preparation method according to claim 1 or 2, 400-600 parts of jojoba oil, 80-120 parts of beeswax, 30-60 parts of candelilla wax, 80-120 parts of polydimethylsiloxane, 100-300 parts of chitosan, 10-30 parts of sodium hyaluronate, 5-15 parts of cochineal red, 20-40 parts of mica powder, 2-8 parts of strawberry essence and 2-8 parts of ethyl paraben.

4. The color-retaining water-gloss lip gloss according to claim 3, characterized in that: The raw materials include, by weight, 800 parts of dried soluble fiber, 600 parts of jojoba oil, 120 parts of beeswax, 30 parts of candelilla wax, 120 parts of polydimethylsiloxane, 100 parts of chitosan, 30 parts of sodium hyaluronate, 15 parts of cochineal, 20 parts of mica powder, 2 parts of strawberry flavor and 2 parts of ethyl paraben.

5. The color-retaining water-gloss lip gloss according to claim 3, characterized in that: The raw materials include, by weight, 1500 parts of dried soluble fiber, 400 parts of jojoba oil, 80 parts of beeswax, 60 parts of candelilla wax, 80 parts of polydimethylsiloxane, 300 parts of chitosan, 10 parts of sodium hyaluronate, 5 parts of cochineal, 40 parts of mica powder, 8 parts of strawberry flavor and 8 parts of ethyl paraben.

6. The color-retaining water-gloss lip gloss according to claim 3, characterized in that: The raw materials include, by weight, 1000 parts of dried soluble fiber, 500 parts of jojoba oil, 100 parts of beeswax, 50 parts of candelilla wax, 100 parts of polydimethylsiloxane, 200 parts of chitosan, 20 parts of sodium hyaluronate, 10 parts of cochineal, 30 parts of mica powder, 5 parts of strawberry flavor and 3 parts of ethyl paraben.

7. The color-fixing water-gloss lip gloss according to claim 3, characterized in that: The soluble fiber dry product is prepared from pistachios, has an average solubility of 91.08%, and an average flavan-3-ol content of 205.51 μg / g.

8. A method for preparing a color-retaining water-gloss lip gloss, characterized in that: include: 1) Preparing a soluble fiber dry product; 2) Provide 800-1500 parts of dried soluble fiber, 400-600 parts of jojoba oil, 80-120 parts of beeswax, 30-60 parts of candelilla wax, 80-120 parts of polydimethylsiloxane, 100-300 parts of chitosan, 10-30 parts of sodium hyaluronate, 5-15 parts of cochineal, 20-40 parts of mica powder, 2-8 parts of strawberry flavor and 2-8 parts of ethyl paraben; 3) Mix and melt the formulated amounts of jojoba oil, beeswax and candelilla wax at 70-80°C to obtain an oil phase liquid; 4) Add the formulated amount of polydimethylsiloxane and sodium hyaluronate to the oil phase liquid whose temperature has dropped to 60°C, and fully dissolve them in the mixed oil phase liquid; 5) Add the formulated amount of dried soluble fiber and chitosan to a deionized water solution containing 1% glacial acetic acid and fully dissolve them; dissolve the anhydrous ethanol used for cochineal red until the pigment is evenly dispersed to obtain an aqueous phase liquid; 6) While stirring, first slowly drop the aqueous phase into the obtained mixed oil phase, then add mica powder, strawberry essence and ethyl paraben. After the dropwise addition is completed, continue stirring to fully blend all the ingredients to obtain lip gloss liquid; 7) Pour the stirred lip gloss liquid into the lip gloss tube and let it cool naturally.

9. Use of the dried soluble fiber product obtained by the method of claim 1 or 2 in the preparation of lip gloss or lipstick with antioxidant and light-resistant repair properties.

Citation Information

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