Preparation method of algae component with ultraviolet absorption and application thereof in sunscreen cosmetics
By combining algae ingredients with ultraviolet absorption with traditional sunscreens, the skin and environmental hazards caused by the use of chemical sunscreens in the prior art were solved, and the goal of significantly improving the sunscreen effect and reducing potential hazards was achieved.
Patent Information
- Application Number
- CN202510046075.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Priority Date
- 2024-10-12
- Filing Date
- 2025-01-10
- Publication Date
- 2025-04-04
AI Technical Summary
The prior art is prone to increase the use of chemical sunscreen agents when increasing the sunscreen index SPF, resulting in potential harm to the skin and the environment, and lacks the auxiliary effect of non-sunscreen agents on skin sunscreen.
Using a preparation method of algae components with ultraviolet absorption, algae components with a solvent are mixed and ultrasonic extraction is performed. After obtaining the extracted product, cell debris and insoluble impurities are removed, and the algae components with sun protection and synergistic effect are prepared. This algae ingredient combined with traditional sunscreen can significantly improve the sunscreen effect.
This method not only reduces the use of chemical sunscreens and reduces potential hazards to the skin and the environment, but also significantly improves sun protection, providing longer-lasting and comprehensive UV protection, while maintaining the gentleness and naturalness of the sunscreen composition.
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Abstract
Description
Technical Field
[0001] The invention relates to a preparation method of an algae component with ultraviolet absorption and application of the algae component in sunscreen cosmetics, belonging to the field of cosmetics and skin care products. Background Art
[0002] The main mechanisms of skin photoaging caused by ultraviolet rays include oxidative stress, inflammatory response, cell apoptosis, and degradation of collagen and elastin. Long-term exposure to ultraviolet rays can cause skin problems such as erythema, edema, thickening, pigmentation, cell sunburn, immunosuppression, photoaging, and tumors. Ultraviolet radiation causes oxidative stress in skin tissue, generates excessive reactive oxygen species (ROS), destroys the integrity of cell membranes and the antioxidant system in cells, and then causes cell inflammation, cell apoptosis, and tumor formation.
[0003] With environmental changes and ozone layer depletion, people's awareness of skin protection continues to increase, and the market demand for high SPF (Sun Protection Factor) sunscreen products is also increasing. The selection of sunscreen agents is the core of sunscreen products. Therefore, the development of high SPF sunscreen compositions has become a research hotspot. The most direct way to increase the sun protection index is to increase the amount of sunscreen agents added, but many sunscreen agents are irritating and photosensitizing. The higher the concentration, the greater the risk of causing allergies, and excessive addition of sunscreen agents is also subject to regulatory restrictions.
[0004] The main methods for improving the SPF of sunscreen formulas in the prior art include: utilizing the synergistic effect between sunscreens to improve the SPF value and prevent skin allergies caused by excessive use of ultraviolet absorbers. Adding film-forming ingredients to form a continuous film with a certain thickness of matrix after application. However, the existing technical solutions for improving SPF mainly focus on the use of sunscreens, ignoring the auxiliary role of non-sunscreens in skin sun protection.
[0005] Therefore, it has become a technical problem to be solved urgently to develop a sunscreen product that can reduce potential harm to the skin and the environment, significantly improve the sunscreen effect, and provide more lasting and comprehensive ultraviolet protection. Summary of the invention
[0006] Problem that the invention aims to solve
[0007] In view of the technical problems existing in the prior art, the present invention first provides a method for preparing an algae component with ultraviolet absorption. The algae component obtained by the preparation method has a sunscreen synergistic effect, which can not only reduce the use of chemical sunscreens and reduce potential harm to the skin and the environment, but also significantly improve the sunscreen effect and provide more lasting and comprehensive ultraviolet protection.
[0008] Furthermore, the present invention also provides a sunscreen composition. The sunscreen composition of the present invention has a simple composition and excellent sunscreen effect, while maintaining the mildness and naturalness of the sunscreen composition, reducing irritation to the skin, and meeting environmental protection requirements.
[0009] Solutions for solving problems
[0010] [1] A method for preparing an algae component having ultraviolet absorption, comprising the following steps:
[0011] The algae sample is immersed in a solvent and subjected to ultrasonic extraction to obtain an extraction product;
[0012] removing cell debris and insoluble impurities from the extraction product to obtain a purified product;
[0013] The purified product is concentrated to obtain a concentrated solution of algae components.
[0014] [2] The preparation method according to [1] above, wherein the algae sample is derived from desert algae, preferably comprising one or a combination of two or more of Chlorella vulgaris, Microcoleus spp., and Hassarum spp.;
[0015] Preferably, the desert algae is frozen and ground to break cell walls and release cell contents to obtain the algae sample.
[0016] [3] The preparation method according to [1] or [2] above, wherein the mass ratio of the algae sample to the solvent is 1:1 to 100; and / or
[0017] The frequency of the ultrasonic extraction is 20-40 kHz, the time of the ultrasonic extraction is 30-150 minutes, and the temperature of the ultrasonic extraction is 20-30°C.
[0018] [4] The preparation method according to any one of [1] to [3] above, wherein the solvent comprises an organic solvent; preferably, the organic solvent comprises one or a combination of two or more of acetonitrile, acetone, ethanol and methanol.
[0019] [5] The preparation method according to any one of [1] to [4] above, wherein the cell debris and insoluble impurities in the extract are removed by solid-liquid separation;
[0020] Preferably, the solid-liquid separation comprises centrifugal separation and / or filtration separation;
[0021] More preferably, the centrifugal separation comprises centrifugation at a rotation speed of 5000-15000 rpm for 10-20 minutes; and the filtration separation comprises filtration treatment using filter paper or a microporous filter membrane.
[0022] [6] The preparation method according to any one of [1] to [5] above, wherein the purified product is concentrated using a rotary evaporator to remove more than 80 wt% of the solvent; and / or
[0023] Drying the concentrated liquid of the algae component to obtain the algae component;
[0024] Preferably, the content of algae components in the concentrated solution of algae components is 1-10 g / L.
[0025] [7] A sunscreen composition comprising a sunscreen agent and a sunscreen enhancer, wherein the sunscreen enhancer comprises an algae component prepared by the preparation method described in any one of [1] to [6] above; preferably, based on the total mass of the sunscreen composition as 100%, the content of the sunscreen enhancer is 0.01-20%, preferably 0.01-10%; the content of the sunscreen agent is 0.01-20%, preferably 0.01-10%.
[0026] [8] The sunscreen composition according to [7] above, wherein the sunscreen composition further comprises one or a combination of two or more of an emulsifier, an emollient, a thickener, a humectant, a chelating agent, a skin conditioner, a flavoring agent, a preservative, and a pH adjuster;
[0027] Preferably, based on the total mass of the sunscreen composition as 100%, the content of the emulsifier is 0.01-20%, preferably 0.01-10%; the content of the emollient is 0.01-50%, preferably 0.01-20%; the content of the thickener is 0.01-8%, preferably 0.01-1%; the content of the humectant is 0.01-40%, preferably 0.01-20%; the content of the chelating agent is 0-1%, preferably 0-0.08%; the content of the skin conditioner is 0-50%, preferably 0-20%; the content of the flavoring agent is 0-1%, preferably 0-0.2%; the content of the preservative is 0.01-3%, preferably 0.01-2%; the content of the pH adjuster is 0-3%, preferably 0-2%.
[0028] [9] A method for preparing a sunscreen composition according to [7] or [8] above, comprising the step of mixing the components of the sunscreen composition;
[0029] Preferably, the preparation method comprises the following steps:
[0030] Mix the moisturizer, thickener and solvent and heat to 80-90° C. to obtain phase A;
[0031] Mix the emollient, sunscreen, and emulsifier and heat to 80-90°C to obtain phase B;
[0032] After mixing the phase A and the phase B, homogenize at a rotation speed of 2500-3000 rpm for 5-8 minutes to obtain a mixed product;
[0033] Add the preservative and the algae component to the mixed product, and homogenize at a rotation speed of 2500-3000 rpm for 1-3 minutes to obtain a sunscreen composition.
[0034]
[10] Use of the sunscreen composition according to [7] or [8] above for preparing cosmetics; preferably, the cosmetics include sunscreen milk, sunscreen lotion, sunscreen cream, sunscreen liquid, sunscreen spray, sunscreen gel, isolation cream, isolation milk, isolation lotion or BB cream.
[0035] Effects of the Invention
[0036] The preparation method of the algae component with ultraviolet absorption of the present invention is simple and easy, the raw materials are easy to obtain, and it is suitable for mass production. In addition, the algae component obtained by the preparation method of the present invention has a sunscreen synergistic effect, which can not only reduce the use of chemical sunscreens and reduce potential harm to the skin and the environment, but also significantly improve the sunscreen effect and provide more lasting and comprehensive ultraviolet protection.
[0037] The sunscreen composition of the present invention has a simple composition and excellent sunscreen effect, while maintaining the mildness and naturalness of the sunscreen composition, reducing irritation to the skin, and meeting environmental protection requirements. DETAILED DESCRIPTION
[0038] Various exemplary embodiments, features and aspects of the present invention will be described in detail below. The word "exemplary" used here means "used as an example, embodiment or illustrative". Any embodiment described here as "exemplary" is not necessarily interpreted as being superior or better than other embodiments.
[0039] In addition, in order to better illustrate the present invention, numerous specific details are provided in the following specific embodiments. It should be understood by those skilled in the art that the present invention can be implemented without certain specific details. In other examples, methods, means, equipment and steps well known to those skilled in the art are not described in detail in order to highlight the subject matter of the present invention.
[0040] Unless otherwise stated, the units used in this specification are all international standard units, and the numerical values and numerical ranges appearing in the present invention should be understood to include the inevitable systematic errors in industrial production.
[0041] In this specification, the word "may" includes both performing a certain process and not performing a certain process.
[0042] In this specification, the references to "some specific / preferred embodiments", "other specific / preferred embodiments", "embodiments", etc., mean that the specific elements (e.g., features, structures, properties and / or characteristics) described in connection with the embodiments are included in at least one embodiment described herein, and may or may not exist in other embodiments. In addition, it should be understood that the elements may be combined in various embodiments in any suitable manner.
[0043] In this specification, the numerical range expressed using "a numerical value A to a numerical value B" means a range including the endpoints A and B.
[0044] <First aspect>
[0045] A first aspect of the present invention provides a method for preparing an algae component having ultraviolet absorption, comprising the following steps:
[0046] The algae sample is immersed in a solvent and subjected to ultrasonic extraction to obtain an extraction product;
[0047] removing cell debris and insoluble impurities from the extraction product to obtain a purified product;
[0048] The purified product is concentrated to obtain a concentrated solution of algae components.
[0049] The preparation method of the algae component of the present invention is simple and easy, the raw materials are easy to obtain, and it is suitable for mass production. In addition, the algae component obtained by the preparation method of the present invention has a sunscreen synergistic effect, which can not only reduce the use of chemical sunscreens and reduce potential harm to the skin and the environment, but also significantly improve the sunscreen effect and provide more lasting and comprehensive ultraviolet protection.
[0050] In some specific embodiments, the algae sample is derived from desert algae. The inventors of the present invention have found that the mycosporin-like amino acids rich in desert algae have the function of absorbing ultraviolet rays, which can significantly improve the sunscreen efficacy of sunscreen cosmetics containing known traditional sunscreens, thereby reducing the dosage of known traditional sunscreens and making sunscreen cosmetics more gentle and safe. Preferably, the algae sample is derived from one or a combination of two or more of Chlorella, Microcoleus, and Hasa algae. The algae component of the present invention contains mycosporin-like amino acids (MAAs).
[0051] Desert algae show strong survival ability in extreme environments, especially under strong ultraviolet (UV) radiation. They can effectively absorb and resist the damage of ultraviolet rays through a series of biochemical mechanisms and structural characteristics. It is a natural sunscreen synergist with great potential. Its sunscreen synergist mechanism is mainly achieved through the following aspects:
[0052] On the one hand, in terms of ultraviolet absorption, desert algae are rich in mycosporin-like amino acids, which are a class of small molecule compounds that have the ability to absorb ultraviolet rays. Their chemical structure contains conjugated double bonds, which enables them to effectively absorb ultraviolet rays. Mycosporin-like amino acids can absorb ultraviolet rays in the UVA (320-400nm) and UVB (280-320nm) bands, thereby reducing the direct damage of these ultraviolet rays to cells.
[0053] On the other hand, in terms of antioxidant protection, the antioxidants such as astaxanthin, carotenoids and vitamin E rich in desert algae can neutralize reactive oxygen species (ROS) caused by ultraviolet rays and reduce the damage of oxidative stress to skin cells. These antioxidants reduce cell damage and aging by capturing free radicals and preventing them from reacting with cell membranes, DNA and proteins.
[0054] On the other hand, in terms of enhancing the skin barrier function, the moisturizing ingredients in desert algae, such as polysaccharides and other natural moisturizing factors, can enhance the skin's barrier function, maintain the skin's moisture balance, and reduce the damage of ultraviolet rays to the skin barrier. These ingredients help form a protective film and enhance the skin's ability to resist the external environment.
[0055] In terms of synergistic effects, the algae component of the present invention is used in combination with traditional sunscreens to exert a synergistic effect and significantly increase the SPF value of sunscreen products. The algae component of the present invention not only has sunscreen and antioxidant capabilities, but also can enhance the effect of traditional sunscreens, reduce their dosage, and thus reduce skin irritation and allergy risks. By combining the algae component of the present invention with traditional sunscreens, the sunscreen enhancement system of the present invention can significantly increase the SPF value of sunscreen products while maintaining the mildness and naturalness of the formula, reducing irritation to the skin, and meeting environmental protection requirements. By using the algae component of the present invention, not only the effect of sunscreen products is improved, but also safer and more effective skin protection is provided.
[0056] As known in the art, the sunscreen effect is usually characterized by the parameters SPF and PA. Among them, SPF (Sun Protection Factor) refers to the ratio of the energy required to produce the minimum erythema on the skin coated with sunscreen cosmetics to the energy required to produce the same degree of erythema on the skin not coated with sunscreen cosmetics. It is calculated based on the minimum erythema dose of the skin. The calculation method is: assuming that the intensity of ultraviolet rays does not change with time, a person who does not take any sunscreen measures will turn red after staying in the sun for 20 minutes, and when using sunscreen cosmetics with SPF15, it means that the time can be extended by 15 times, that is, the skin will turn red after 300 minutes. The sun protection index SPF is a parameter to measure the defense ability of sunscreen cosmetics against UVB in sunlight. PA (Protection of UVA) is a parameter that reflects the defense ability of sunscreen cosmetics against UVA in sunlight. The defense ability is usually represented by "+". The more "+" signs, the larger the PA value, and the stronger the effect of preventing long-wave ultraviolet rays. Generally, PA values of 2-4 are "+", PA values of 4-8 are "++", and PA values of 8 or more are "+++". The algae component obtained by the preparation method of the present invention can increase the sun protection index SPF of sunscreen cosmetics by about 30-50%.
[0057] Further, in the present invention, fresh desert algae can be collected first, and usually dried by air drying or freeze drying to maintain the stability of the active ingredients. Specifically, the dried desert algae can be frozen and ground to break the cell wall and release the cell contents to obtain the algae sample.
[0058] In the present invention, an algae sample is immersed in a solvent and subjected to ultrasonic extraction to obtain an extraction product. The inventors of the present invention have found that the mycosporin-like amino acids can be effectively dissolved by using a solvent, especially an organic solvent. Ultrasonic extraction can further break the mycosporin-like cell wall and cell membrane of the algae sample, release the mycosporin-like amino acids inside, and thus obtain the algae components.
[0059] In some specific embodiments, the mass ratio of the algae sample to the solvent is 1:1-100, preferably 1:5-15, for example, 1:2, 1:5, 1:8, 1:10, 1:12, 1:15, 1:20, 1:30, 1:40, 1:50, 1:60, 1:70, 1:80, 1:90, etc. When the mass ratio of the algae sample to the solvent is 1:1-100, the algae components can be effectively extracted.
[0060] In some specific embodiments, the frequency of the ultrasonic extraction is 20-40kHz, for example: 22kHz, 25kHz, 28kHz, 30kHz, 32kHz, 35kHz, 38kHz, etc.; the time of the ultrasonic extraction is 30-150 minutes, for example: 35 minutes, 45 minutes, 55 minutes, 65 minutes, 75 minutes, 85 minutes, 95 minutes, 105 minutes, 115 minutes, 125 minutes, 135 minutes, 145 minutes, etc.; the temperature of the ultrasonic extraction is 20-30°C, for example: 21°C, 22°C, 23°C, 24°C, 25°C, 26°C, 27°C, 28°C, 29°C, etc. By setting the temperature of the ultrasonic extraction to 20-30°C, thermal degradation of mycosporin-like amino acids can be avoided, so that the efficacy of the algae components can be effectively exerted.
[0061] Specifically, in the present invention, the solvent includes an organic solvent, such as an alcohol solvent, etc.; preferably, the organic solvent includes one or a combination of two or more of ethanol, acetonitrile, acetone or methanol.
[0062] Further, the cell debris and insoluble impurities in the extract are removed to obtain a purified product. In some specific embodiments, the cell debris and insoluble impurities in the extract are removed by solid-liquid separation; preferably, the solid-liquid separation includes centrifugation and / or filtration separation; more preferably, the centrifugation includes centrifugation at a speed of 5000-15000 rpm for 10-20 minutes.
[0063] Specifically, the present invention can remove cell debris and insoluble impurities by centrifugal separation, and then further filter the supernatant obtained by centrifugal separation using filter paper or microporous filter membrane to further remove residual solid impurities.
[0064] Furthermore, the present invention obtains a concentrated solution of algae components by concentrating the purified product. Specifically, the extracted product can be concentrated using a rotary evaporator to remove more than 80wt% of the solvent. Finally, the concentrated solution of the algae components is separated and identified, and the maximum absorption wavelength of the concentrated solution of the extracted algae components is determined to be 332nm by ultraviolet spectrum scanning. Furthermore, the content of the algae components in the concentrated solution of the algae components is 1-10g / L.
[0065] In some specific embodiments, the concentrated solution of the algae component can be dried to obtain a dried product. Specifically, the present invention does not specifically limit the drying, and it can be freeze-dried. Finally, the dried product is stored in a cool and dry environment to avoid light and moisture.
[0066] <Second Aspect>
[0067] The second aspect of the present invention provides a sunscreen composition, comprising a sunscreen and a sunscreen enhancer, wherein the sunscreen enhancer comprises an algae component prepared according to the preparation method described in the first aspect of the present invention. The present invention can make the sunscreen more effective by adding an algae component to the sunscreen composition.
[0068] The present invention adds a sunscreen synergist to the conventional chemical sunscreen combination, which can not only reduce the use of chemical sunscreens and reduce potential harm to the skin and the environment, but also significantly improve the sunscreen effect and provide more lasting and comprehensive ultraviolet protection.
[0069] Specifically, in the present invention, based on the total mass of the sunscreen composition as 100%, the content of the sunscreen synergist is 0.01-20%, preferably 0.01-10%; the content of the sunscreen agent is 0.01-20%, preferably 0.01-10%.
[0070] In the present invention, if the content of the sunscreen enhancer is too low, the sunscreen effect is insufficient. If the content of the sunscreen enhancer is too low, it may not be able to significantly enhance the effect of the sunscreen, resulting in the sun protection index (SPF) not reaching the expected effect and being unable to effectively resist ultraviolet (UV) damage. In addition, the sunscreen enhancer sometimes also has a stabilizing effect. If the content is insufficient, the sunscreen may be rapidly degraded under sunlight, shortening the duration of the sunscreen effect. In addition, the skin protection effect will also be weakened. The sunscreen enhancer also has antioxidant and anti-inflammatory properties. When the content is insufficient, it may not be able to fully exert its skin protection effect, increasing the risk of ultraviolet damage.
[0071] If the content of sunscreen enhancer is too high, the excessive content of sunscreen enhancer may cause the instability of the formula, and the texture of the sunscreen product may become too sticky and difficult to apply, affecting the user's experience. Excessive content of sunscreen enhancer may cause skin irritation or allergic reaction, especially for users with sensitive skin, increasing the risk of adverse skin reactions. In addition, too much sunscreen enhancer may antagonize with other sunscreen ingredients, reduce the actual protection ability of the sunscreen, and may even cause the sunscreen effect to be less than expected. Therefore, in the present invention, based on the total mass of the sunscreen composition as 100%, the content of the sunscreen enhancer is 0.01-20%, preferably 0.01-10%, for example: 0.1%, 0.3%, 0.5%, 0.8%, 1%, 3%, 5%, 7%, 9%, 11%, 13%, 15%, 17%, 19%, etc.
[0072] In the present invention, generally speaking, if the content of the sunscreen is too low, the sunscreen effect is insufficient; if the content of the sunscreen is too high, the sunscreen effect cannot be improved more effectively and will cause waste. Therefore, based on the total mass of the sunscreen composition as 100%, the content of the sunscreen of the present invention is 0.01-20%, preferably 0.01-10%, for example: 0.1%, 0.3%, 0.5%, 0.8%, 1%, 3%, 5%, 7%, 9%, 11%, 13%, 15%, 17%, 19%, etc.
[0073] In the present invention, the sunscreen agent includes one or a combination of two or more selected from octyl methoxycinnamate, ethylhexyl methoxycinnamate, ethylhexyl salicylate, octyl p-dimethylaminobenzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylaminohydroxybenzoyl hexyl benzoate, ethylhexyl triazone, phenylbenzimidazole sulfonic acid, octocrylene, homosalate, ethylhexyl salicylate, butyl methoxydibenzoylmethane, 4-methoxybenzyl camphor, methyl anthranilate, nano-scale ultrafine titanium dioxide, and zinc oxide.
[0074] Specifically, in the present invention, the sunscreen composition further comprises one or a combination of two or more of an emulsifier, an emollient, a thickener, a humectant, a chelating agent, a skin conditioner, a fragrance, a preservative and a pH adjuster.
[0075] Preferably, based on the total mass of the sunscreen composition as 100%, the content of the emulsifier is 0.01-20%, preferably 0.01-10%; the content of the emollient is 0.01-50%, preferably 0.01-20%; the content of the thickener is 0.01-8%, preferably 0.01-1%; the content of the humectant is 0.01-40%, preferably 0.01-20%; the content of the chelating agent is 0-1%, preferably 0-0.08%; the content of the skin conditioner is 0-50%, preferably 0-20%; the content of the flavoring agent is 0-1%, preferably 0-0.2%; the content of the preservative is 0.01-3%, preferably 0.01-2%; the content of the pH adjuster is 0-3%, preferably 0-2%.
[0076] In the present invention, the emulsifier includes one or more of PEG-100 stearate, polyglyceryl-3 methyl glucose distearate, potassium cetyl phosphate, cetearyl glucoside, cetearyl olive oil ester, cetearyl glucoside / cetearyl alcohol, hydrogenated lecithin, sorbitan olive oil ester and polyglyceryl-3 distearate; preferably, the emulsifier is selected from one or a combination of two or more of cetearyl glucoside, cetearyl glucoside / cetearyl alcohol, potassium cetyl phosphate and hydrogenated lecithin.
[0077] The emollient includes one or a combination of two or more of tri(ethylhexanoin)glyceryl, caprylic / capric triglyceride, pentaerythritol tetra(ethylhexanoin), butyloctanol salicylate, diethoxyethyl succinate, isododecane, rice germ oil, hydrogenated palm kernel oil, cocoa seed butter cetyl ethylhexanoate, isopropyl myristate, isopropyl palmitate, diisopropyl sebacate, polydimethylsiloxane, cetearyl alcohol, dibutyl adipate, C12-15 alcohol benzoate, dicaprylyl carbonate, coconut oil alcohol-caprylate / caprate, polydimethylsiloxane, caprylyl polymethylsiloxane, cyclopentasiloxane and phenyl trimethylsiloxane.
[0078] The thickener comprises one or a combination of two or more of xanthan gum, acrylic acid (ester) / C 1 0-30 alkyl acrylate cross-linked polymer, carbomer, ammonium acryloyldimethyltaurate / VP copolymer and sodium acrylate / sodium acryloyldimethyltaurate copolymer.
[0079] The preservative includes one or a combination of two or more of phenoxyethanol, ethylhexylglycerin, hexylene glycol and pentylene glycol.
[0080] The pH regulator includes one or a combination of two or more of arginine, sodium hydroxide, potassium hydroxide, triethanolamine and aminomethyl propanol.
[0081] The moisturizing agent includes one or a combination of two or more of ethanol, glycerol, propylene glycol, dipropylene glycol, 1,3-butylene glycol, trehalose, xylitol, glycerol polyether-26, β-glucan, methyl gluceth-20, methyl gluceth-10, erythrulose, biosaccharide gum-1, rhamnose, oat β-glucan, acetyl chitosan, polyethylene glycols, water-soluble oils, water-soluble silicone oil and sodium hyaluronate.
[0082] The chelating agent includes one or a combination of two or more of disodium EDTA, tetrasodium EDTA and sodium phytate.
[0083] The skin conditioning agent includes one or a combination of two or more of ceramide, collagen, plant extract, glucan, panthenol, asiatica glycoside, etc.
[0084] The flavoring agent includes essence, essential oil, or a combination of two or more thereof.
[0085] Furthermore, the present invention also provides a method for preparing the sunscreen composition according to the present invention, which comprises the steps of mixing the components of the sunscreen composition;
[0086] Preferably, the preparation method comprises the following steps:
[0087] Mix the moisturizer, thickener and solvent and heat to 80-90° C. to obtain phase A;
[0088] Mix the emollient, sunscreen, and emulsifier and heat to 80-90°C to obtain phase B;
[0089] After mixing the phase A and the phase B, homogenize at a rotation speed of 2500-3000 rpm for 5-8 minutes to obtain a mixed product;
[0090] Add a preservative and a sunscreen synergist to the mixed product, and homogenize at a rotation speed of 2500-3000 rpm for 1-3 minutes to obtain a sunscreen composition.
[0091] In addition, the present invention also provides a use of the sunscreen composition according to the present invention for preparing cosmetics; preferably, the cosmetics include sunscreen milk, sunscreen lotion, sunscreen cream, sunscreen liquid, sunscreen spray, sunscreen gel, isolation cream, isolation milk, isolation lotion or BB cream.
[0092] Example
[0093] The embodiments of the present invention will be described in detail below in conjunction with the examples, but those skilled in the art will appreciate that the following examples are only used to illustrate the present invention and should not be considered to limit the scope of the present invention. If no specific conditions are specified in the examples, they are carried out according to normal conditions or the conditions recommended by the manufacturer. If the manufacturer is not specified for the reagents or instruments used, they are all conventional products that can be obtained commercially.
[0094] Example
[0095] The algae component is used as a desert algae skin care raw material and a sunscreen enhancer. Various experiments have been conducted on the desert algae skin care raw material, and the experiments have proved that the desert algae skin care raw material in the present application has a sunscreen enhancer effect.
[0096] The specific preparation method of the algae component used in the application examples is:
[0097] 1. Preparation of Chlorella
[0098] Cultivation: Select a suitable Chlorella species and cultivate it in appropriate culture medium and environmental conditions until sufficient biomass is reached.
[0099] 2. Cell disruption
[0100] Freeze-grinding: The harvested dried Chlorella is frozen and ground to break the cell walls and release the cell contents to obtain the Chlorella sample.
[0101] 3. Extraction
[0102] Ultrasonic treatment: The Chlorella sample was mixed with ethanol at a mass ratio of 1:10, and the cells were ultrasonically treated using an ultrasonic crusher to further destroy the cell wall and improve the extraction efficiency. The frequency of ultrasonic extraction was 25 kHz, the time of ultrasonic extraction was 40 minutes, and the temperature of ultrasonic extraction was 30°C. Steps 2 and 3 were repeated for secondary extraction to obtain an extraction product.
[0103] 4. Separation
[0104] Centrifugal separation: The extract was separated by centrifugation at 5000 rpm for 30 minutes to remove cell debris and obtain the supernatant containing the target compound. The supernatant was filtered using a 0.22 μm filter membrane.
[0105] 5. Concentration
[0106] Evaporation and concentration: A rotary evaporator is used to remove part of the solvent in the extraction product, and the removal mass of the solvent is about 90%, thereby obtaining a concentrated solution of the algae component.
[0107] 6. Analysis and Purity Determination
[0108] The analysis was performed using a UV-Vis spectrophotometer. Specifically, the scanning range of the UV-Vis spectrophotometer was set to a scanning wavelength range from 200 nm to 400 nm, and the wavelength with the highest absorbance was observed by scanning the spectrum. The maximum absorption wavelength of the algae component was 332 nm.
[0109] 7. Sample Purity Determination
[0110] Accurately measure 2 ml of the concentrated solution of algae components to prepare the sample measurement solution, and then analyze and measure it at a wavelength of 332 nm. Quantify it using the standard curve method and calculate the content of the algae components. The concentration of the algae components in the concentrated solution of the algae components is determined to be 5.12 g / L.
[0111] 8. Drying
[0112] 100 ml of the algae component concentrate was freeze-dried using a freeze dryer to obtain an algae component.
[0113] 9. Storage
[0114] Store algae ingredients in a cool, dry environment away from light and moisture.
[0115] Application Examples
[0116] The preparation was carried out according to the formula in Table 1 and Table 2 below. The preparation process of the specific application example is as follows:
[0117] 1. Heat phase A and phase B in application example 1-13 to 90°C respectively and stir evenly at 30 rpm.
[0118] 2. Mix phase A and phase B and homogenize at 3000 rpm for 8 minutes.
[0119] 3. Cool down to below 45°C, add phase C, stir evenly, and homogenize at 3000rpm for 3 minutes.
[0120] 4. Material discharging inspection.
[0121] Table 1
[0122]
[0123] Table 2
[0124]
[0125] Application comparison
[0126] The preparation was carried out according to the formula in Table 3 below, and with reference to the preparation process of Application Examples 1-12, wherein the calendula extract and tea extract were purchased from Guizhou Keyichuang Biotechnology Co., Ltd.
[0127] Table 3
[0128]
[0129] Performance Testing
[0130] 1. Sunscreen test method
[0131] 1.1 Experimental instruments and subjects selection
[0132] Light source: Xenon arc lamp with sunlight simulator as light source
[0133] 1. It can continuously generate ultraviolet light with a wavelength of 290nm to 400nm;
[0134] 2. After the light source output is filtered by the filter, the ultraviolet light with a wavelength less than 290nm should be less than 1%;
[0135] 3. After the light source output is filtered by the filter, the ultraviolet rays with a wavelength greater than 400nm should be less than 5%;
[0136] 4. The light source should have stable output and uniform light, and the fluctuation range on the radiated plane should be less than 10%.
[0137] 1.2 Selection of subjects:
[0138] 1. Select healthy volunteers aged 18 to 60 years old, both male and female.
[0139] 2. No history of photosensitivity disease and no recent use of drugs that affect photosensitivity;
[0140] 3. The subjects' skin types are I, II, or III, that is, they are sensitive to sunlight or ultraviolet rays, and are prone to sunburn but not pigmentation after exposure;
[0141] 4. The skin of the test area should be free of pigmentation, inflammation, scars, pigmented nevi, excessive hair growth, etc.;
[0142] 5. Those who are pregnant, breastfeeding, taking oral or topical corticosteroids or other anti-inflammatory drugs, or have received similar tests within the past month should be excluded from the subjects;
[0143] 6. According to this method, 5 people are tested for each type of sunscreen cosmetic.
[0144] 2. SPF value test
[0145] The samples of application examples 1-12 and application comparative examples 1-8 prepared above were subjected to MED tests respectively, and the results are shown in Table 4 below.
[0146] 2.1 Test Method
[0147] 1. Subject position: For irradiation of the back, the subject can be in a forward leaning or prone position.
[0148] 2. The sample coating area is not less than 30cm 2 .
[0149] 3. Sample dosage and coating method: 2 mg sample / cm 2 Weigh the sample in the required amount, apply it evenly to the test area using a latex finger cot, and wait for 15 minutes.
[0150] 4. Predict the MED of the subject: This should be completed 24 hours before testing the product. Select an irradiation area on the back of the subject and irradiate 5 points with different doses of ultraviolet rays. The SPF value range designed for sunscreen product formulas can be referred to: for products with SPF values ≤ 25, the dose increment of the five irradiation points is 25%; for products with SPF values > 25, the dose increment of the five irradiation points does not exceed 12%. Observe the results after 24 hours, and the lowest irradiation dose or shortest irradiation time at which erythema appears on the skin is the MED of the subject's normal skin.
[0151] 5. Determine the SPF value of the test sample: On the day of the test, the MED value under the following three conditions must be determined simultaneously.
[0152] 6. Determine the MED of the subject: adjust the ultraviolet radiation dose according to the predicted MED value above, and measure the MED of the subject's unprotected skin again on the day of the test. Apply the test product to the subject's skin, and then measure the MED of the skin under product protection according to the above method. When selecting the irradiation dose increase of the 5-point test site, refer to the SPF value range designed for the sunscreen product formula: for products with SPF values <15, the dose increase of the five irradiation points is 25%; for products with SPF values >15, the dose increase of the five irradiation points is 15%.
[0153] 7. Apply the SPF standard sample to the test area and measure the MED of the skin under the protection of the standard sample.
[0154] Exclusion criteria: When performing the above measurement, if no erythema appears at any of the five test points, or erythema appears at all five test points, or erythema appears at a test point and then disappears with the increase of ultraviolet radiation dose, the result should be considered invalid and the instrument should be calibrated and re-measured.
[0155] 2.2 SPF value calculation method
[0156] Individual SPF = MED of protected skin / MED of unprotected skin
[0157] Note: Individual SPF values are required to be accurate to one decimal place. Calculate the arithmetic mean of the SPF values of all subjects protected by the sample, and take the integer part as the SPF value of the measured sample. The standard error of the group of data can be calculated by estimating the sampling error of the mean. The 95% confidence interval (95% CI) of the mean is required to be no more than 17% of the mean (e.g., if the mean is 10, the 95% CI should be between 8.03-11.7). Otherwise, the number of subjects should be increased (no more than 25) until the above requirements are met.
[0158] Table 4 SPF values
[0159] Serial number Experimental Group Measured SPF value 1 Application Example 1 21.05 2 Application Example 2 22.26 3 Application Example 3 23.20 4 Application Example 4 23.87 5 Application Example 5 25.45 6 Application Example 6 28.78 7 Application Example 8 1.12 8 Application Example 9 1.34 9 Application Example 10 2.14 10 Application Example 11 2.86 11 Application Example 12 4.32 12 Application Example 13 7.82 13 Application Comparative Example 1 19.8 14 Application Comparative Example 2 18.90 15 Application Comparative Example 3 19.50 16 Application Comparative Example 4 20.05 17 Application Comparative Example 5 19.95 18 Application Comparative Example 6 19.52 19 Application Comparative Example 7 18.54 20 Application Comparative Example 8 0.35
[0160] As can be seen from Table 4, from Application Examples 1-6, as the content of mycosporin-like amino acids increases, the sunscreen synergistic effect of the sunscreen agent is significantly improved. When the content reaches 5%, the sunscreen synergistic effect tends to be flat. Considering the cost of sunscreen products, the optimal addition range of mycosporin-like amino acids is 0.01-3%.
[0161] It can be seen from Application Examples 7-12 that when no sunscreen is used, the mycosporin-like amino acids contribute a certain sunscreen SPF value, proving that the mycosporin-like amino acids have relatively good ultraviolet absorption.
[0162] From the comparative examples 1-8, it can be seen that the sunscreen synergistic effect of marigold extract and tea extract is weak, and even has a certain negative impact on the sunscreen effect of the sunscreen. This shows that marigold extract and tea extract have no sunscreen synergistic effect on the sunscreen. In addition, when the sunscreen and algae components are not used, there is almost no sunscreen effect.
[0163] 2. Human skin patch test
[0164] According to the above experimental conclusions, taking Application Example 3, Application Example 9 and Application Comparative Example 1 as examples, the skin patch safety of the test samples can reflect the skin patch test results of all the application examples and application comparative examples of the present invention.
[0165] 2.1 Purpose of the experiment
[0166] Test samples for the potential to cause adverse skin reactions.
[0167] 2.2 Experimental materials and methods
[0168] 1) Test substance: the original cosmetic final product.
[0169] 2) Negative control: blank control.
[0170] 3) Subjects: A total of 30 subjects, including 1 male and 29 females, aged 20 to 59 years old, with an average age of 38.9±13.0 years old.
[0171] Meet the volunteer inclusion criteria.
[0172] 4) Patch test method: Select qualified patch test equipment and use the closed patch test method. Place about 0.020g~0.025g of the test substance (white to light yellow emulsion) in the patch tester and apply it to the back of the subject with low-allergenic tape. Remove the test substance after 24 hours and observe the skin reaction 0.5, 24, and 48 hours after removal. Record the results according to the skin reaction grading standards in the "Technical Specifications for Safety of Cosmetics" (2015 edition).
[0173] 2.3 Test results
[0174] The results of human skin patch test are shown in Table 5-7:
[0175] Table 5 Human skin patch test results of application example 3
[0176]
[0177] Table 6 Human skin patch test results of application example 9
[0178]
[0179] Table 7 Human skin patch test results of comparative example 1
[0180]
[0181] As can be seen from Table 5 and Table 6, the patch test results of Application Example 3 and Application Example 9 show that no adverse skin reaction occurred in 30 people, indicating that the sunscreen composition can not only improve the SPF value of the sample, but also help to improve the mildness of the product.
[0182] As can be seen from Table 7, the results of applying the patch of Comparative Example 1 showed that 2 cases of grade 1 adverse skin reactions occurred among 30 people, indicating that the sunscreen has a certain degree of allergenicity to the skin.
[0183] It should be noted that, although the technical solution of the present invention is introduced with specific examples, those skilled in the art will appreciate that the present invention should not be limited thereto.
[0184] The embodiments of the present invention have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles of the embodiments, practical applications, or technical improvements in the market, or to enable other persons of ordinary skill in the art to understand the embodiments disclosed herein.
Claims
1. A method for preparing an algae component having ultraviolet absorption, characterized in that: The following steps are involved: The algae sample is immersed in a solvent and subjected to ultrasonic extraction to obtain an extraction product; removing cell debris and insoluble impurities from the extraction product to obtain a purified product; The purified product is concentrated to obtain a concentrated solution of algae components.
2. The preparation method according to claim 1, characterized in that: The algae sample is derived from desert algae, preferably including one or a combination of two or more of Chlorella vulgaris, Microcoleus scaly, and Hasa algae; Preferably, the desert algae is frozen and ground to break cell walls and release cell contents to obtain the algae sample.
3. The preparation method according to claim 1 or 2, characterized in that: The mass ratio of the algae sample to the solvent is 1:1 to 100; and / or, The frequency of the ultrasonic extraction is 20-40 kHz, the time of the ultrasonic extraction is 30-150 minutes, and the temperature of the ultrasonic extraction is 20-30°C.
4. The preparation method according to any one of claims 1 to 3, characterized in that The solvent includes an organic solvent; preferably, the organic solvent includes one or a combination of two or more of acetonitrile, acetone, ethanol and methanol.
5. The preparation method according to any one of claims 1 to 4, characterized in that: Removing cell debris and insoluble impurities from the extraction product by solid-liquid separation; Preferably, the solid-liquid separation comprises centrifugal separation and / or filtration separation; More preferably, the centrifugal separation comprises centrifuging at a speed of 5000-15000 rpm for 10-20 minutes; The filtration separation includes filtration treatment using filter paper or microporous filter membrane.
6. The preparation method according to any one of claims 1 to 5, characterized in that: The purified product is concentrated by a rotary evaporator to remove more than 80 wt % of the solvent; and / or, Drying the concentrated liquid of the algae component to obtain the algae component; Preferably, the content of algae components in the concentrated solution of algae components is 1-10 g / L.
7. A sunscreen composition, characterized in that: It comprises a sunscreen and a sunscreen enhancer, wherein the sunscreen enhancer comprises an algae component prepared by the preparation method according to any one of claims 1 to 6; preferably, based on the total mass of the sunscreen composition as 100%, the content of the sunscreen enhancer is 0.01-20%, preferably 0.01-10%; the content of the sunscreen is 0.01-20%, preferably 0.01-10%.
8. The sunscreen composition according to claim 7, characterized in that The sunscreen composition further comprises one or a combination of two or more of an emulsifier, an emollient, a thickener, a moisturizer, a chelating agent, a skin conditioner, a fragrance, a preservative, and a pH adjuster; Preferably, based on the total mass of the sunscreen composition as 100%, the content of the emulsifier is 0.01-20%, preferably 0.01-10%; the content of the emollient is 0.01-50%, preferably 0.01-20%; the content of the thickener is 0.01-8%, preferably 0.01-1%; the content of the humectant is 0.01-40%, preferably 0.01-20%; the content of the chelating agent is 0-1%, preferably 0-0.08%; the content of the skin conditioner is 0-50%, preferably 0-20%; the content of the flavoring agent is 0-1%, preferably 0-0.2%; the content of the preservative is 0.01-3%, preferably 0.01-2%; the content of the pH adjuster is 0-3%, preferably 0-2%.
9. A method for preparing the sunscreen composition according to claim 7 or 8, characterized in that: The method comprises the steps of mixing the components of the sunscreen composition; Preferably, the preparation method comprises the following steps: Mix the moisturizer, thickener and solvent and heat to 80-90° C. to obtain phase A; Mix the emollient, sunscreen, and emulsifier and heat to 80-90°C to obtain phase B; After mixing the phase A and the phase B, homogenize at a rotation speed of 2500-3000 rpm for 5-8 minutes to obtain a mixed product; Add a preservative and a sunscreen synergist to the mixed product, and homogenize at a rotation speed of 2500-3000 rpm for 1-3 minutes to obtain a sunscreen composition.
10. Use of the sunscreen composition according to claim 7 or 8 for preparing cosmetics; preferably, the cosmetics include sunscreen milk, sunscreen lotion, sunscreen cream, sunscreen liquid, sunscreen spray, sunscreen gel, isolation cream, isolation milk, isolation lotion or BB cream.