KR20230065093A - Composition for sunscreen comprising wakame extract - Google Patents

Abstract

The present invention relates to a sunscreen composition comprising seaweed extract and an inorganic sunscreen agent and a method for preparing the same. More specifically, in the case of using the sunscreen composition of the present invention, seaweed extract is used instead of a chemical substance as a dispersant for inorganic sunscreen, so it is harmless to the human body, environmentally friendly, and exhibits high sunscreen performance, and at the same time, no cloudiness occurs. Since it has excellent spreadability, it can be usefully used in a cosmetic composition with a sunscreen function.

Description

Composition for sunscreen comprising wakame extract}

The present invention relates to a sunscreen composition comprising seaweed extract as a dispersing agent.

Exposure to ultraviolet rays has adverse effects on the skin, such as pigment degeneration of the skin, sunburn, collagen damage, DNA damage in skin tissue, premature skin aging, and skin cancer. As these risks of UV exposure become known, the use of sunscreens is gradually increasing.

Sunscreens include chemical sunscreens and physical sunscreens. Chemical sunscreens include organic UV filters such as oxybenzone, octinoxate, homosalate, and octocrylene, which absorb high-energy ultraviolet rays. It is excited to a high-energy state and returns to the ground state, converting the absorbed energy into low-energy heat to disperse ultraviolet rays, and after 20 minutes of application to the skin, the UV blocking effect is exhibited. Organic sunscreens are known to be toxic chemicals and are harmful to the human body. Organic sunscreens are absorbed into the skin and bloodstream, causing dermatitis and allergies, which adversely affect health. In addition, it causes environmental problems such as destroying coral reefs when discharged into the sea through sea bathing and domestic sewage.

Physical sunscreens that are relatively safer than chemical sunscreens include inorganic sunscreens such as mineral zinc oxide and titanium dioxide, which block ultraviolet rays by reflecting or refracting them from the skin. do. When applied in a thin layer, the inorganic sunscreen provides an immediate sunscreen effect. Inorganic sunscreens, which are minerals, are safe because they are not absorbed by the human body, so they do not cause skin inflammation and do not cause environmental problems such as coral reef destruction.

However, inorganic sunscreens have disadvantages in that they do not apply smoothly when applied to the skin, resulting in poor usability and applicability and whitening of the skin. This is a phenomenon caused by the high refractive indices of zinc oxide and titanium dioxide, 2.2 and 2.7, respectively. When the content of zinc oxide and / or titanium dioxide is increased to increase the sunscreen effect, the application property is deteriorated and the white cast phenomenon is increased, resulting in unnatural skin expression, adversely affecting natural skin makeup.

In order to suppress the whitening phenomenon of the inorganic sunscreen, there is a method of nanoparticles of the inorganic sunscreen and preventing aggregation of the nanoparticles. In order to prevent aggregation, a dispersant is required, and stearic acid, a chemical substance, is mainly used as the dispersant. According to the Material Safety Data Sheet (MSDS), stearic acid is harmful to humans by causing skin irritation and eye irritation, and is particularly toxic to aquatic life, causing environmental problems.

Therefore, it is necessary to develop a functional sunscreen that has high UV blocking performance, is harmless to the human body, is environmentally friendly, and does not have a white cast phenomenon.

KR 10-2249023 B

The present inventors have intensively researched to develop a functional sunscreen that has high sunscreen performance, is harmless to the human body, is environmentally friendly, and does not cause cloudiness. As a result, when seaweed extract is used as a dispersant for inorganic sunscreen, it shows a high sunscreen index, is harmless to the human body and is environmentally friendly, and the nanoparticles of the inorganic sunscreen are well dispersed without aggregation, resulting in cloudiness when applied to the skin. The present invention was completed by clarifying this inhibiting effect.

Accordingly, an object of the present invention is to provide a sunscreen composition comprising seaweed extract and an inorganic sunscreen agent.

Another object of the present invention is to provide a method for preparing the above-described sunscreen composition.

According to one aspect of the present invention, the present invention provides a sunscreen composition comprising a wakame extract and an inorganic sunscreen agent.

The present inventors have intensively researched to develop a functional sunscreen that has high sunscreen performance, is harmless to the human body, is environmentally friendly, and does not cause cloudiness. As a result, when seaweed extract is used as a dispersant for inorganic sunscreen, it shows a high sunscreen index, is harmless to the human body and is environmentally friendly, and the nanoparticles of the inorganic sunscreen are well dispersed without aggregation, resulting in cloudiness when applied to the skin. This inhibitory effect was investigated.

As used herein, the term 'ultraviolet ray (UV)' refers to electromagnetic waves having a wavelength of 10 nm to 400 nm. The ultraviolet rays of the present specification include ultraviolet rays A, ultraviolet B, ultraviolet C, near ultraviolet rays, intermediate ultraviolet rays, deep ultraviolet rays, vacuum ultraviolet rays, and extreme ultraviolet rays.

The term 'ultraviolet ray C' used herein is also referred to as UVC and refers to electromagnetic waves having a wavelength of 200 nm to 290 nm. As used herein, the term 'ultraviolet ray B' is also called UVB and refers to electromagnetic waves having a wavelength of 290 nm to 320 nm. The term 'ultraviolet A' used herein is also referred to as UVA and refers to electromagnetic waves having a wavelength of 320 nm to 400 nm.

As used herein, the term 'sunscreen composition' refers to a functional composition that is effective in protecting the skin from ultraviolet rays. The sunscreen composition of the present invention may be used as a cosmetic composition or included in a cosmetic composition. As used herein, the term 'cosmetic composition' refers to a composition used to clean, beautify, maintain health, or promote health of the skin.

As used herein, the term 'wakame (seaweed)' refers to algae belonging to the seaweed family ( Laminariales ) and seaweed ( Alariaceae ). The seaweed of the present invention includes seaweed from the kelp tree and brown algae belonging to the genus Undaria . It will be apparent to those skilled in the art that seaweed that can be used in the present invention can be used without limitation as long as it is an alga belonging to the seaweed family.

The seaweed includes at least one selected from the group consisting of Undaria pinnatifida , Undaria peterseniana , Undaria crenata , Undaria undarioides , and variants thereof, It is not necessarily limited thereto. The brown seaweed may be a southern type of brown seaweed ( U. pinnatifida f. typica ), a northern type of brown seaweed ( U. pinnatifida f. distans ) or a cultivated strain thereof.

For example, the seaweed of the present invention may be seaweed that mainly inhabits the waters of Ulleung-gun, Gyeongsangbuk-do, Korea. For another example, the seaweed of the present invention may be so-called 'seaweed seaweed' cultivated in the Songjeong area, which is the intersection of the East Sea and the West Sea of Korea.

In one embodiment of the present invention, the seaweed extract is obtained from brown algae.

In one embodiment of the present invention, the inorganic sunscreen agent is dispersed by the seaweed extract.

In the present invention, seaweed extract was added as a dispersing agent so that the inorganic sunscreen agent existed in a nanometer size without aggregation. Specifically, the inorganic sunscreen agent of the present invention is dispersed in nanoparticle size by seaweed extract in purified water or distilled water.

As used herein, the term 'dried seaweed powder' refers to a powder obtained by drying and grinding seaweed.

As used herein, the term 'seaweed extract powder' means a solid component obtained by precipitating a seaweed water extract, and more specifically means a solid component precipitated by adding alcohol to the seaweed water extract. More specifically, 'seaweed water extract' in the present specification refers to an extract obtained by mixing seaweed with water as an extraction solvent and then sonication. In the step of precipitating solid components by adding alcohol from the seaweed water extract, the alcohol used may be more specifically, for example, methanol or ethanol, and more preferably, ethanol may be used for extraction. . As the ethanol described above, 50% to 99% ethanol may be used, but is not particularly limited.

As used herein, the term 'wakame extract (seaweed extract)' refers to a solution extracted by adding an extraction solvent to seaweed. For example, the seaweed extract of the present invention may be a solvent extract prepared by extracting the seaweed using water as an extraction solvent, a solvent fraction thereof, a purified product or a dried product of the solvent extract or solvent fraction. For another example, the seaweed extract of the present invention may be a solution extracted by adding a solvent to the dried seaweed powder. As another example, the seaweed extract of the present invention may be a re-dissolved seaweed extract powder obtained by mixing purified water with the seaweed extract powder.

As used herein, the term 'reconstituted solution (redissolved solution)' refers to a solution obtained by dissolving a dried and stored powdered material in a solvent, solution, or diluent and restoring it to a liquid state.

The seaweed extract may be obtained from all or part of the seaweed. The seaweed extract of the present invention is a leaf, sporophyll, thallus, lamina, sorus, bladder, stem (petiole), holdfast of seaweed and/or from haptera (root). For example, the seaweed extract of the present invention can be extracted from Underia pinnatifida sporophyll. Seaweed is a spore leaf of seaweed.

The extraction solvent includes purified water, distilled water, deionized water, alcohol or a mixture thereof, but is not necessarily limited thereto. The extraction solvent may be reverse osmosis water. The distilled water may be first, double or triple distilled water. The alcohol may be a primary alcohol. The primary alcohol may be metalol or ethanol.

As used herein, the term 'dispersion' refers to a state in which a composition composed of at least two materials includes at least two different phases. For example, the two phases can be completely different, one can be a continuous phase and the other can be a dispersed phase, usually present at the nanoscale of 10 nm to 100 nm. .

The dispersion of nanoparticles in an aqueous medium is well described in the theory of DLVO (Deryagin, Landau, Verwey and Overbeek), which is well known in the art (Derjaguin B.V., Churaev N.V., Muller V.M. (1987) The Derjaguin—Landau—Verwey— See Overbeek (DLVO) Theory of Stability of Lyophobic Colloids. In: Surface Forces. Springer, Boston, MA.).

Inorganic sunscreens such as titanium dioxide nanoparticles or zinc oxide nanoparticles are not well dispersed in an aqueous solution and are aggregated, resulting in a particle size of at least 1 micrometer. In order for the inorganic sunscreen to exist in the nano size without aggregation, a dispersant is required.

The aggregation of the inorganic sunscreen is a major cause of degrading the ultraviolet ray absorption performance and causing reduced transparency when applied to the skin, that is, a whitish phenomenon. In addition, when the particle size of the sunscreen particles is about half of the wavelength to be scattered, that is, the 320 nm to 400 nm wavelength of UVA and/or the 290 nm to 320 nm wavelength of UVB, the wavelength is optimally scattered. become (blocked).

Therefore, when the inorganic sunscreen agent is stably dispersed in the composition without forming agglomerates and at the same time exists as nanoparticles having a size of tens to hundreds of nanometers, it is difficult to achieve the same sunscreen factor (SPF) compared to the sunscreen agent in which large agglomerates are formed. The concentration of the required sunscreen is significantly lower, which is not only effective but also minimizes the impact on the environment (Labille J et al., (2020) Assessing Sunscreen Lifecycle to Minimize Environmental Risk Posed by Nanoparticulate UV-Filters - A Review for Safer- by-Design Products. Front. Environ. Sci. 8:101).

The dispersant imparts hydrophilic, amphiphilic, or lipophilic characteristics to the nanoparticles of the inorganic sunscreen so that they can be easily dispersed in the water phase or oil phase of the emulsion. For example, a silane-type polymer such as polydimethylsiloxane (PDMS) or stearic acid is mainly used as a dispersing agent, and such a dispersing agent coats the surface of nanoparticles of an inorganic sunscreen to impart lipophilic characteristics to the nanoparticles. For another example, the amphiphilic properties allow nanoparticles to be dispersed in oil and aqueous phases via simethicone coating (Labille J et al., (2020) Front. Environ. Sci. 8:101. See above. ).

As used herein, the term 'dispersant (dispersant, dipersing agent)' refers to a substance used to prepare a suspension of solid or liquid particles in a liquid such as a colloid or emulsion, and by pulverizing large particles and agglomerated particles into small Formed into particles and colloidal particles, it has a meaning encompassing substances added to prevent aggregation of the formed small particles and colloidal particles.

There are three compositions of conventional sunscreen formulations mainly used for sun protection: i) titanium dioxide (TiO ₂ ), aluminum oxide (Al ₂ O ₃ ) and stearic acid; ii) titanium dioxide, aluminum hydroxide (Al(OH) ₃ ) and polydimethylsiloxane (PDMS); and iii) titanium dioxide and silicon dioxide (SiO ₂ ). The above-described conventional sunscreen formulation composition needs improvement in cloudiness, feeling of use, and application, and needs to be replaced with environmentally friendly components.

Specifically, stearic acid used as a dispersant of composition i) is known to be harmful to the human body and very toxic to aquatic organisms by causing skin rashes and eye irritation, as described above. In addition, aluminum oxide of composition i) and silicon dioxide of composition iii) are used to cover the surface of titanium dioxide in order to prevent component denaturation and pigment deposition that may be caused by the high photocatalytic power of titanium dioxide. When the surface of titanium dioxide nanoparticles is covered with aluminum oxide and silicon dioxide, there is a disadvantage in that application properties are not good.

Instead of using stearic acid as a dispersing agent or using aluminum oxide or silicon dioxide to cover the surface of titanium dioxide, the present inventors used seaweed extract as a dispersing agent, thereby significantly suppressing the cloudiness phenomenon that looks white when applied to the skin, and feeling of use And a composition for sunscreen that is harmless to the human body and friendly to the environment, which also has excellent application properties, was completed.

In one embodiment of the present invention, the seaweed extract is characterized in that a layer is formed by coating the inorganic sunscreen nanoparticles.

In one specific embodiment of the present invention, the wakame extract is characterized by forming a layer by coating the inorganic sunscreen nanoparticles through electrostatic adsorption.

Specifically, a repulsion force acts between the inorganic sunscreens coated with the wakame extract to be dispersed in the size of nanoparticles (NP).

More specifically, a repulsive force acts between the titanium dioxide coated with the seaweed extract to be dispersed in nanoparticle size (see FIG. 4).

More specifically, a repulsive force acts between the zinc oxide coated with the seaweed extract to be dispersed in nanoparticle size.

In an additional embodiment of the present invention, the inorganic sunscreen has a positive surface charge, and the seaweed extract has a negative charge.

In another further embodiment of the present invention, the seaweed extract having a negative charge is coated with the inorganic sunscreen having a positive surface charge through electrostatic adsorption to form a layer, and the repulsive force acts to disperse it in nanoparticle size. do.

As used herein, the term 'electrostatic adsorption' refers to adsorption of ions through Coulombic force. The Coulomb force is a force acting between two point charges, and means F=q1q2/4Πεr ² , which is a force acting between two point charges q1 and q2 separated by a distance r, and ε means permittivity. If the two charges are of the same sign, the force of attraction acts if they are of different signs.

Since the wakame extract of the present invention is negatively charged and the inorganic sunscreen is positively charged, the two substances are adsorbed through the Coulomb force acting as an attraction between the positively charged inorganic sunscreen by the negatively charged seaweed extract, The inorganic sunscreens coated with the extract are dispersed in nanoparticle size through the Coulombic force acting as a repulsive force between the negatively charged seaweed extracts.

As used herein, the term 'adsoprtion' refers to a phenomenon in which a specific material is accumulated at an interface.

It is known that polysaccharides contained in seaweed are usually negatively charged. Polysaccharides contained in wakame mainly include carrageenan, agar, and alginic acid. Carrageenan and agar are composed of galactan, a polymer form of galactose, and alginic acid is composed of mannuronic acid and guluronic acid residues. Galactan, manuronic acid, and guluronic acid, which are the backbones of polysaccharides, have various functional groups such as sulfate or methoxy, all of which are known to be negatively charged (Katerina Alba, Vassilis Kontogiorgos, Seaweed Polysaccharides (Agar, Alginate Carrageenan) , Editor(s): Laurence Melton, Fereidoon Shahidi, Peter Varelis, Encyclopedia of Food Chemistry, Academic Press, 2019 , Pages 240-250, see).

It is known that the surface of titanium dioxide nanoparticles in ultrapure water has a strong positive charge of +31 ± 0.5 mV at pH 3.0, and the pH at which the sorbent surface charge takes a zero value , the point of zero charge, pH _pzc ) has been known as pH _pzc = 5.8 ± 0.1 or pH _pzc = 6.2 (Ramirez, L.; Ramseier Gentile, S.; Zimmermann, S.; Stoll, S. Behavior of TiO2 and CeO2 Nanoparticles and Polystyrene Nanoplastics in Bottled Mineral, Drinking and Lake Geneva Waters. Impact of Water Hardness and Natural Organic Matter on Nanoparticle Surface Properties and Aggregation. Water 2019 , 11 , 721.).

In addition, it is generally known that wurtzite-type zinc oxide (ZnO) nanoparticles have a positive surface charge. However, it is known that when zinc oxide nanoparticles are coated with citrate at pH 7.0, they have a negative surface charge, whereas when coated with L-serine at pH 6.0, they have a positive surface charge (Kim, KM , Choi, MH, Lee, JK, Jeong, J., Kim, YR, Kim, MK, Paek, SM, & Oh, JM (2014) Physicochemical properties of surface charge-modified ZnO nanoparticles with different particle sizes.International see journal of nanomedicine , 9 Suppl 2 (Suppl 2), 41-56.).

Therefore, the positively charged inorganic sunscreen coated through electrostatic adsorption by the negatively charged wakame extract of the present invention is dispersed in nanoparticle size due to the repulsive force between the particles as shown in the schematic diagram shown in FIG. Specifically, inorganic sunscreen nanoparticles with a positive surface charge form a layer through electrostatic adsorption by a seaweed extract with a negative charge, and are dispersed in the size of nanoparticles due to the repulsive force between the particles (see FIG. 4) .

For example, the sunscreen composition of the present invention contains titanium dioxide nanoparticles dispersed by seaweed extract as an active ingredient.

For example, the sunscreen composition of the present invention contains zinc oxide nanoparticles dispersed by seaweed extract as an active ingredient.

Therefore, the sunscreen composition of the present invention contains inorganic sunscreen nanoparticles dispersed by seaweed extract at pH 5.0 to pH 6.0 as an active ingredient.

Specifically, the sunscreen composition of the present invention includes inorganic sunscreen nanoparticles dispersed by seaweed extract through electrostatic adsorption at pH 5.0 to pH 6.0.

More specifically, when the oxidation degree of the sunscreen composition of the present invention is pH 5.5, the surface charge of the inorganic sunscreen nanoparticles is positively charged, and the wakame extract is negatively charged, so that a layer is formed through electrostatic adsorption, The seaweed extract allows the inorganic sunscreen nanoparticles to be well dispersed without aggregation.

The particle size (particle size) of the inorganic sunscreen of the present invention is measured using a method known in the art, for example, a particle size analysis method by laser diffraction using a particle size analyzer (PSA). and/or calculated. In addition, the particle diameter may be analyzed according to the instructions of the manufacturer of the particle size analyzer equipment, for example Malvern Panalytical.

The particle diameter of inorganic sunscreen is in inverse proportion to the sunscreen index. Therefore, as described above, it is well known in the art that the sunscreen index increases as the particle size of the inorganic sunscreen agent in the sunscreen composition decreases.

The present inventors used seaweed extract in order to disperse the inorganic sunscreen in the sunscreen composition in nano size, and the inorganic sunscreen dispersed by the seaweed extract according to the present invention is substantially present in nano size using a particle size analyzer. proved that As will be described later, the sunscreen composition of the present invention has a high sun protection factor (SPF) of 30 to 40.

In one embodiment of the present invention, the inorganic sunscreen nanoparticles dispersed by the wakame extract have a particle diameter of 10 nm to 120 nm.

In another embodiment of the present invention, the inorganic sunscreen nanoparticles dispersed by the wakame extract have a particle diameter of 10 nm to 120 nm, 10 nm to 100 nm, 10 nm to 80 nm, 10 nm to 60 nm, 10 nm to 40 nm, 10 nm to 20 nm, 20 nm to 120 nm, 20 nm to 100 nm, 20 nm to 80 nm, 20 nm to 60 nm, 20 nm to 40 nm, 40 nm to 120 nm, 40 nm to 100 nm, 40 nm to 80 nm, 40 nm to 60 nm, 60 nm to 120 nm, 60 nm to 100 nm, 60 nm to 80 nm, 80 nm to 120 nm, 80 nm to 100 nm or 100 nm to 120 It may be nm, but is not necessarily limited thereto.

In one embodiment of the present invention, the seaweed extract is a re-dissolved seaweed extract powder in which water and seaweed extract powder are mixed.

As described above, the term 'dried seaweed powder' in the present specification means a powder obtained by drying and grinding seaweed.

As described above, the term 'seaweed extract powder' in the present specification means a solid component obtained by precipitating a seaweed water extract, and more specifically means a solid component precipitated by adding alcohol to the seaweed water extract. . More specifically, 'seaweed water extract' in the present specification refers to an extract obtained by mixing seaweed with water as an extraction solvent and then sonication. In the step of precipitating solid components by adding alcohol from the seaweed water extract, the alcohol used may be more specifically, for example, methanol or ethanol, and more preferably, ethanol may be used for extraction. . As the ethanol described above, 50% to 99% ethanol may be used, but is not particularly limited.

As described above, the term 'wakame extract (seaweed extract)' used herein refers to a solution extracted by adding an extraction solvent to seaweed. For example, the seaweed extract of the present invention may be a solvent extract prepared by extracting the seaweed using water as an extraction solvent, a solvent fraction thereof, a purified product of the solvent extract or solvent fraction, or a dried product. For another example, the seaweed extract of the present invention may be a solution extracted by adding a solvent to the dried seaweed powder. As another example, the seaweed extract of the present invention may be a re-dissolved seaweed extract powder obtained by mixing water with the seaweed extract powder.

As described above, the term 'reconstituted solution (redissolved solution)' in this specification refers to a solution obtained by dissolving a dried and stored powdered material in a solvent, solution, or diluent to restore it to a liquid state. .

In one embodiment of the present invention, the composition includes the wakame extract powder and inorganic sunscreen powder in a weight ratio of 1:6 to 1:20.

In another embodiment of the present invention, the composition contains the seaweed extract powder and inorganic sunscreen powder in an amount of 1:6 to 1:20, 1:6 to 1:18, 1:6 to 1:16, 1:6 to 1:14, 1:6 to 1:12, 1:6 to 1:10, 1:6 to 1:8, 1:8 to 1:20, 1:8 to 1:18, 1:8 to 1 :16, 1:8 to 1:14, 1:8 to 1:12, 1:8 to 1:10, 1:10 to 1:20, 1:10 to 1:18, 1:10 to 1:16 , 1:10 to 1:14, 1:10 to 1:12, 1:12 to 1:20, 1:12 to 1:18, 1:12 to 1:16, 1:12 to 1:14, 1 :14 to 1:20, 1:14 to 1:18, 1:14 to 1:16, 1:16 to 1:20, 1:16 to 1:18, or 1:18 to 1:20 in weight ratios include

In another embodiment of the present invention, the composition includes the wakame extract powder and the inorganic sunscreen powder in a weight ratio of 1:12 to 1:14.

In a specific embodiment of the present invention, the composition includes the wakame extract powder and the inorganic sunscreen powder in a weight ratio of 1.00:13.33, that is, 3:40.

In one embodiment of the present invention, the seaweed extract powder is included in 0.5 parts by weight to 3.5 parts by weight based on 100 parts by weight of the sum of the water and inorganic sunscreen powder.

In another embodiment of the present invention, the seaweed extract powder is 0.5 parts by weight to 3.5 parts by weight, 0.5 parts by weight to 3.4 parts by weight, 0.5 parts by weight based on 100 parts by weight of the sum of the water and inorganic sunscreen powder. part by weight to 3.3 parts by weight, 0.5 parts by weight to 3.2 parts by weight, 0.5 parts by weight to 3.1 parts by weight, 0.5 parts by weight to 3.0 parts by weight, 0.5 parts by weight to 2.8 parts by weight, 0.5 parts by weight to 2.6 parts by weight, 0.5 parts by weight to 2.4 parts by weight, 0.5 parts by weight to 2.2 parts by weight, 0.5 parts by weight to 2.0 parts by weight, 0.5 parts by weight to 1.8 parts by weight, 0.5 parts by weight to 1.6 parts by weight, 0.5 parts by weight to 1.4 parts by weight, 0.5 parts to 1.2 parts by weight 0.5 parts by weight to 1.0 parts by weight, 0.5 parts by weight to 0.8 parts by weight, 0.5 parts by weight to 0.6 parts by weight, 0.6 parts by weight to 3.5 parts by weight, 0.6 parts by weight to 3.4 parts by weight, 0.6 parts by weight to 3.3 parts by weight, 0.6 parts by weight to 3.2 parts by weight, 0.6 parts by weight to 3.1 parts by weight, 0.6 parts by weight to 3.0 parts by weight, 0.6 parts by weight to 2.8 parts by weight, 0.6 parts by weight to 2.6 parts by weight, 0.6 parts by weight to 2.4 parts by weight, 0.6 parts by weight part by weight to 2.2 parts by weight, 0.6 parts by weight to 2.0 parts by weight, 0.6 parts by weight to 1.8 parts by weight, 0.6 parts by weight to 1.6 parts by weight, 0.6 parts by weight to 1.4 parts by weight, 0.6 parts by weight to 1.2 parts by weight, 0.6 parts by weight to 1.0 parts by weight, 0.6 parts by weight to 0.8 parts by weight, 0.8 parts by weight to 3.5 parts by weight, 0.8 parts by weight to 3.4 parts by weight, 0.8 parts by weight to 3.3 parts by weight, 0.8 parts by weight to 3.2 parts by weight, 0.8 parts by weight to 3.1 parts by weight 0.8 parts by weight to 3.0 parts by weight, 0.8 parts by weight to 2.8 parts by weight, 0.8 parts by weight to 2.6 parts by weight, 0.8 parts by weight to 2.4 parts by weight, 0.8 parts by weight to 2.2 parts by weight, 0.8 parts by weight to 2.0 parts by weight, 0.8 parts by weight to 1.8 parts by weight, 0.8 parts by weight to 1.6 parts by weight, 0.8 parts by weight to 1.4 parts by weight, 0.8 parts by weight to 1.2 parts by weight, 0.8 parts by weight to 1.0 parts by weight, 1.0 parts by weight to 3.5 parts by weight, 1.0 parts by weight part by weight to 3.4 parts by weight, 1.0 parts by weight to 3.3 parts by weight, 1.0 parts by weight to 3.2 parts by weight, 1.0 parts by weight to 3.1 parts by weight, 1.0 parts by weight to 3.0 parts by weight, 1.0 parts by weight to 2.8 parts by weight, 1.0 parts by weight to 2.6 parts by weight, 1.0 parts by weight to 2.4 parts by weight, 1.0 parts by weight to 2.2 parts by weight, 1.0 parts by weight to 2.0 parts by weight, or 1.0 parts by weight to 3.5 parts by weight.

In one specific embodiment of the present invention, the seaweed extract powder is included in 3 parts by weight based on 100 parts by weight of the sum of the water and inorganic sunscreen powder.

In one embodiment of the present invention, the inorganic sunscreen powder is included in an amount of 20 wt% to 60 wt% based on 100 wt% of the sum of the water and the inorganic sunscreen powder.

In another embodiment of the present invention, the inorganic sunscreen powder is 20 wt% to 60 wt%, 20 wt% to 55 wt%, 20 wt% to 100 wt% of the sum of the water and the inorganic sunscreen powder. wt% to 50 wt%, 20 wt% to 45 wt%, 20 wt% to 40 wt%, 20 wt% to 35 wt%, 20 wt% to 30 wt%, 20 wt% to 25 wt%, 25 wt% to 60 wt%, 25 wt% to 55 wt%, 25 wt% to 50 wt%, 25 wt% to 45 wt%, 25 wt% to 40 wt%, 25 wt% to 35 wt%, 25 wt% to 30 wt% wt%, 30 wt% to 60 wt%, 30 wt% to 55 wt%, 30 wt% to 50 wt%, 30 wt% to 45 wt%, 30 wt% to 40 wt%, 30 wt% to 45 wt% , 30 wt% to 40 wt%, 30 wt% to 35 wt%, 35 wt% to 60 wt%, 35 wt% to 55 wt%, 35 wt% to 50 wt%, 35 wt% to 45 wt%, 35 wt% to 40 wt%, 40 wt% to 60 wt%, 40 wt% to 55 wt%, 40 wt% to 50 wt%, 40 wt% to 45 wt%, 45 wt% to 60 wt%, 45 wt% to 55 wt%, 45 wt% to 50 wt%, 50 wt% to 60 wt%, 50 wt% to 55 wt%, or 55 wt% to 60 wt%.

In one specific embodiment of the present invention, the inorganic sunscreen powder is included at 40 wt% based on 100 wt% of the sum of the water and the inorganic sunscreen powder.

As used herein, the term 'inorganic UV blocking agent' refers to a component containing inorganic particles having UV blocking ability. Specifically, for example, it means an inorganic metal oxide. More specifically, for example, the inorganic sunscreen agent of the present invention may include zinc oxide (ZnO), titanium dioxide (TiO ₂ ), or a mixture thereof, but is not necessarily limited thereto.

As used herein, the term 'zinc oxide (ZnO) or zinc oxide' refers to physical or inorganic particles having an effect of scattering, refracting, or reflecting UVA and UVB. Zinc oxide used in the present invention has a nanoparticle size.

As used herein, the term 'titanium dioxide (TiO ₂ ), titanium dioxide, or titanium dioxide' refers to inorganic particles having an effect of scattering, refracting, or reflecting UVA and UVB. The titanium dioxide used in the present invention has a nanoparticle size. The titanium dioxide nanoparticles used in the present invention are in the form of pure anatase phase, pure rutile phase, mixture of anatase and rutile phase, brookite phase or amorphous phase. can be More specifically, the titanium dioxide nanoparticles in the present invention are in the form of rutile.

The 'titanium dioxide nanoparticle (TiO ₂ NP) used in the present invention may be in the form of a commercially available powder. For example, a TiO ₂ NP that can be used in the present invention is commercially available as P25 TiO ₂ (a 4:1, or 7:3 mixture of anatase and rutile phases) with a diameter of about 21 nm sold by the company Evonik Degussa. ), an 85:15 mixture of rutile/anatase phases of about 10 nm to 40 nm in diameter plated in ACS Material®, and the like.

In addition, the titanium dioxide nanoparticles used in the present invention may be prepared in powder form by a method known in the art _{, for example, a TiCl 4 Hydroxy} -oxygen Flame Hydrolysis Method.

It is already known that a mixture of zinc oxide and titanium dioxide has a broader range of sunscreen effects than a single type of inorganic sunscreen. In the present invention, the mixture of zinc oxide and titanium dioxide may be prepared in any method and/or ratio known in the art to exert a sunscreen effect.

The composition for sunscreen according to the present invention contains the above-described inorganic sunscreen agent as an active ingredient for sunscreen.

In this specification, an inorganic sunscreen agent and an organic sunscreen agent are distinguished.

As used herein, the term 'organic UV blocking agent' refers to a component containing organic particles having UV blocking ability. Specifically, the organic sunscreen agent of the present specification includes avobenzene, oxybenzone, octisalate, octinoxate, homosalate, octocrylene, octyl methoxycinnamate, octyl dimethyl p-aminobenzoic acid, octyl salicylate, ethyl hexyl methoxycinnamate, ethylhexylsal Ethylhexylsalicylate, butyl methoxydibenzoylmethane, octyl triazone, menthyl anthranilate, 3,4-methylbenzylidene camphor and bis-ethylhexyloxyphenol methoxyphenyl triazine, but are included, but are not necessarily limited thereto.

In one embodiment of the present invention, the seaweed extract contains polysaccharide.

As used herein, the term 'polysaccharide or polysaccharide' refers to a polymer in which monosaccharide units are linked by a glycosidic bond. The monosaccharide may be glucose, fructose, or galactose, but is not necessarily limited thereto.

In one embodiment of the present invention, the polysaccharide is at least one polysaccharide selected from the group consisting of alginate, carrageenan, fucoidan, laminarin and agar. Including, but not necessarily limited thereto. For example, the polysaccharide may be alginic acid.

In one embodiment of the present invention, the inorganic sunscreen agent is zinc oxide (ZnO), titanium dioxide (TiO ₂ ), or a mixture thereof.

In one embodiment of the present invention, the composition has an acidity of pH 5.0 to pH 6.0.

In another embodiment of the present invention, the composition has an acidity of pH 5.0 to pH 6.0, pH 5.0 to pH 5.9, pH 5.0 to pH 5.8, pH 5.0 to pH 5.7, pH 5.0 to pH 5.6, pH 5.0 to pH 5.5 , pH 5.0 to pH 5.4, pH 5.0 to pH 5.3, pH 5.0 to pH 5.2, pH 5.0 to pH 5.1, pH 5.1 to pH 6.0, pH 5.1 to pH 5.9, pH 5.1 to pH 5.8, pH 5.1 to pH 5.7, pH 5.1 to pH 5.6, pH 5.1 to pH 5.5, pH 5.1 to pH 5.4, pH 5.1 to pH 5.3, pH 5.1 to pH 5.2, pH 5.2 to pH 6.0, pH 5.2 to pH 5.9, pH 5.2 to pH 5.8, pH 5.2 to pH 5.7, pH 5.2 to pH 5.6, pH 5.2 to pH 5.5, pH 5.2 to pH 5.4, pH 5.2 to pH 5.3, pH 5.3 to pH 6.0, pH 5.3 to pH 5.9, pH 5.3 to pH 5.8, pH 5.3 to pH 5.7 , pH 5.3 to pH 5.6, pH 5.3 to pH 5.5, pH 5.3 to pH 5.4, pH 5.4 to pH 6.0, pH 5.4 to pH 5.9, pH 5.4 to pH 5.8, pH 5.4 to pH 5.7, pH 5.4 to pH 5.6, pH 5.4 to pH 5.5, pH 5.5 to pH 6.0, pH 5.5 to pH 5.9, pH 5.5 to pH 5.8, pH 5.5 to pH 5.7, pH 5.5 to pH 5.6, pH 5.6 to pH 6.0, pH 5.6 to pH 5.9, pH 5.6 to pH 5.8, pH 5.6 to pH 5.7, pH 5.7 to pH 6.0, pH 5.7 to pH 5.9, pH 5.7 to pH 5.8, pH 5.8 to pH 6.0, pH 5.8 to pH 5.9 or pH 5.9 to pH 6.0, but necessarily limited thereto. It is not.

In another embodiment of the present invention, the composition has an acidity of pH 5.5.

In one embodiment of the present invention, the composition has a sun protection factor (SPF) of 30 to 40.

The term 'sun protection factor (SPF)' in this specification has the definition described in the "Korean Measurement Standards for UV Protection Efficacy (KMSUV)" in the notification of the Ministry of Food and Drug Safety. More specifically, it means an index representing the blocking effect of a product that blocks UVB. The sunscreen index of the present invention can be measured by the method described in KMSUV.

In another embodiment of the present invention, the composition has an SPF of 30 to 40, 30 to 39, 30 to 38, 30 to 37, 30 to 36, 30 to 35, 30 to 34, 30 to 33, 30 to 32 , 30 to 31, 31 to 40, 31 to 39, 31 to 38, 31 to 37, 31 to 36, 31 to 35, 31 to 34, 31 to 33, 31 to 32, 32 to 40, 32 to 39, 32 to 38, 32 to 37, 32 to 36, 32 to 35, 32 to 34, 32 to 33, 33 to 40, 33 to 39, 33 to 38, 33 to 37, 33 to 36, 33 to 35, 33 to 34 , 34 to 40, 34 to 39, 34 to 38, 34 to 37, 34 to 36, 34 to 35, 35 to 40, 35 to 39, 35 to 38, 35 to 37, 35 to 36, 36 to 40, 36 to 39, 36 to 38, 36 to 37, 37 to 40, 37 to 39, 37 to 38, 38 to 40, 38 to 39, or 39 to 40.

In another embodiment of the present invention, the composition has an SPF of 31.0 to 37.0.

In a specific embodiment of the present invention, the composition has an SPF of 35.2 ± 2.5. That is, the SPF of the sunscreen composition of the present invention is 32.7 to 37.7.

In one embodiment of the present invention, the whitening phenomenon is suppressed when the composition is applied to the skin.

As used herein, the term 'suppression' encompasses the calming, eradication, or relative reduction of a certain phenomenon.

Compared to a composition containing only an inorganic sunscreen, the sunscreen composition of the present invention suppresses cloudiness when applied to the skin. In addition, the composition for sunscreen of the present invention suppresses cloudiness when applied to the skin compared to a composition containing a conventional dispersant and an inorganic sunscreen agent. Specifically, the composition for sunscreen of the present invention contains ammonium polyacrylic acid (APA), dibasic ammonium citrate (DAC), or polyvinylpyrrolidone (PVP) as a dispersant and inhibits cloudiness when applied to the skin compared to a composition containing an inorganic sunscreen agent do.

In another embodiment of the present invention, the sunscreen composition has improved or improved spreadability when applied to the skin compared to a sunscreen composition containing only an inorganic sunscreen agent. In addition, the sunscreen composition of the present invention improves or improves the spreadability when applied to the skin compared to a conventional composition containing a dispersant and an inorganic sunscreen agent. Specifically, the sunscreen composition of the present invention contains APA, DAC or PVP as a dispersant and has improved or improved applicability when applied to the skin compared to a composition containing an inorganic sunscreen agent.

The sunscreen composition of the present invention may further include ingredients commonly used in cosmetic compositions, for example, antioxidants, stabilizers, solubilizers, vitamins, pigments, and conventional adjuvants such as fragrances, and carriers. may additionally include.

In one embodiment of the present invention, the composition of the present invention further comprises a cosmetically acceptable carrier. The cosmetically acceptable carrier of the present invention includes purified water, monohydric alcohols (ethanol or propyl alcohol), polyhydric alcohols (glycerol, 1,3-butyrene glycol or propylene glycol), higher fatty acids (palmitylic acid or linolenic acid) , Fats and oils (wheat germ oil, camellia oil, jojoba oil, olive oil, squalene, sunflower oil, macadamia peanut oil, avogard oil, soybean hydrolyzed lecithin or fatty acid glycerides) may be used, but are not necessarily limited thereto. . In addition, bactericides, antioxidants, anti-inflammatory and cooling agents can be added as needed.

Hinothiol, triclosan, chlorhexidine gluconate, phenoxyethanol, resorcin, isopropylmethylphenol, azulene, salicylic acid, zinc pyritaone, and the like can be used as the disinfectant of the present invention.

As the antioxidant of the present invention, at least one selected from the group consisting of butylhydroxyanisole, gallic acid, gallic acid propyl, and erythorbic acid may be used.

As the anti-inflammatory agent of the present invention, dipotassium glycyrrhizinate or allantoin may be used, and as a cooling agent, red pepper tincture or 1-menthol may be used.

In one embodiment of the present invention, the composition of the present invention is skin, lotion, toner, essence, gel, cream, eye cream, hand cream, pack, BB cream, CC cream, spray, makeup base, makeup foundation, liquid foundation , It may have any one formulation selected from the group consisting of cream foundation, stick foundation, powder, powder pact, cushion cosmetic composition, blush, pencil, spot, concealer, lipstick, lip gloss and eye shadow.

The sunscreen composition of the present invention may have functions such as color expression, brightness, whitening, moisturizing, anti-wrinkle, anti-aging, and pearl feeling as well as a sun protection function.

According to another aspect of the present invention, the present invention provides a method for preparing a sunscreen composition according to an embodiment comprising the following steps:

i) Seaweed extract powder, which is a re-dissolved seaweed extract powder, by mixing seaweed extract powder with water so that the seaweed extract powder is 0.5 to 3.5 parts by weight based on 100 parts by weight of the sum of water and inorganic sunscreen powder. Obtaining; and

ii) The inorganic sunscreen powder is added to the seaweed extract, which is a re-dissolved seaweed extract powder, so that the inorganic sunscreen powder is 20 wt% to 60 wt% with respect to 100 wt% of the sum of the water and inorganic sunscreen powder step of adding.

As described above, in the present specification, 'dried seaweed powder' refers to a powder obtained by drying and pulverizing seaweed, and in the present specification, 'seaweed extract powder' is after adding distilled water to the dried seaweed powder, sonicating, bathing in water, and It means a powder obtained from the precipitate obtained by mixing alcohol with the filtrate obtained after filtration. In addition, in the present specification, 'seaweed extract' refers to a solution extracted by adding an extraction solvent to seaweed, and encompasses a re-dissolved seaweed extract powder obtained by mixing water or purified water as an extraction agent with the seaweed extract powder. In the present specification, 'redissolved material' refers to a solution obtained by dissolving a dried and stored powdered material in a solvent, solution, or diluent and restoring it to a liquid state.

The inventors of the present invention, through a relatively simple manufacturing method of stirring and sonicating seaweed extract powder and titanium dioxide nanoparticle powder at room temperature, a sunscreen composition containing titanium dioxide nanoparticles dispersed by seaweed extract as an active ingredient has been developed.

In one embodiment of the present invention, the inorganic sunscreen agent is zinc oxide (ZnO), titanium dioxide (TiO ₂ ), or a mixture thereof.

In one embodiment of the present invention, the step of stirring at room temperature is additionally included after step i).

In one embodiment of the present invention, a step of ultrasonication is further included after step ii).

In one embodiment of the present invention, the ultrasonic treatment (ultrasonication) is performed for 5 minutes to 1 hour at 20 kHz. In another embodiment of the present invention, the ultrasonic treatment (ultrasonication) is performed for 30 minutes at 20 kHz.

In one embodiment of the present invention, the seaweed extract powder is obtained by a method comprising the following steps:

a) drying and pulverizing seaweed to obtain dried seaweed powder;

b) mixing the dried seaweed powder and distilled water at a weight ratio of 1:10 to 1:30 and then ultrasonicating;

c) heating the sonication product at 40° C. to 60° C.;

d) obtaining a filtrate by centrifuging the product of the water bath and filtering the solid content; and

e) mixing the filtrate with ethanol to obtain a precipitate.

In one embodiment of the present invention, the seaweed in step a) is an algae belonging to the seaweed family Laminariales ( Alariaceae ).

In another embodiment of the present invention, the wakame of step a) belongs to brown algae.

In one embodiment of the present invention, after step d) and before step e), the step of storing the filtrate obtained in step d) at 4°C is additionally included.

In one embodiment of the present invention, the precipitate of step e) contains polysaccharide.

In one embodiment of the present invention, the polysaccharide is at least one polysaccharide selected from the group consisting of alginate, carrageenan, fucoidan, laminarin and agar. include

As used herein, the term 'ultrasonication' refers to a process of disrupting or homogenizing a chemical solution or biological medium using ultrasound. Frequencies above 20 kHz are generally used for sonication, and ultrasonic probes, also known in the art as ultrasonic baths, ultrasonic homogenizers, or sonicators ) can be used for sonication.

The manufacturing method of the sunscreen composition of the present invention will be described step by step.

Step i) The seaweed extract powder is mixed with water so that the seaweed extract powder is 0.5 to 3.5 parts by weight based on 100 parts by weight of the sum of water and inorganic sunscreen powder, and the seaweed extract powder is re-dissolved seaweed. obtaining an extract

This step i) is a step for obtaining the seaweed extract. Seaweed extract powder is mixed with water so that the seaweed extract powder is 0.5 parts by weight to 3.5 parts by weight, for example, 3.0 parts by weight, based on 100 parts by weight of the sum of water and inorganic sunscreen powder. to obtain The seaweed extract is a re-dissolved seaweed extract powder.

A step of stirring at room temperature may be additionally included after step i).

The seaweed extract powder of step i) can be obtained by a method comprising the following steps: a) drying and pulverizing seaweed to obtain dried seaweed powder; b) mixing the dried seaweed powder and distilled water at a weight ratio of 1:10 to 1:30 and then ultrasonicating; c) heating the sonication product at 40° C. to 60° C.; d) obtaining a filtrate by centrifuging the product of the water bath and filtering the solid content; and e) mixing the filtrate with ethanol to obtain a precipitate.

Step a) is a process of obtaining dried seaweed powder by drying and pulverizing seaweed. The drying may be performed in natural light. The crushing may be performed using a blender. The wakame of step a) is algae belonging to the seaweed family of the kelp order, or belongs to brown algae.

Step b) is a step of mixing distilled water with the dried seaweed powder and ultrasonicating it. The dried seaweed powder and distilled water may be mixed at a weight ratio of 1:10 to 1:30, for example, at a weight ratio of 1:20. After mixing, it is sonicated.

Step c) is a step of heating the ultrasonic treatment product, which is the result of step b). The water bath may be performed at 40° C. to 60° C. in an oil bath, for example, at 50° C. After the hot water bath, it may be cooled to room temperature.

Step d) is a step of centrifuging the product of step c), filtering the solid content, and obtaining a filtrate. The resulting water bath is centrifuged at 4,000 rpm for 10 minutes to precipitate. Then, the precipitated solids are filtered and a filtrate, that is, an extract after filtration is obtained. The filtrate, that is, an extract after filtration can be stored at 4° C. until used in the next step.

Step e) is a step of obtaining a precipitate by mixing ethanol with the filtrate, which is the result of step d). Ethanol was added to the filtrate in a volume ratio of 1:3 to precipitate under gravity. Any solvent that can precipitate the polysaccharide in seaweed can be used as a substitute for ethanol without limitation. After precipitation, the supernatant is discarded to obtain a precipitate. The precipitate contains polysaccharides. The polysaccharide contains alginic acid.

The obtained precipitate may be additionally subjected to a drying step. The obtained precipitate containing the polysaccharide may be additionally subjected to a step of drying at room temperature and 0.1 atm.

The seaweed before performing step a) may be desalted. The seaweed may be desalted using distilled water. The seaweed may be dried after removing salt. The seaweed may be dried in natural light after desalination. The seaweed may be dried in natural light after removing salt using distilled water.

Seaweed extract powder obtained by the above method is mixed with water to obtain seaweed extract. Specifically, the seaweed extract powder and water may be mixed at room temperature to obtain the seaweed extract. More specifically, the seaweed extract powder and water may be mixed at room temperature and then stirred to obtain the seaweed extract. More specifically, the seaweed extract powder is mixed at room temperature so that the seaweed extract powder is 0.5 to 3.5 parts by weight, for example, 3.0 parts by weight, based on 100 parts by weight of the sum of water and inorganic sunscreen powder. ) and then stirred to obtain seaweed extract powder re-dissolved seaweed extract.

Step ii) The inorganic sunscreen powder is added to the seaweed extract, which is a re-dissolved seaweed extract powder, so that the inorganic sunscreen powder is 20 wt% to 60 wt% with respect to 100 wt% of the sum of the water and the inorganic sunscreen powder additional step of adding

Step ii) is a step of obtaining a sunscreen composition by additionally adding an inorganic sunscreen agent to the wakame extract obtained in step i).

Inorganic sunscreen powder is additionally added to the seaweed extract, which is a re-dissolved seaweed extract powder, so that the inorganic sunscreen powder is 20 wt% to 60 wt% with respect to 100 wt% of the sum of the water and inorganic sunscreen powder. . Stirring may be done after addition. A step of sonicating after the stirring, that is, after the step ii) may be additionally included. The sonication may be performed at 20 kHz for 5 minutes to 1 hour, for example, 30 minutes. A slurry can be obtained after sonication. The resulting slurry may be dried.

For example, 0.5 parts by weight to 3.5 parts by weight of the seaweed extract powder is included with respect to 100 parts by weight of the sum of water and inorganic sunscreen powder, and 100 wt% of the total of water and inorganic sunscreen powder Inorganic sunscreen powder is additionally added to the seaweed extract, which is the re-dissolved seaweed extract powder, so that the weight of the inorganic sunscreen powder is 20 wt% to 60 wt%.

Specifically, in step i), seaweed extract powder is mixed with water so that the weight of seaweed extract powder is 3.0 parts by weight based on 100 parts by weight of the sum of water and titanium dioxide powder. An extract is obtained. In step ii), inorganic sunscreen powder is additionally added to the seaweed extract, which is a re-dissolved seaweed extract powder, so that the weight of the inorganic sunscreen powder is 40 wt% with respect to 100 wt% of the sum of water and titanium dioxide powder . Mixing by stirring and sonication to obtain a 40 wt% titanium dioxide slurry dispersed by the seaweed extract, thereby obtaining a sunscreen composition comprising the seaweed extract and titanium dioxide of the present invention.

Specifically, in step i), seaweed extract powder is mixed with water so that the seaweed extract powder is 3.0 parts by weight based on 100 parts by weight of the sum of water and zinc oxide powder. to obtain In step ii), the inorganic sunscreen powder is additionally added to the seaweed extract, which is the re-dissolved seaweed extract powder, so that the inorganic sunscreen powder is 40 wt% with respect to 100 wt% of the sum of water and zinc oxide powder. Mixing by stirring and sonication to obtain a 40 wt% zinc oxide slurry dispersed by the seaweed extract, thereby obtaining a sunscreen composition comprising the seaweed extract and zinc oxide of the present invention.

Since the manufacturing method of the sunscreen composition of the present invention is a method of manufacturing the sunscreen composition, which is another aspect of the present invention described above, duplicate contents are used to avoid excessive complexity of the description in this specification, and the description thereof is omitted. do.

The features and advantages of the present invention are summarized as follows:

(a) The present invention provides a sunscreen composition comprising seaweed extract and an inorganic sunscreen agent.

(b) The present invention provides a method for preparing the above-described sunscreen composition.

(c) In the case of using the sunscreen composition of the present invention, seaweed extract is used instead of chemical substances as a dispersant for inorganic sunscreen, so it is harmless to the human body, environmentally friendly, and exhibits high sunscreen performance, and at the same time, there is no clouding phenomenon, so it has good spreadability Since it is excellent, it can be usefully used in a cosmetic composition with a sunscreen function.

Figure 1 shows a method for producing seaweed extract according to an embodiment of the present invention.
Figure 2 shows the wakame extract according to one embodiment of the present invention contained in a 50 ml conical tube (Conical tube).
Figure 3 shows a method for producing a functional sunscreen using seaweed extract according to an embodiment of the present invention.
4 shows nanoparticles of a functional sunscreen according to an embodiment of the present invention. The nanoparticles are composed of a core part made of TiO ₂ and a shell part made of seaweed extract coating the core part.
Figure 5a shows a macroscopic image of the functional blocking composition for each dispersant before centrifugation in the sedimentation test (Wakame extract: seaweed extract; APA: Ammonium Polyacrylic Acid; DAC: Dibasic Ammonium Citrate; and PVP: PolyVinylPyrrolidone).
Figure 5b shows a macroscopic image of the functional blocking composition for each dispersant after centrifugation in the sedimentation test. The presence and size of sedimentation are highlighted with circles so that they can be compared.
FIG. 6a is a result of particle distribution analysis of a 1 wt% TiO ₂ suspension, and shows the volume (%) according to the particle diameter (μm).
Figure 6b shows the results of particle distribution analysis for each dispersant (Wakame (▼), DAC (●), APA (■), and PVP (▲)) added to the 1 wt% TiO ₂ suspension, and the volume according to the particle diameter (μm). (%). The particle diameter distribution of the sunscreen composition containing wakame extract, which was well distributed without aggregation, was indicated by arrows, and the particle diameter distribution of the composition containing DAC or APA in which aggregation was formed was indicated by red circles.
Figure 7 (a) shows the spreadability test results of the sunscreen containing titanium dioxide nanoparticles (TiO ₂ bare) to which no dispersant is added, and (b) of Figure 7 shows the dioxide to which the wakame extract dispersant of the present invention is added. The spreadability test results of the sunscreen containing titanium nanoparticles are shown.
8 shows the L-value, that is, skin color, before and after skin application of the sunscreen composition containing seaweed extract and the control composition (TiO ₂ bare) for sunscreen without seaweed extract according to the present invention measured using a color difference meter.

Hereinafter, the present invention will be described in more detail through examples. These examples are only for explaining the present invention in more detail, and it will be apparent to those skilled in the art that the scope of the present invention is not limited by these examples according to the gist of the present invention. .

Example

The present inventors prepared a composition for sunscreen including an inorganic blocking component dispersed by the seaweed extract by using the seaweed extract as a dispersing agent. Hereinafter, a method for preparing a seaweed extract and a method for preparing a sunscreen composition including the seaweed extract as a dispersant for an inorganic blocking component will be described.

Example 1: Preparation of seaweed extract

The method for preparing seaweed extract according to the present invention includes the following steps: washing and drying; crushing step; sonication step; bathing step; filtration step; precipitation step; and a drying step. A schematic diagram of the method for preparing the seaweed extract of the present invention is shown in FIG.

The seaweed used to prepare the seaweed extract was brown algae native to Korea belonging to the Laminariales seaweed family ( Alariaceae ), but the seaweed that can be used in the present invention is an alga belonging to the seaweed family It will be apparent to those skilled in the art that it can be used without limitation.

1-1: washing and drying step

The brown algae described above, that is, seaweed, was washed with distilled water, desalted, and then dried in natural light.

1-2: crushing step

The washed and dried seaweed was pulverized using a blender to prepare "dried seaweed powder".

1-3: sonication step

The dry seaweed powder obtained in 1-2 and distilled water were mixed in a weight ratio of 1:20, and then ultrasonication was continuously performed on the mixture for 30 minutes.

1-4: Bathing step

After the ultrasonic treatment performed in 1-3 above, it was heated in a water bath at 50° C. and cooled to room temperature. Silicone oil was used for the oil bath. In this specification, 'room temperature' means 20 ± 5 ℃.

1-5: filtration step

After the water bath, the mixture cooled to room temperature was centrifuged at 4,000 rpm for 10 minutes to precipitate. Then, the precipitated solids were filtered, and only the filtrate, i.e., the extract after filtration, was obtained and stored at 4°C.

1-6: precipitation step

Ethanol was mixed with the filtrate stored at 4° C. in a volume ratio of 1:3 and then precipitated under gravity. The supernatant was discarded and a precipitate was obtained. The precipitate contains polysaccharide.

1-7: drying step

The precipitate containing the polysaccharide obtained in 1-6 above was dried at room temperature and 0.1 atm to obtain the “seaweed extract powder” of the present invention.

1-8: Preparation of seaweed extract of the present invention

Mix the seaweed extract powder with water so that the seaweed extract powder is 3 parts by weight based on 100 parts by weight of the sum of water and TiO ₂ NP powder (titanium dioxide nanoparticle powder), and at about 200 rpm at room temperature 1 Stir for an hour. The result was referred to as "seaweed extract", which is a re-dissolved seaweed extract powder. The wakame extract of the present invention is shown in FIG. 2 . As used herein, 'about' means ±10%, specifically ±5%, and more specifically ±1% of the designated value, unless stated otherwise.

Example 2: Preparation of the sunscreen composition of the present invention - TiO ₂ /Seaweed extract suspension

A TiO ₂ /seaweed extract suspension, which is an embodiment of the sunscreen composition according to the present invention, was prepared. Titanium dioxide nanoparticle powder (TiO ₂ NP powder) with D50 (median diameter) = 15 nm of the anatase phase was purchased from US Research Nanomaterials, Inc.

An inorganic sunscreen powder is additionally added to the seaweed extract, which is the re-dissolved seaweed extract powder of Example 1, so that the TiO ₂ NP powder is 40 wt% with respect to 100 wt% of the sum of the water and the TiO ₂ NP powder. . They were then mixed by stirring and ultrasonication at 20 kHz for 30 minutes.

As a result, 40 wt% of a titanium dioxide slurry dispersed by the seaweed extract was obtained (see FIG. 3). The resulting slurry was referred to as TiO ₂ /seaweed extract suspension. The composition of the TiO ₂ /seaweed extract suspension, which is a sunscreen composition according to an embodiment of the present invention, is shown in Table 1 below.

Hereinafter, in order to compare the dispersion characteristics of suspensions containing titanium dioxide nanoparticles according to the type of dispersant, a suspension of titanium dioxide nanoparticles was prepared using a conventional dispersant.

Comparative Example 1: TiO ₂ /APA (ammonium polyacrylate) suspension

A TiO ₂ /APA suspension was prepared in the same manner as in Example 2, using ammonium polyacrylate (APA) as a dispersing agent for titanium dioxide. APA powder was purchased from Samchun Chemicals.

APA powder was added to water so that the APA powder was 3 parts by weight based on 100 parts by weight of the total of water and TiO ₂ NP powder, and stirred at room temperature at about 200 rpm for 1 hour. After stirring, 40 wt% of TiO ₂ NP powder was added to 100 wt% of the sum of water and TiO ₂ NP powder, and mixed by stirring and sonication at 20 kHz for 30 minutes.

As a result, 40 wt% of a titanium dioxide slurry containing APA as a dispersant was obtained. The resulting slurry was referred to as Comparative Example 1 TiO ₂ /APA Suspension. The composition of the TiO ₂ /APA suspension according to a comparative example of the present invention is shown in Table 1 below.

Comparative Example 2: TiO ₂ /DAC (Dibasic Ammonium Citrate) Suspension

A TiO ₂ /DAC suspension was prepared in the same manner as in Example 2, using diammonium citrate (DAC) as a dispersing agent for titanium dioxide. DAC powder was purchased from Sigma-Aldrich.

DAC powder was added to water so that the DAC powder was 3 parts by weight based on 100 parts by weight of the sum of water and TiO ₂ NP powder, and stirred at room temperature at about 200 rpm for 1 hour. After stirring, 40 wt% of TiO ₂ NP powder was added to 100 wt% of the sum of water and TiO ₂ NP powder, and mixed by stirring and sonication at 20 kHz for 30 minutes.

As a result, 40 wt% of a titanium dioxide slurry containing DAC as a dispersant was obtained. The resulting slurry was referred to as TiO ₂ /DAC suspension. The composition of the TiO ₂ /DAC suspension according to a comparative example of the present invention is shown in Table 1 below.

Comparative Example 3: TiO ₂ /PVP (polyvinylpyrrolidone) suspension

A TiO ₂ /PVP suspension was prepared in the same manner as in Example 2, using polyvinylpyrrolidone (PVP) as a dispersing agent for titanium dioxide. PVP powder was purchased from BASF (Germany).

PVP powder was added to water so that the PVP powder was 3 parts by weight based on 100 parts by weight of the total of water and TiO ₂ NP powder, and stirred at room temperature at about 200 rpm for 1 hour. After stirring, 40 wt% of TiO ₂ NP powder was added to 100 wt% of the sum of water and TiO ₂ NP powder, and mixed by stirring and sonication at 20 kHz for 30 minutes.

As a result, 40 wt% of a titanium dioxide slurry containing PVP as a dispersant was obtained. The resulting slurry was referred to as TiO ₂ /PVP suspension. The composition of the TiO ₂ /PVP suspension according to a comparative example of the present invention is shown in Table 1 below.

Comparative Example 4: 1 wt% TiO ₂ Suspension - no dispersant

1 wt% of titanium dioxide nanoparticle powder was added to 99 wt% of water, that is, 1 part by weight of titanium dioxide nanoparticle powder was added to 99 parts by weight of water, stirred and Mix by sonicating for 10 minutes. As a result, 1 wt% of titanium dioxide slurry was obtained. The resulting slurry was referred to as a 1 wt % TiO ₂ suspension. The 1 wt% TiO ₂ suspension was used as a control in the particle diameter distribution analysis of Example 4 to be described later. The composition of the 1 wt% TiO ₂ suspension according to a comparative example of the present invention is shown in Table 1 below.

Comparative Example 5: 40 wt% TiO ₂ Suspension - no dispersant

40 wt% of titanium dioxide nanoparticle powder is added to 60 wt% of water, that is, 40 parts by weight of titanium dioxide nanoparticle powder is added to 60 parts by weight of water, stirred and 30 parts by weight at 20 kHz Mix by sonicating for 10 minutes. As a result, 40 wt% of a wt% titanium dioxide slurry dispersed by the wakame extract was obtained. The resulting slurry was referred to as 40 wt % TiO ₂ suspension or TiO ₂ bare. The 40 wt% TiO ₂ suspension was used as a control in the spreadability test of Example 5 to be described later. The composition of the 40 wt% TiO ₂ suspension according to a comparative example of the present invention is shown in Table 1 below.

division dispersant water TiO ₂ nanoparticle powder gun parts by weight Total 100 parts by weight parts by weight Example 2 Seaweed Extract Powder 3 60 40 103 Comparative Example 1 APA powder 3 60 40 103 Comparative Example 2 DAC powder 3 60 40 103 Comparative Example 3 PVP powder 3 60 40 103 Comparative Example 4 doesn't exist 0 99 One 100 Comparative Example 5 doesn't exist 0 60 40 100

Example 3: Sedimentation Test - Comparison of Dispersion Characteristics of Titanium Dioxide Nanoparticles for Different Dispersing Agents

The above-described TiO ₂ /seaweed extract suspension of Example 2, TiO ₂ /APA suspension of Comparative Example 1, TiO ₂ /DAC suspension of Comparative Example 2, and TiO ₂ /PVP suspension of Comparative Example 3 were subjected to a sedimentation test to form a precipitate. Whether or not and the degree of formation were analyzed.

Titanium dioxide nanoparticle dispersion (TiO ₂ nanoparticle dispersion) is mainly used as a white pigment (pigment) because of its high refractive index, strong light scattering, light reflection ability and high UV resistance. That is, the dispersed titanium dioxide nanoparticle suspension has a white color.

In the sedimentation test, when aggregation between particles in a suspension occurs, the size of the particles increases and settles. However, when aggregation between particles in the suspension does not occur, the size of the well-dispersed particles does not increase and does not settle. Therefore, it can be seen that the more precipitate is generated after the sedimentation test, the more aggregation between the particles in the suspension occurs.

Before Sedimentation Test

Before performing the sedimentation test, 40 ml each of TiO ₂ /seaweed extract suspension, TiO ₂ /APA suspension, TiO ₂ /DAC suspension and TiO ₂ /PVP suspension was placed in a 50 ml conical tube (Falcon ^® ). added. For comparison with after the sedimentation test, before the sedimentation test, the tube was turned upside down and a photograph was taken, and shown in FIG. 5A.

As shown in Figure 5a, all the tubes containing the TiO ₂ suspension before the sedimentation test showed a white color.

Sedimentation test method

A sedimentation test was performed by centrifuging 40 ml of the suspension at 4,000 rpm for 30 minutes at room temperature. Carefully take out each conical tube from the centrifuge, turn the tube upside down as before performing the sedimentation test, take a picture of the tube, and, as shown in FIG. 5B, for comparison of the presence and size of sedimentation, the conical tube The bottom is highlighted with a circle.

After Sedimentation Test

As shown in Figure 5b, no sedimentation was observed at the bottom of the conical tube (wakame extract) containing the TiO ₂ / seaweed extract suspension according to the present invention (no sedimentation), and the TiO ₂ / seaweed extract suspension was still white. showed up This means that the titanium dioxide nanoparticles were well dispersed by the seaweed extract and hardly aggregated in the suspension.

However, in the TiO ₂ suspension containing APA, DAC, and PVP as dispersing agents, precipitates were observed at the bottom of the conical tube, and the size of the precipitates increased in the order of APA, DAC, and PVP (see the circle mark in Fig. 5b and the note at the top). . Particularly, in PVP, it was confirmed that almost all titanium dioxide nanoparticles were not dispersed and aggregated and precipitated to the extent that the color of the suspension, which was white before centrifugation, became transparent.

From the above results, it was confirmed that the titanium dioxide nanoparticles dispersed by the wakame extract according to the present invention were well dispersed in the suspension without forming agglomerates compared to conventional dispersants.

Example 4: Particle diameter distribution analysis

In the above-described Example 3, the dispersibility of titanium dioxide nanoparticles for each dispersant was compared by visually checking the presence and size of titanium dioxide nanoparticle precipitates for each dispersant through a sedimentation test using centrifugation. In this Example 4, particle size distribution by laser diffraction was measured using a particle size analyzer (PSA, Malvern Panalytical).

4-1: 1 wt % TiO ₂ Particle diameter distribution analysis result of suspension

First, the ratio of the 1 wt% TiO ₂ suspension of Comparative Example 4 without the addition of a dispersant and distilled water was diluted to 1:100, and the volume (%) for each particle size was analyzed using a particle size analyzer (PSA), and the results are It is shown in Figure 6a.

As shown in FIG. 6a, the particle size was about 900 μm to 1500 μm, which indicates poor stabilization as expected because no _dispersant was added. It was confirmed that the titanium nanoparticles were not dispersed but agglomerated.

4-2: TiO by dispersant ₂ Particle diameter distribution analysis result of suspension

TiO ₂ /seaweed extract suspension of Example 2, TiO ₂ /APA suspension of Comparative Example 1, TiO ₂ /DAC suspension of Comparative Example 2, and TiO ₂ /PVP suspension of Comparative Example 3 with distilled water and The ratio of was diluted to 1:100, and the volume (%) for each particle size was analyzed using PSA, and the results are shown in FIG. 6B.

As shown in Figure 6b, the TiO ₂ /seaweed extract suspension (Wakame, ▼) of Example 2 of the present invention exhibits a particle size distribution of 10 nm to 120 nm (ie, 0.01 μm to 0.120 μm), It was confirmed that the dispersion was well performed and there was no aggregation.

In the case of the TiO ₂ /APA suspension (APA, ■) of Comparative Example 1, dispersion was achieved, but the volume graph by particle size compared to Wakame, which is Example 2 of the present invention, showed a rightward shifted particle size distribution, and slightly at about 900 μm. showed aggregation. In the case of the TiO ₂ /DAC suspension (DAC, ●) of Comparative Example 2, although dispersion was achieved, the volume graph by particle size compared to Wakame, which is Example 2 of the present invention, showed a particle size distribution that moved upward, and at about 900 μm Aggregation was shown by about 2% by volume.

Moreover, the TiO ₂ /PVP suspension (PVP, ▲) of Comparative Example 3 had no volume corresponding to the particle size of 10 nm to 120 nm, and the 1 wt% TiO ₂ suspension of Comparative Example 4 without the addition of a dispersant was The stabilization was poor, similar to the volume graph. Therefore, it was confirmed that when PVP was used as a dispersing agent, titanium dioxide was not dispersed and agglomerated.

The result of particle diameter distribution analysis by laser diffraction in this example is consistent with the result of the sedimentation test in which the size of the precipitate increases in the order of APA, DAC, and PVP visually confirmed in Example 3 described above.

From the above results, the present inventors confirmed that the titanium dioxide nanoparticles were well dispersed without aggregation by 3 wt% of the seaweed extract compared to other dispersants.

Example 5: Spreadability test

In Examples 3 and 4 described above, it was confirmed that the seaweed extract worked well as a dispersing agent for titanium dioxide. In this Example 5, it was attempted to confirm whether the TiO ₂ /seaweed extract suspension of the present invention was well dispersed without aggregation and had excellent spreadability.

The above-described TiO ₂ /seaweed extract suspension of Example 2 and the 40 wt% TiO ₂ suspension of Comparative Example 5 containing no seaweed extract were applied to the back of the hand or black colored paper, and the spreadability was tested. 50 μl/cm ² of each suspension was applied to the skin and black paper in an area of 10 cm ² each, and images were obtained with a camera and are shown in FIG. 7 .

In (a) of FIG. 7, 40 wt% TiO ₂ suspension (bare) to which no dispersant was added was applied to the back of the hand and black colored paper, and the spreadability test results were shown to examine whether clumping and whether or not there was a clouding phenomenon were shown. As shown in the part marked with a red circle in the lower left part of Figure 7 (a), the suspension was clumped on the back of the hand, so it was not spread well, and a whitish phenomenon appeared, and even when applied to black paper, clumping and The cloudiness phenomenon appeared conspicuously.

As shown in (b) of FIG. 7, the result of applying the TiO ₂ /seaweed extract suspension of Example 2 to the back of the hand and black paper, compared with (a) of FIG. 7 in which the suspension without a dispersant was applied. Then, it was confirmed that the cloudiness phenomenon, in which the suspension aggregates or turns white, was significantly reduced. The titanium dioxide nanoparticle suspension dispersed by the wakame extract of the present invention hardly showed aggregation and cloudiness on the back of the hand and black colored paper.

From the above results, the present inventors confirmed that when the titanium dioxide nanoparticle suspension dispersed by the wakame extract was applied to the skin and black paper, there was little or no clumping and whitening phenomenon, resulting in excellent spreadability.

By using the seaweed extract of the present invention as a dispersing agent for inorganic sunscreen, it was possible to solve the problems of the prior art, such as poor application of inorganic sunscreen, cloudiness, and unnatural skin expression during application.

Example 6: Skin patch safety evaluation

In order to evaluate the skin safety of the seaweed extract-containing sunscreen composition (TiO ₂ /seaweed extract suspension) according to Example 2 of the present invention, a skin patch safety human application test was requested to the Oriental Bioindustry Clinical Support Center of Semyung University. The skin patch safety human application test study was conducted in accordance with the evaluation criteria presented by the International Contact Dermatitis Research Group (ICDRG) and the regulations of the Oriental Bioindustry Clinical Support Center of Semyung University (research control number: JI- 1126-A; Report Control Number: SMC-210305-7453). As a control composition, a 40 wt% TiO ₂ suspension of Comparative Example 5 not containing seaweed extract was used.

6.1: Skin patch safety evaluation method

The skin patch safety evaluation was conducted in a closed patch method using a Finn Chamber on 30 adults aged 20 to 55 years. The subject's back was wiped with 70% ethanol and dried, and the suspension of Example 2 (labeled as sunscreen (LB-20210128-01)) and the suspension of Comparative Example 5 (sunscreen (LB-C-20210128-01) 01)) was dropped into the pin chamber by 25 μl each, and then placed on the subject's back and fixed.

The patch was removed after 24 hours, and after removing the patch, the test site was marked with a marking pen, and after 30 minutes, 24 hours, and 48 hours, the test site was observed and the skin reaction was evaluated. The evaluation was performed according to the center's internal guidelines (SOP), and matters not specified in the Ministry of Food and Drug Safety notice were performed by referring to the references.

Judgment was made at 30 minutes, 24 hours, and 48 hours after removing the patch, and the degree of irritation was classified according to the skin reaction criteria of the International Contact Dermatitis Research Group (ICDRG) below.

1) Negative (-): no stimulation (score: 0)

2) Doubtful or slight reaction and erythema (±): no stimulation (score: 0.5)

Faint or barely perceptible mild erythema

3) Erythema + Induration (+): mild stimulation (score: 1)

Well-circumscribed but mild erythema, edema, and papules

4) Erythema + Induration + Vesicle (++): Moderate stimulation (score: 2)

Marked erythema, papules and vesicles

5) Erythema + Induration + Bullae (++++): strong stimulation (score: 3)

Severe erythema and blisters, scab formation

6.2: Skin patch safety evaluation results

The human application test results for skin patch safety evaluation are shown in Tables 2 and 3 below. As shown in Table 2 below, "Sunscreen (LB-C-20210128-01)", a suspension of Comparative Example 5 of the present invention, did not cause irritation at 30 minutes, 24 hours, and 48 hours after patch removal. The average skin reactivity was 0.00, and the suspension of Comparative Example 5, "Sunscreen (LB-C-20210128-01)", was judged to be non-irritating according to the criteria of the skin patch test.

In addition, as shown in Table 3 below, "Sunscreen (LB-20210128-01)", the suspension of Example 2 of the present invention, did not cause irritation at 30 minutes, 24 hours, and 48 hours after patch removal. The average skin reactivity was 0.00, and the suspension of Example 2 of the present invention, "Sunscreen (LB-20210128-01)", was determined to be non-irritating according to the criterion of the skin patch test.

From the above results, the present inventors confirmed that the sunscreen composition containing wakame extract belongs to the non-irritant group, thereby confirming skin safety when applied to the human body.

Example 7: Evaluation of UV blocking performance

In order to evaluate the sunscreen performance of the seaweed extract-containing sunscreen composition of the present invention, a human application test was requested to evaluate the sunscreen index at the Clinical Support Center for Oriental Bioindustry, Semyung University. In this evaluation, the basic test data obtained according to the standard operating instructions of the Oriental Bioindustry Clinical Support Center of Semyung University and the guideline for cosmetics human application test (Ministry of Food and Drug Safety Notice No. 2019-47) were accurately reflected (research control number: JI -1454-A and JI-1455-A; report control numbers: SMC-210324-9044 and SMC-210324-9045).

7.1: How to evaluate UV protection factor

According to Fitzpatrick's skin type classification criteria, 10 physically healthy subjects aged 18 to 60 without skin diseases corresponding to skin types I, II, and III were selected as subjects. A standard sample with a high sun protection factor of Ministry of Food and Drug Safety Notice No. 2019-47 was purchased (Cosmetech Labotratories Inc., USA) and used, and the sun protection factor (SPF) of the standard sample is 15.5 ± 3.0.

An artificial solar irradiator (Multi-port Solar simulator 601-300W V2.5, Solar Light, USA) equipped with a xenon arc lamp (300 watt Xenon arc lamp), a light source that removes ultraviolet rays below 290 nm, was used as a light source. A light intensity meter (PMA-2100, Solar Light, USA) was used to measure the UV light intensity.

In this test, the sun protection factor (SPF) is an index representing the blocking effect of a product that blocks UVB, and the minimum erythema amount obtained by applying a sunscreen product is divided by the minimum amount of erythema obtained without applying a sunscreen product value, and the Minimum Erythema Dose (MED) is the minimum amount of ultraviolet radiation that can show the amount of erythema in the entire area of the irradiated area within the range of 16 to 24 hours after irradiating UVB to human skin.

The standard sample, the suspension of Comparative Example 5 (LB-C-20210128-01) and the suspension of Example 2 (LB-20210128-01) were each 2.0 mg/cm ² of each 35 cm ² area of the subject's back excluding the spine. 70.0 mg/35 cm ² of the total sample was applied and dried for 15 minutes.

After the sample application area was divided into 6 areas, ultraviolet rays were irradiated by setting the light irradiation area of each port to a minimum of 0.5 cm ² . The amount of light was adjusted by fixing the light intensity of each port and adjusting the irradiation time.

A preliminary test was conducted with the expected sun protection index of the suspension of Comparative Example 5 (LB-C-20210128-01) and the suspension of Example 2 (LB-20210128-01) set to 30. As a result of preliminary experiments with three subjects, the expected SPF index of the suspension of Comparative Example 5 (LB-C-20210128-01) was 32.8 and the expected SPF index of the suspension of Example 2 (LB-20210128-01) was It was 34.7. Therefore, the final expected index SPF of the suspension (LB-C-20210128-01) of Comparative Example 5 was 32, and the final expected index SPF of the suspension (LB-20210128-01) of Example 2 was 34, and 10 people, respectively, were applied. This test was conducted on subjects.

The minimum amount of erythema in the area where the sample was not applied was 30.0 mJ/cm ² for most Koreans as a result of a study by the Clinical Support Center for Oriental Bioindustry, Semyung University, so this was used as a standard. Since the expected SPF index of the standard sample was 15.0 for the minimum erythema amount of the area where the standard sample was applied, the amount of light was adjusted by adjusting the UV irradiation time (seconds) using this. The minimum erythema amount of the suspension of Comparative Example 5 (LB-C-20210128-01) and the suspension of Example 2 (LB-20210128-01) was also 32 and 34 respectively, so the UV irradiation time (seconds) was adjusted to calculate the amount of light.

Within the range of 16 to 24 hours after ultraviolet (UV) irradiation, the erythema status of the subjects was determined by two experienced researchers under a sufficiently bright light source. The criterion for erythema status is as follows.

1) - : No change in skin.

2) ±: Visually distinguishable erythema is visible, but erythema is not visible in all areas irradiated with ultraviolet rays.

3) + : Visually recognizable in all areas of the irradiation area irradiated with UVB

Erythema observed.

4) ++ : Clear erythema that can be recognized with the naked eye was observed in all areas of the irradiation area irradiated with UVB.

5) ++++ : Dark erythema that can be recognized with the naked eye is observed in all areas of the irradiation area irradiated with UVB, and blisters are formed.

The minimum amount of erythema in the area where the product was not applied and the amount of minimum erythema in the area where the product was applied were calculated, and the sun protection factor (SPF) was determined as the arithmetic average value for a total of 10 subjects by calculating the sun protection factor for each subject as shown in Equation 1 below. did SPF values were expressed as integers with decimal places discarded.

[Equation 1]

Sun protection index of each subject = Minimum amount of erythema in the area where the product was applied χ Minimum amount of erythema in the area where the product was not applied

7.2: UV protection index evaluation results

In accordance with the Ministry of Food and Drug Safety Notice No. 2019-47 on Functional Cosmetics Review [Appendix 3] UV protection effect measurement method and standards, 10 subjects with skin types I, II, and III were tested for human body application. As a result of the test, the SPF of the standard sample was within the range of 15.5 ± 3.0: <12.5 ~ 18.5> suggested by the notification, and the reliability verification also met the criteria.

In the reliability verification of the SPF of the suspension of Comparative Example 5 (LB-C-20210128-01) and the suspension of Example 2 (LB-20210128-01), the SPF of the sample met the reliability described in the notice. As shown in Tables 3 and 4 below, the sunscreen index of the suspension (sunscreen LB-C-20210128-01) of Comparative Example 5 confirmed through this test was 35.3 ± 2.6 (see Table 4), Example The sunscreen index of the suspension of 2 (sunscreen LB-20210128-01) was 35.2 ± 2.5 (see Table 5).

From the above results, both the sunscreen composition containing seaweed extract and titanium dioxide according to Example 2 of the present invention and the control composition containing titanium dioxide without any dispersant of Comparative Example 5 had a high sun protection factor of 30 or more. expression could be confirmed. More specifically, as shown in Table 5, the sunscreen composition of the present invention exhibited a sunscreen index ranging from 31.0 to 37.0 and an average sunscreen index of 35.2 ± 2.5.

Example 8: Skin color change evaluation - whitening evaluation

In order to evaluate the skin color change before and after application of the sunscreen composition containing seaweed extract and titanium dioxide according to Example 2 of the present invention to confirm the whitening phenomenon that the skin becomes white when applied to the skin, Semyung University Oriental Medicine Bio Industry A human application test on the skin color improvement effect was requested to the clinical support center. In this evaluation, the basic test data obtained according to the standard operating guidelines of the Clinical Support Center for the Oriental Bioindustry of Semyung University were accurately reflected (research control number: JI-1113-A; report control number: SMC-210219-4207).

8.1: How to evaluate changes in skin color

Twenty-one healthy adult women between the ages of 30 and 55 without skin disease were selected as subjects. The subject's facial area was kept clean and dry.

The image was taken using a facial camera (VISIA-CR, Canfield, USA) equipped with a camera (Canon, EOS5D Mark II, JAPAN), and standard 2 mode and UV-NF mode were used. The face camera (VISIA-CR, Canfield) fixes the forehead and chin to minimize the movement of the subject, and a gray card is also recorded so that the change in light can be seen during shooting. The measurement was conducted before and after using the product, and the overlay function was used to capture the same area, and the image was obtained.

For skin color, L-value was measured using a color difference meter (Spectrophotometer CM-2600D, Minolta, JAPAN) from the image obtained above, and the measured value was measured in a dimensionless unit (Arbitrary Unit: A.U.). The measurement was conducted before and after using the product, and each subject's measurement site was measured three times and the average value was used. The measurement variable L-value (Brightness) means that the larger the measurement value, the brighter the skin color.

Before using the product, the subject's skin condition was checked and instrumental evaluation (VISIA-CR, Spectrophotometer) was performed. After using the product, skin irritation evaluation and instrument evaluation (VISIA-CR, Spectrophotometer) were performed in parallel to evaluate the effect. Skin irritation evaluation was described later.

8.2: Skin color change evaluation results

The amount of change in skin color was calculated by subtracting the skin color measurement result before product use from the skin color measurement result after product use. Statistics were considered statistically significant when p < 0.05 by an independent test, and SPSS 18.0 software was used for statistical analysis.

The results of measuring skin color using a color difference meter are shown in Table 6 and FIG. 6 below.

As shown in Table 6 and FIG. 6, both compositions (two sunscreens) tended to increase the L ^* average value after use compared to before use. In particular, after use, the L ^* average value of 60.73 of the suspension of Comparative Example 5 (Sunscreen LB-C-20210128-01) was significantly higher than the L ^* average value of 59.64 of the suspension of Example 2 (Sunscreen LB-20210128-01) was confirmed ( p = 0.003). This means that the use of the suspension of Comparative Example 5 brightens the skin color compared to the suspension of Example 2, that is, when the suspension of Example 2 is applied to the skin, the whitening phenomenon of the skin is significantly different from that of the suspension of Comparative Example 5. means suppressed or reduced.

This is consistent with the results of Examples 3 and 4, in which titanium dioxide nanoparticles were well dispersed without aggregation, and Example 5, which confirmed excellent spreadability when seaweed extract was used as a dispersing agent.

From the above results, the present inventors confirmed that, compared to the suspension of Comparative Example 5, when the sunscreen composition containing the seaweed extract and titanium dioxide according to Example 2 was applied to the skin, the whitening phenomenon of the skin was suppressed or reduced.

8.3: Skin irritation evaluation method and results

Subjects were asked to report the following adverse skin reactions immediately after using the product. Skin irritation evaluation was performed on the test product for adverse reactions such as Erythema, Edema, Scaling, Itching, Stinging, Burning, Tightness, and Prickling. ) or other adverse reactions were closely observed, and when adverse skin reactions occurred, the following grades were marked according to the severity and test findings were written.

0: none (no adverse reaction)

1: mild

2: severe

3: very severe

As a result of skin irritation evaluation, no adverse skin reactions were observed for all test products in the subjects. In the visual evaluation by the researcher, no adverse skin reactions were also observed. From the above results, it was confirmed that the composition for sunscreen containing wakame extract (Example 2) according to the present invention did not cause any abnormal reaction when applied to the skin.

From the results of Examples 6 to 8, the seaweed extract-containing sunscreen composition prepared according to the present invention has skin safety when applied to the human body, exhibits a high sun protection index of 30 or more, and whites the skin when applied to the skin. It was confirmed that the phenomenon was significantly reduced. The control composition without seaweed extract also had skin safety suitable for human application and showed a sun protection factor of 30 or more, but when applied to the skin, the skin color was significantly higher than that of the composition of the present invention, and it was confirmed that white cast occurred. .

Therefore, the sunscreen composition containing the inorganic blocking component excellently dispersed by the wakame extract of the present invention has been verified for skin safety and functional sunscreen performance, has excellent spreadability and no cloudiness, and is not only harmful to the human body and the environment. It is harmless and suitable for both beauty and protection of the skin and environment, so it can be usefully used not only for sunscreens but also for cosmetic compositions that require sunscreen.

Claims (23)

A sunscreen composition comprising seaweed extract and an inorganic sunscreen agent.
According to claim 1,
The inorganic sunscreen is a composition for sunscreen that is dispersed by the seaweed extract.
According to claim 2,
The seaweed extract is a sunscreen composition, characterized in that to form a layer by coating the inorganic sunscreen nanoparticles.
According to claim 2,
The inorganic sunscreen nanoparticles dispersed by the wakame extract have a particle diameter of 10 nm to 120 nm, a sunscreen composition.
According to claim 1,
The seaweed extract is a sunscreen composition that is a re-dissolution of seaweed extract powder in which water and seaweed extract powder are mixed.
According to claim 5,
The seaweed extract powder is contained in 0.5 parts by weight to 3.5 parts by weight based on 100 parts by weight of the sum of the water and inorganic sunscreen powder.
According to claim 5,
The inorganic sunscreen powder is included in 20 wt% to 60 wt% based on 100 wt% of the sum of the water and the inorganic sunscreen powder.
According to claim 1,
The seaweed extract is a composition for blocking ultraviolet rays that contains polysaccharide (polysaccharide).
According to claim 8,
The polysaccharide is a sunscreen composition comprising at least one polysaccharide selected from the group consisting of alginate, carrageenan, fucoidan, laminarin, and agar. .
According to claim 1,
The inorganic sunscreen is zinc oxide (ZnO), titanium dioxide (TiO ₂ ), or a mixture thereof, a sunscreen composition.
According to claim 1,
The composition has an acidity of pH 5.0 to pH 6.0, a composition for sunscreen.
According to claim 1,
The composition has a sun protection factor (SPF) of 30 to 40, a sunscreen composition.
According to claim 1,
When the composition is applied to the skin, whitening is suppressed, a composition for sunscreen.
A method for preparing the sunscreen composition according to any one of claims 1 to 13, comprising the following steps:
i) Seaweed extract powder is mixed with water so that the seaweed extract powder is 0.5 parts by weight to 3.5 parts by weight based on 100 parts by weight of the sum of water and inorganic sunscreen powder, and seaweed extract powder is re-dissolved. Obtaining; and
ii) The inorganic sunscreen powder is added to the wakame extract, which is a re-dissolved seaweed extract powder, so that the inorganic sunscreen powder is 20 wt% to 60 wt% based on 100 wt% of the sum of the water and the inorganic sunscreen powder step of adding.
According to claim 14,
The inorganic sunscreen agent is zinc oxide (ZnO), titanium dioxide (TiO ₂ ), or a mixture thereof, the manufacturing method.
According to claim 14,
A manufacturing method further comprising the step of stirring at room temperature after step i).
According to claim 14,
Further comprising the step of ultrasonicating (ultrasonication) after the step ii), the manufacturing method.
According to claim 17,
The step of ultrasonication (ultrasonication) is carried out for 5 minutes to 1 hour at 20 kHz, the manufacturing method.
According to claim 14,
The preparation method, wherein the seaweed extract powder is obtained by a method comprising the following steps:
a) drying and pulverizing seaweed to obtain dried seaweed powder;
b) mixing the dried seaweed powder and distilled water at a weight ratio of 1:10 to 1:30 and then ultrasonicating;
c) heating the sonication product at 40° C. to 60° C.;
d) obtaining a filtrate by centrifuging the product of the water bath and filtering the solid content; and
e) mixing the filtrate with ethanol to obtain a precipitate.
According to claim 19,
The seaweed of step a) is an algae belonging to the kelp tree ( Laminariales ), seaweed family ( Alariaceae ), a manufacturing method.
According to claim 19,
Further comprising the step of storing the filtrate obtained in step d) at 4° C. after step d) and before step e).
According to claim 19,
Wherein the precipitate of step e) contains polysaccharide.
The method of claim 22,
The polysaccharide comprises at least one polysaccharide selected from the group consisting of alginate, carrageenan, fucoidan, laminarin and agar.

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