CN115887245A - Calcium alginate coated tea polyphenol modified nano particle, sunscreen composition and preparation method thereof - Google Patents
Calcium alginate coated tea polyphenol modified nano particle, sunscreen composition and preparation method thereof Download PDFInfo
- Publication number
- CN115887245A CN115887245A CN202211304543.3A CN202211304543A CN115887245A CN 115887245 A CN115887245 A CN 115887245A CN 202211304543 A CN202211304543 A CN 202211304543A CN 115887245 A CN115887245 A CN 115887245A
- Authority
- CN
- China
- Prior art keywords
- tea polyphenol
- percent
- calcium alginate
- coated
- polyphenol modified
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
Abstract
The invention discloses a calcium alginate coated tea polyphenol modified nano particle, a sun-screening agent composition and a preparation method thereof, wherein tea polyphenol modified nano titanium dioxide/zinc oxide particles are adopted, and sodium alginate and calcium chloride are coated, so that free radicals on the surface of the nano particle are eliminated, and the light stability of a product is improved; overcomes the defects that the nano particles are difficult to disperse and easy to aggregate in the using process. The tea polyphenol, sodium alginate and the like are used, the sources are rich, the price is low, the safety and the non-toxicity are realized, the preparation process is carried out at normal temperature and normal pressure, the process is simple, and the production efficiency is high. The nano particle/tea polyphenol/calcium alginate composite nano particle prepared by the invention has good dispersibility and good compatibility with other components in a sun-screening agent, and can obviously improve the ultraviolet resistance of a product in a sun-screening product.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to tea polyphenol modified nanoparticles coated with calcium alginate, a sunscreen composition and a preparation method of the sunscreen composition.
Background
Since ultraviolet rays are a main factor causing skin aging and formation of spots on the skin surface, prevention of the generation of pigments is a prerequisite for constantly maintaining skin moisture. Due to different requirements of consumers, the dosage forms of sunscreen products include cream, lotion, foundation cream, stick and the like, and can be roughly divided into organic sunscreen agents and inorganic sunscreen agents according to the action mechanism of ultraviolet sunscreen agents. The organic sunscreen agent mainly absorbs ultraviolet rays through a specific chemical structure, and converts the absorbed energy into harmless heat energy and the like to be released, so that the aim of resisting the ultraviolet rays is fulfilled. However, organic sunscreens are highly irritating, have poor photostability, are easily decomposed, and cause side effects such as skin allergy and inflammation.
The mechanisms of action of inorganic sunscreens include mainly absorption, scattering and reflection. TiO 2 2 And ZnO is currently the most predominant inorganic sunscreen agent on the market; but to solve TiO 2 The problem of easy agglomeration is often required for TiO 2 The modification can solve the problem of nano TiO to a certain extent 2 The sunscreen agent is easy to agglomerate, but modified raw materials have certain toxicity, or toxic substances are required to be used in the modification process, so that the cost is increased to a certain extent, and the residual toxic substances have harm to the skin of a human body.
The sunscreen cream added with the nano zinc oxide can improve the SPF value, the nano zinc oxide has good effect in the filtering operation of ultraviolet UVA and ultraviolet UVB, and is a broad-spectrum sunscreen agent with excellent performance, and the effects of shielding ultraviolet radiation, sterilizing, preventing mildew, resisting aging and the like can be realized. Therefore, the use value and the acceptable degree of the zinc oxide material in the field of cosmetic sun protection can be greatly improved after the zinc oxide is in the nano level. However, in the process of manufacturing cosmetics, the separation strength of nano zinc oxide is weak, the particle size is difficult to disperse to its original size, and its transparency and ultraviolet ray shielding ability are not sufficiently exhibited.
Therefore, in order to solve the above problems, it is urgent to provide materials with biological environmental protection and low toxicity to modify particles of titanium dioxide, zinc oxide, etc., to promote the dispersibility thereof in sunscreen lotion and cosmetics, to solve the problem of easy agglomeration of nanoparticles, etc., and to improve the sunscreen performance.
Disclosure of Invention
In order to overcome the defects of the prior art, the first object of the invention is to provide a preparation method of tea polyphenol modified nanoparticles coated with calcium alginate, wherein tea polyphenol modified zinc oxide or titanium dioxide nanoparticles are used, and sodium alginate and calcium chloride are used for coating the nanoparticles to obtain nanoparticle/calcium alginate microcapsules, so that the problems of nonuniform dispersion and easy agglomeration of zinc oxide and titanium dioxide in a sun-screening agent are solved, and the sun-screening performance is improved; and the used raw materials are all pure natural macromolecular compounds, so the composition is nontoxic and harmless to human bodies.
The second purpose of the invention is to provide a tea polyphenol modified nano particle coated with calcium alginate.
It is a third object of the present invention to provide a sunscreen composition.
The fourth purpose of the invention is to provide a preparation method of the sunscreen composition.
One of the purposes of the invention can be achieved by adopting the following technical scheme:
a preparation method of calcium alginate-coated tea polyphenol modified nanoparticles comprises the following steps:
s11, dispersing the nanoparticles in a tea polyphenol water solution with the mass concentration of 5-10%, and uniformly dispersing to obtain a mixed dispersion liquid; wherein the nano particles are one or a mixture of two of zinc oxide and titanium dioxide;
s12, adding sodium alginate into distilled water, and uniformly dispersing to obtain a sodium alginate solution with the mass concentration of 1% -5%;
and S13, placing the mixed dispersion liquid of the S11 into a sodium alginate solution of the S12, fully mixing to obtain a mixed liquid, dripping the mixed liquid into a calcium chloride solution by using an injector, standing for 0.5-2h, carrying out suction filtration, washing a filter cake with water, and drying in vacuum to obtain the tea polyphenol modified nanoparticles coated with calcium alginate.
Further, the zinc oxide and the titanium dioxide in the S11 are nano zinc oxide and nano titanium dioxide with the particle size of 10-80 nm.
Further, S11 and S12 are dispersed by stirring at 40-50 ℃ and 150-300rpm for 10-60 min; the volume ratio of the S11 mixed dispersion liquid to the S12 sodium alginate solution in the S13 mixed solution is (2-3): 1.
further, the mass fraction of the calcium chloride solution in the S13 is 0.5-4%.
The second purpose of the invention can be achieved by adopting the following technical scheme:
the calcium alginate-coated tea polyphenol modified nanoparticles are prepared by any one of the preparation methods of the calcium alginate-coated tea polyphenol modified nanoparticles.
The third purpose of the invention can be achieved by adopting the following technical scheme:
the sunscreen composition comprises the following components in percentage by mass: 2 to 4% of stearic acid, 3 to 5% of A component, 4 to 6% of phytosterol, 2 to 4% of octadecanol, 2 to 4% of glyceryl stearate, 0.8 to 1.2% of polydimethylsiloxane, 1 to 3% of xanthan gum, 1 to 3% of preservative, 3 to 6% of calcium alginate-coated tea polyphenol-modified nanoparticles, 0.8 to 1.2% of pH regulator, 1 to 3% of humectant, 0.3 to 0.6% of EDTA disodium, and the balance of water; the component A is one or a composition of more than two of diethylhexyl butamido triazone, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine or diethylamino hydroxybenzoyl hexyl benzoate.
Further, the pH regulator is one or a composition of more than two of triethanolamine, sodium hydroxide, potassium hydroxide, arginine, aminomethyl propanol or tetrahydroxypropyl ethylenediamine.
Further, the preservative is one or a composition of more than two of phenoxyethanol, p-hydroxyacetophenone, 1, 2-hexanediol and pentanediol.
Further, the humectant is one or a composition of more than two of glycerin, butanediol, propylene glycol and sorbitol.
The fourth purpose of the invention can be achieved by adopting the following technical scheme:
a preparation method of the sunscreen composition comprises the following steps: according to the amount of the formula,
s21, dispersing the tea polyphenol modified nanoparticles coated with calcium alginate into stearic acid, the component A, phytosterol, glyceryl stearate, polydimethylsiloxane and xanthan gum under high-speed stirring to prepare powder slurry;
s22, adding octadecanol, a preservative, a pH regulator, a humectant and EDTA disodium into water to prepare a water phase;
and S23, slowly adding the powder slurry into the water phase under a homogenizing condition, and homogenizing for 5-10min after the powder slurry is added to obtain the sun-screening agent composition.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, tea polyphenol modified nano titanium dioxide/zinc oxide particles are adopted, and sodium alginate and calcium chloride are coated, so that free radicals on the surfaces of the nano particles are eliminated, and the light stability of the product is improved; overcomes the defects that inorganic nano particles are difficult to disperse and easy to aggregate in the using process. The tea polyphenol, sodium alginate and the like are rich in sources, low in price, safe and non-toxic, the preparation process is carried out at normal temperature and normal pressure, the process is simple, and the production efficiency is high.
2. The nano particle/tea polyphenol/calcium alginate composite nano particle prepared by the invention has good dispersibility and good compatibility with other components in the sun-screening agent, and can obviously improve the ultraviolet resistance of the product in the sun-screening product.
Drawings
FIG. 1 is a TEM image of sodium alginate and tea polyphenol mixed modified nano titanium dioxide particles of comparative example 1;
FIG. 2 is a TEM image of tea polyphenol-modified titanium dioxide particles of comparative example 3;
fig. 3 is a TEM image of calcium alginate coated tea polyphenol modified nanoparticles of example 1.
Detailed Description
The technical solution of the present invention will be clearly and completely described with reference to the specific embodiments. It is to be understood that the described embodiments are merely some embodiments of the invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. The starting materials used in the examples of the present invention are all commercially available unless otherwise specified.
TiO 2 And ZnO is currently the most predominant inorganic sunscreen agent on the market; nano TiO 2 2 Has strong ultraviolet absorption ability, can transmit visible light, and can be used in cosmetic without whitening. However, nano TiO 2 There are also some problems associated with the use as sunscreens. Such as nano TiO 2 Has strong photochemical activity, can easily oxidize and decompose nutrients in cosmetic to deteriorate cosmetic, and has strong oxidation ability and high reactivity of hydroxyl radical (. OH) and other oxygen species (O) generated by surface photochemical reaction - ，O 2 - And OOH) accelerates the aging of epidermal cells, causing direct damage to the skin. Nano TiO 2 2 The particle size of the nano TiO is very small, the specific surface energy is large, the nano TiO is not easy to disperse in an organic medium and is easy to agglomerate in a polar medium, and the nano TiO is limited to a great extent 2 The application of the composition in the cosmetic industry is developed. Thus, the nano TiO is reduced or eliminated 2 The photocatalytic activity of the photocatalyst is improved, and the sunscreen performance, the dispersibility and the like of the photocatalyst have great research values. For TiO at home and abroad 2 The modification method mainly comprises organic modification and inorganic modification, such as sodium dodecyl benzene sulfonate, octadecyl trimethyl ammonium chloride, etc. for TiO 2 Modifying, or coating titanium dioxide with silicon dioxide formed by sodium silicate and ethyl orthosilicate, and modifying TiO 2 Applied to sun-screening liquid and cosmetics and solves the problem of TiO 2 Poor dispersibility and easy agglomeration, and improves the ultraviolet shielding performance and the sun-screening performance of the product.
Aiming at the problem of toxicity of the existing modified material, the invention provides a method for preparing nano particles by modifying nano zinc oxide and titanium dioxide by using natural tea polyphenol and sodium alginate as raw materials.
A preparation method of calcium alginate-coated tea polyphenol modified nanoparticles comprises the following steps:
s11, dispersing the nanoparticles in a tea polyphenol water solution with the mass concentration of 5-10%, and uniformly dispersing to obtain a mixed dispersion liquid; wherein the nano particles are one or a mixture of two of zinc oxide and titanium dioxide;
s12, adding sodium alginate into distilled water, and uniformly dispersing to obtain a sodium alginate solution with the mass concentration of 1% -5%;
and S13, placing the mixed dispersion liquid of the S11 into a sodium alginate solution of the S12, fully mixing to obtain a mixed liquid, dripping the mixed liquid into a calcium chloride solution by using an injector, standing for 0.5-2h, carrying out suction filtration, washing a filter cake with water, and drying in vacuum to obtain the tea polyphenol modified nanoparticles coated with calcium alginate.
The tea polyphenol can prevent the skin from being damaged by sunlight, and the tea polyphenol can be used together with the traditional inorganic sun-screening agents of zinc oxide and titanium dioxide to provide better sunlight protection performance in a synergistic way. The zinc oxide or titanium dioxide particles are coated by algal polysaccharide, so that the problems of poor particle dispersibility and easy aggregation can be solved while the ultraviolet absorption and scattering performance of the particles are maintained, and the defect that free radicals are generated under photochemical catalysis to damage skin cells is overcome. And the polymer such as sodium alginate reacts with calcium chloride to form calcium alginate, can coat zinc oxide or titanium oxide, and is mixed with other components of the sunscreen cosmetic together with a dispersion in an oily component of an inorganic ultraviolet screening agent (zinc oxide or titanium oxide), so that the dispersibility of the inorganic ultraviolet screening agent is improved, and the problem of agglomeration of the inorganic ultraviolet screening agent such as zinc oxide or titanium oxide is solved.
In one embodiment, the mass concentration of the nanoparticles in the mixed dispersion in step S11 is 50-200mg/mL; preferably, the mass concentration of the nanoparticles in the mixed dispersion liquid in the step S11 is 67-100mg/mL.
As one embodiment, the zinc oxide and the titanium dioxide in S11 are nano zinc oxide and nano titanium dioxide with the particle size of 10-80 nm.
The nano zinc oxide and the nano titanium dioxide have better sun-screening effect, but are easier to gather, have poor weather resistance and strong photochemical catalytic activity. But the modification method of the invention can also overcome the problems of the nano zinc oxide and the nano titanium dioxide. Preferably, the particle size of the zinc oxide is 40nm, and the particle size of the titanium dioxide is 50nm.
As one embodiment, S11 and S12 are dispersed by stirring at 40-50 deg.C and 150-300rpm for 10-60 min; the volume ratio of the S11 mixed dispersion liquid to the S12 sodium alginate solution in the S13 mixed solution is (2-3): 1. s11, zinc oxide and titanium dioxide can be fully mixed and contacted with tea polyphenol through stirring and dispersion, and catechol in the tea polyphenol has strong metal ion chelating capacity, so that the surface of the zinc oxide and the surface of the titanium dioxide can be modified by the tea polyphenol.
According to one embodiment, the mass fraction of the calcium chloride solution in S13 is 0.5-4%. Calcium chloride as a reactant reacts with sodium alginate to form calcium alginate, thereby forming a coating.
The invention provides calcium alginate-coated tea polyphenol modified nanoparticles prepared by the preparation method of the calcium alginate-coated tea polyphenol modified nanoparticles.
The calcium alginate-coated tea polyphenol modified nanoparticles are prepared by any one of the preparation methods of the calcium alginate-coated tea polyphenol modified nanoparticles.
The invention provides a sunscreen composition.
The sunscreen composition comprises the following components in percentage by mass: 2 to 4 percent of stearic acid, 3 to 5 percent of component A, 4 to 6 percent of phytosterol, 2 to 4 percent of octadecanol, 2 to 4 percent of glyceryl stearate, 0.8 to 1.2 percent of polydimethylsiloxane, 1 to 3 percent of xanthan gum, 1 to 3 percent of preservative, 3 to 6 percent of calcium alginate-coated tea polyphenol modified nano particles, 0.8 to 1.2 percent of pH regulator, 1 to 3 percent of humectant, 0.3 to 0.6 percent of EDTA disodium and the balance of water; the component A is one or a composition of more than two of diethylhexyl butamido triazone, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine or diethylamino hydroxybenzoyl hexyl benzoate.
Wherein, the 3-6% of the tea polyphenol modified nanoparticles coated by calcium alginate are the tea polyphenol modified nanoparticles coated by calcium alginate prepared by the preparation method, and the tea polyphenol modified nanoparticles have good compatibility with other components in the sun-screening agent, and can obviously improve the ultraviolet resistance of the product in the sun-screening product.
The component A is one or a composition of more than two of diethylhexyl butamido triazone, ethylhexyl triazone, bis-ethylhexyl oxyphenol methoxyphenyl triazine or diethylamino hydroxybenzoyl hexyl benzoate. Diethylhexyl butamido triazone is an oil soluble UVB absorber, which hardly penetrates into the skin; the ethylhexyl triazone has a larger molecular structure and high UVB ultraviolet absorption capacity; bis-ethylhexyloxyphenol methoxyphenyl triazine is an oily UV all-band sunscreen component; diethylaminohydroxybenzoylhexyl benzoate is an oily UVA absorber. Wherein, the ethylhexyl butamido triazone, ethylhexyl triazone, bis-ethylhexyl phenol methoxyphenyl triazine or diethylamino hydroxybenzoyl hexyl benzoate in the component A can be optionally matched for use; preferably, the component A is a composition consisting of diethyl hexyl butyryl amino triazone, ethylhexyl triazone, bis-ethylhexyl oxyphenol methoxyphenyl triazine and diethyl amino hydroxybenzoyl hexyl benzoate according to the mass ratio of 1.
In one embodiment, the pH adjuster is one or a combination of two or more of triethanolamine, sodium hydroxide, potassium hydroxide, arginine, aminomethyl propanol, and tetrahydroxypropyl ethylenediamine.
As one embodiment, the preservative is one or a composition of more than two of phenoxyethanol, p-hydroxyacetophenone, 1, 2-hexanediol and pentanediol.
In one embodiment, the humectant is one or a combination of two or more of glycerin, butylene glycol, propylene glycol, and sorbitol.
The pH regulator, the preservative and the humectant are all commonly used reagents in the field, and have good compatibility with the tea polyphenol modified nano-particles coated by the calcium alginate.
The invention provides a preparation method of a sun-screening agent composition.
A preparation method of the sunscreen composition comprises the following steps: according to the amount of the formula, the raw materials,
s21, dispersing the tea polyphenol modified nanoparticles coated with calcium alginate into stearic acid, the component A, phytosterol, glyceryl stearate, polydimethylsiloxane and xanthan gum under stirring to prepare powder slurry;
s22, adding octadecanol, a preservative, a pH regulator, a humectant and EDTA disodium into water, and uniformly stirring to prepare a water phase;
and S23, slowly adding the powder slurry into the water phase under a homogenizing condition, and homogenizing for 5-10min after the powder slurry is added to obtain the sun-screening agent composition.
As one embodiment, the stirring conditions in S21 and S22 are that the dispersion is carried out for 30-120min at the temperature of 40-50 ℃ and the stirring speed of 300-500 rpm; s23, homogenizing at 40-50 ℃ and stirring speed of 300-400rpm.
As one embodiment, S23 is homogenized, cooled to 28-31 ℃, and discharged.
Example 1
A preparation method of calcium alginate-coated tea polyphenol modified nanoparticles comprises the following steps:
dispersing 10g of nano titanium dioxide in 100ml of tea polyphenol water solution, and performing ultrasonic dispersion at 40 ℃ to obtain a mixed dispersion liquid; wherein the mass concentration of the tea polyphenol water solution is 5 percent; uniformly scattering a certain amount of sodium alginate into distilled water, and stirring for 45min at the rotating speed of 300rpm in a water bath at 50 ℃ to form a sodium alginate solution; wherein the mass concentration of the sodium alginate is 5 percent; placing 100mL of mixed dispersion liquid into 50mL of sodium alginate solution, and stirring and fully mixing to obtain mixed liquid; and then dripping the mixture into a calcium chloride solution with the mass concentration of 4% by using an injector, standing for 1h, carrying out suction filtration, washing a filter cake with water, and carrying out vacuum drying to obtain the tea polyphenol modified nanoparticles coated with calcium alginate.
Example 2
A preparation method of particles for a sun-screening agent specifically comprises the following steps:
a preparation method of calcium alginate-coated tea polyphenol modified nanoparticles comprises the following steps:
dispersing 10g of nano zinc oxide in 100ml of tea polyphenol water solution, and performing ultrasonic dispersion at 50 ℃ to obtain a mixed dispersion liquid; wherein the mass concentration of the tea polyphenol water solution is 5 percent; uniformly scattering a certain amount of sodium alginate into distilled water, and stirring for 45min at the rotating speed of 300rpm in a water bath at 50 ℃ to form a sodium alginate solution; wherein the mass concentration of the sodium alginate is 1 percent; placing 100mL of mixed dispersion liquid into 50mL of sodium alginate solution, and stirring and fully mixing to obtain mixed liquid; and then dripping the mixture into a calcium chloride solution with the mass concentration of 0.5% by using an injector, standing for 1h, carrying out suction filtration, washing a filter cake with water, and carrying out vacuum drying to obtain the tea polyphenol modified nanoparticles coated with calcium alginate.
Example 3
A preparation method of tea polyphenol modified nanoparticles coated with calcium alginate comprises the following steps:
dispersing 5g of nano titanium dioxide and 5g of nano zinc oxide in 100ml of tea polyphenol water solution, and performing ultrasonic dispersion at 40 ℃ to obtain a mixed dispersion liquid; wherein the mass concentration of the tea polyphenol water solution is 5 percent; uniformly scattering a certain amount of sodium alginate into distilled water, and stirring for 45min at the rotating speed of 300rpm in a water bath at 50 ℃ to form a sodium alginate solution; wherein the mass concentration of the sodium alginate is 3 percent; placing 100mL of mixed dispersion liquid into 50mL of sodium alginate solution, and stirring and fully mixing to obtain mixed liquid; and then dripping the mixture into a calcium chloride solution with the mass concentration of 2% by using an injector, standing for 1h, carrying out suction filtration, washing a filter cake with water, and carrying out vacuum drying to obtain the tea polyphenol modified nanoparticles coated with calcium alginate.
Example 4
A preparation method of calcium alginate-coated tea polyphenol modified nanoparticles comprises the following steps:
dispersing 15g of nano titanium dioxide in 200ml of tea polyphenol water solution, and performing ultrasonic dispersion at 40 ℃ to obtain a mixed dispersion liquid; wherein the mass concentration of the tea polyphenol water solution is 10 percent; uniformly scattering a certain amount of sodium alginate into distilled water, and stirring for 50min at the rotating speed of 300rpm in a water bath at 60 ℃ to form a sodium alginate solution; wherein the mass concentration of the sodium alginate is 5 percent; placing 150mL of mixed dispersion liquid into 50mL of sodium alginate solution, and stirring and fully mixing to obtain mixed liquid; and then dripping the mixture into a calcium chloride solution with the mass concentration of 4% by using an injector, standing for 1h, carrying out suction filtration, washing a filter cake with water, and carrying out vacuum drying to obtain the calcium alginate-coated tea polyphenol modified nanoparticles.
Example 5
A preparation method of tea polyphenol modified nanoparticles coated with calcium alginate comprises the following steps:
dispersing 15g of nano zinc oxide in 150ml of tea polyphenol water solution, and performing ultrasonic dispersion at 50 ℃ to obtain a mixed dispersion liquid; wherein the mass concentration of the tea polyphenol water solution is 10 percent; uniformly scattering a certain amount of sodium alginate into distilled water, and stirring for 45min at the rotating speed of 300rpm in a water bath at 50 ℃ to form a sodium alginate solution; wherein the mass concentration of the sodium alginate is 1 percent; placing 125mL of mixed dispersion liquid into 50mL of sodium alginate solution, and stirring and fully mixing to obtain mixed liquid; and then dripping the mixture into a calcium chloride solution with the mass concentration of 2% by using an injector, standing for 1h, carrying out suction filtration, washing a filter cake with water, and carrying out vacuum drying to obtain the tea polyphenol modified nanoparticles coated with calcium alginate.
Example 6
A preparation method of tea polyphenol modified nanoparticles coated with calcium alginate comprises the following steps:
dispersing 3g of nano titanium dioxide and 7g of nano zinc oxide in 150ml of tea polyphenol water solution, and performing ultrasonic dispersion at 40 ℃ to obtain a mixed dispersion liquid; wherein the mass concentration of the tea polyphenol water solution is 7.5 percent; uniformly scattering a certain amount of sodium alginate into distilled water, and stirring for 45min at the rotating speed of 300rpm in a water bath at 50 ℃ to form a sodium alginate solution; wherein the mass concentration of the sodium alginate is 3 percent; putting 100mL of mixed dispersion liquid into 50mL of sodium alginate solution, and stirring and fully mixing to obtain mixed liquid; and then dripping the mixture into a calcium chloride solution with the mass concentration of 2% by using an injector, standing for 1h, carrying out suction filtration, washing a filter cake with water, and carrying out vacuum drying to obtain the tea polyphenol modified nanoparticles coated with calcium alginate.
Comparative example 1
A method for preparing particles for a sunscreen agent:
dispersing 10g of nano titanium dioxide in 100ml of tea polyphenol water solution, and performing ultrasonic dispersion at 50 ℃ to obtain a mixed dispersion liquid; wherein the mass concentration of the tea polyphenol water solution is 5 percent; uniformly scattering a certain amount of sodium alginate into distilled water, and stirring for 45min at the rotating speed of 300rpm in a water bath at 50 ℃ to form a sodium alginate solution; wherein the mass concentration of the sodium alginate is 1 percent; placing 100mL of mixed dispersion liquid into 50mL of sodium alginate solution, and stirring and fully mixing to obtain mixed liquid; standing for 1h, carrying out suction filtration, washing a filter cake with water, and drying in vacuum to obtain the sodium alginate and tea polyphenol mixed modified nano titanium dioxide particles.
Comparative example 2
A method for producing sunscreen particles using 100ml of distilled water in place of the aqueous solution of tea polyphenol was the same as in example 1.
Comparative example 3
A process for the preparation of particles for use in sunscreens,
dispersing 10g of nano titanium dioxide in 100ml of tea polyphenol water solution, and performing ultrasonic dispersion at 40 ℃ to obtain a mixed dispersion liquid; wherein the mass concentration of the tea polyphenol water solution is 5 percent; standing for 1h, taking out the solid particles, performing suction filtration, washing with water, and performing vacuum drying to obtain tea polyphenol modified titanium dioxide particles.
Test example:
use of nanoparticles prepared according to examples 1 to 6 and comparative examples 1 to 3 in sunscreen compositions, wherein the composition and content of the sunscreen compositions described in experimental examples A1 to a13, comparative experimental examples C1 to C4 are as given in table 1:
in table 1:
(1) The total parts of examples A1 to A13 and comparative examples C1 to C4 are 100 parts;
(2) Examples A1-A4 and comparative examples C1-C4 used triethanolamine as the pH adjusting agent; the pH regulators used in Experimental examples A5-A13 were a combination of sodium hydroxide and triethanolamine, the mass ratio of sodium hydroxide to triethanolamine was 1;
(3) The preservative used in examples A1-A3 and comparative examples C1-C4 was phenoxyethanol; examples A4-A8 the preservative used was p-hydroxyacetophenone; examples A9-A11 used 1, 2-hexanediol as a preservative; experimental examples A12-A13 the preservative used was pentanediol.
(4) The humectants used in examples A1-A3 and comparative examples C1-C4 were glycerin; examples A4-A6 the humectant used was butylene glycol; A7-A10 the humectant used is propylene glycol; the humectant used in A11-A13 is sorbitol;
(5) Experimental examples A1-A3 used the nanoparticles prepared in example 1; A4-A5 used the nanoparticles prepared in example 2; A6-A7 used the nanoparticles prepared in example 3; A8-A9 used the nanoparticles prepared in example 4; a10 to A11 used were the nanoparticles prepared in example 5; a12 to A13 used were the nanoparticles prepared in example 6; comparative Experimental examples C1 to C3 used the nanoparticles prepared in comparative examples 1 to 3, respectively; c4, unmodified titanium dioxide is used;
(6) In examples A1 to a13 and in comparative examples C1 to C4, the component a was a composition consisting of diethylhexylbutamido triazone, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, and diethylamino oxybenzoyl hexyl benzoate in a mass ratio of 1.
TABLE 1 composition and content Table of sunscreen compositions
And (3) performance testing:
the stability of the sunscreen agent is determined by referring to GB/T29665-2013 skin care lotion and QB/T1857-2013 (skin care cream), and the specific method and test result are as follows:
1. stability test
1) The sunscreen composition was filled in a 50mL transparent sample bottle, placed in a refrigerator at-4 ℃ for 24 hours, taken out and placed at room temperature of 25 ℃ for 24 hours, and then placed in an oven at 40 ℃ for 24 hours, and the cycle was continued for 50 times, and the presence or absence of delamination was observed.
2) And (4) centrifugal test, namely adding the sunscreen composition into a centrifugal tube, centrifuging for 30min at 3500r/min, and observing whether the sunscreen composition is layered or not.
The stability and centrifugation test results for the sunscreen compositions described in examples A1-A13, comparative examples C1-C4 are shown in Table 2:
table 2 stability test results for sunscreen compositions
As can be seen from the stability test and the centrifugal test results in table 2, the sunscreens A1-a13 prepared from the calcium alginate-coated tea polyphenol modified nanoparticles described in the present application are not delaminated in both the centrifugal test and the stability test; whereas comparative examples C1-C4 all showed slight or stratified appearance.
2. TEM analysis
A small amount of the granules prepared in example 1, comparative example 1 and comparative example 3 was taken. Adding equal amount of absolute ethyl alcohol, performing ultrasonic treatment for 30min, uniformly dispersing the sample, dripping 1-2 drops of the treated solution onto a copper net by using a rubber head dropper, airing, and performing TEM characterization, wherein a TEM image is shown in figures 1-3. Wherein FIG. 1 is a TEM image of comparative example 1, FIG. 2 is a TEM image of comparative example 3, and FIG. 3 is a TEM image of example 1.
As can be seen from the TEM image, the agglomeration is serious in comparative example 1 modified with tea polyphenol and sodium alginate and comparative example 3 modified with tea polyphenol; in example 1, the tea polyphenol modified nanoparticles coated with calcium alginate are used for preparation, the particles are dispersed uniformly, and no obvious agglomeration phenomenon occurs, which is mainly because the hydrophobic property of the nanoparticles is improved after the tea polyphenol modified nanoparticles are coated with calcium alginate, and the dispersion of the nanoparticles is facilitated.
3. Sunscreen index analysis of sunscreens
And (3) measuring parameters such as SPF (specific pathogen free) values, PA (Power factor) values, sun simulation irradiation intensity, critical wavelength and the like of the two groups of sunscreen creams by adopting a UV-2000S type sunscreen performance analyzer. The prepared emulsion 32mg is precisely weighed according to the selected Collpa standard and evenly distributed on a clean PMMA plate, a pre-soaked latex finger cot is used for quickly and evenly coating the whole PMMA plate with the sample, the PMMA plate is placed in a dark room temperature environment and stands for 20min, then the in-vitro sun protection index of the PMMA plate is tested, and then the PMMA plate is placed in an Atlas illumination box for illumination for 30min, and the PA value of the PMMA plate is measured.
The mass fractions of the active substances in the slurry are the same and 10%. The SPF and PA values tested are shown in table 3:
TABLE 3 Sun protection factor SPF-value, PA-value of the sunscreen
As can be seen from Table 3, the SPF values of the experimental examples A1-A13 can reach more than 20, and the PA values can reach more than 7 under the condition that the mass fractions of the active substances of the slurry are the same; is obviously higher than the SPF value and the PA value of the control experiments C1-C4. The main reason is that the tea polyphenol modified nanoparticles coated by calcium alginate are dispersed more uniformly in the sunscreen composition without agglomeration, and the ultraviolet shielding capability of the nanoparticles is exerted to the maximum extent.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. A preparation method of tea polyphenol modified nanoparticles coated with calcium alginate is characterized by comprising the following steps:
s11, dispersing the nanoparticles in a tea polyphenol water solution with the mass concentration of 5-10%, and uniformly dispersing to obtain a mixed dispersion liquid; wherein the nano particles are one or a mixture of two of zinc oxide and titanium dioxide;
s12, adding sodium alginate into distilled water, and uniformly dispersing to obtain a sodium alginate solution with the mass concentration of 1% -5%;
and S13, placing the mixed dispersion liquid of the S11 into a sodium alginate solution of the S12, fully mixing to obtain a mixed liquid, dripping the mixed liquid into a calcium chloride solution by using an injector, standing for 0.5-2h, carrying out suction filtration, washing a filter cake with water, and drying in vacuum to obtain the tea polyphenol modified nanoparticles coated with calcium alginate.
2. The method for preparing tea polyphenol modified nanoparticles coated with calcium alginate as claimed in claim 1, wherein the zinc oxide and titanium dioxide in S11 are nano zinc oxide and nano titanium dioxide with particle size of 10-80 nm.
3. The method for preparing calcium alginate-coated tea polyphenol modified nanoparticles as claimed in claim 1 or 2,
s11 and S12 are dispersed by stirring for 10-60min at 40-50 ℃ and 150-300 rpm; the volume ratio of the S11 mixed dispersion liquid to the S12 sodium alginate solution in the S13 mixed solution is (2-3): 1.
4. the method for preparing calcium alginate-coated tea polyphenol modified nanoparticles as claimed in claim 1, wherein the mass fraction of the calcium chloride solution in S13 is 0.5-4%.
5. A calcium alginate-coated tea polyphenol modified nanoparticle, which is characterized in that the calcium alginate-coated tea polyphenol modified nanoparticle is prepared by the preparation method of the calcium alginate-coated tea polyphenol modified nanoparticle of any one of claims 1 to 4.
6. The sunscreen composition is characterized by comprising the following components in percentage by mass: 2 to 4 percent of stearic acid, 3 to 5 percent of component A, 4 to 6 percent of phytosterol, 2 to 4 percent of octadecanol, 2 to 4 percent of glyceryl stearate, 0.8 to 1.2 percent of polydimethylsiloxane, 1 to 3 percent of xanthan gum, 1 to 3 percent of preservative, 3 to 6 percent of calcium alginate-coated tea polyphenol modified nano particles, 0.8 to 1.2 percent of pH regulator, 1 to 3 percent of humectant, 0.3 to 0.6 percent of EDTA disodium and the balance of water; the component A is one or a composition of more than two of diethyl hexyl butyryl amino triazone, ethyl hexyl triazone, bis-ethyl hexyl oxyphenol methoxyphenyl triazine or diethyl amino hydroxyl benzoyl benzoic acid hexyl ester.
7. The sunscreen composition according to claim 6, wherein the pH regulator is one or more of triethanolamine, sodium hydroxide, potassium hydroxide, arginine, aminomethyl propanol, and tetrahydroxypropyl ethylenediamine.
8. The sunscreen composition according to claim 6, wherein the preservative is one or a combination of more than two of phenoxyethanol, p-hydroxyacetophenone, 1, 2-hexanediol and pentanediol.
9. The sunscreen composition according to claim 6, wherein the humectant is one or more of glycerin, butylene glycol, propylene glycol, and sorbitol.
10. A process for the preparation of a sunscreen composition according to any of claims 6 to 9 comprising the steps of: according to the amount of the formula,
s21, dispersing the tea polyphenol modified nanoparticles coated with calcium alginate into stearic acid, the component A, phytosterol, glyceryl stearate, polydimethylsiloxane and xanthan gum under high-speed stirring to prepare powder slurry;
s22, adding octadecanol, a preservative, a pH regulator, a humectant and EDTA disodium into water to prepare a water phase;
and S23, slowly adding the powder slurry into the water phase under a homogenizing condition, and homogenizing for 5-10min after the powder slurry is added to obtain the sun-screening agent composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211304543.3A CN115887245A (en) | 2022-10-24 | 2022-10-24 | Calcium alginate coated tea polyphenol modified nano particle, sunscreen composition and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211304543.3A CN115887245A (en) | 2022-10-24 | 2022-10-24 | Calcium alginate coated tea polyphenol modified nano particle, sunscreen composition and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115887245A true CN115887245A (en) | 2023-04-04 |
Family
ID=86483311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211304543.3A Pending CN115887245A (en) | 2022-10-24 | 2022-10-24 | Calcium alginate coated tea polyphenol modified nano particle, sunscreen composition and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115887245A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115252442A (en) * | 2022-07-21 | 2022-11-01 | 武汉纺织大学 | Preparation method of plant microsphere sunscreen composition embedded with titanium dioxide and sunscreen agent |
-
2022
- 2022-10-24 CN CN202211304543.3A patent/CN115887245A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115252442A (en) * | 2022-07-21 | 2022-11-01 | 武汉纺织大学 | Preparation method of plant microsphere sunscreen composition embedded with titanium dioxide and sunscreen agent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1231543C (en) | Particulate metal oxide | |
| CN107582422B (en) | A kind of titanium dioxide/algal polysaccharides composite nanometer particle and its preparation method and application | |
| WO2001093812A1 (en) | Cosmetic preparation | |
| CN115887245A (en) | Calcium alginate coated tea polyphenol modified nano particle, sunscreen composition and preparation method thereof | |
| CN113440423B (en) | Modified titanium dioxide particle, preparation method thereof and skin care product | |
| CN113332170A (en) | Preparation method of lignin/titanium dioxide nanoparticle sun-screening agent | |
| WO2021174715A1 (en) | Personal care sunscreen composition, preparation method therefor and use thereof | |
| KR101210371B1 (en) | Manufacturing method of emulsion containing titanium dioxide and zinc oxide and cosmetic composition for protecting containing thereof | |
| CN103230355A (en) | Sunscreen cream cosmetic composition containing nano crystal cellulose | |
| CN116211722A (en) | Sun-screening raw material, preparation method thereof and cosmetics | |
| CN106176354A (en) | A kind of moisture retention water containing astaxanthin and preparation method thereof | |
| CN104800093A (en) | Sunscreen composition containing layered composite metal hydroxide and preparation method thereof | |
| Lyu et al. | Nanoparticles in sunscreen: exploration of the effect and harm of titanium oxide and zinc oxide | |
| WO2013161553A1 (en) | Surface modified inorganic oxide fine particles, and sunscreen cosmetic material containing same | |
| CN114344234A (en) | Skin-beautifying emulsion-isolating pearl shell sun cream and preparation method thereof | |
| CN108272647B (en) | Whitening and moisturizing cosmetic based on hydroxyl free radicals and preparation process thereof | |
| KR101322869B1 (en) | A complexed powder coated with Octyl methoxy cinnamate and anti-UV cosmetic composition using the same | |
| JP2000264823A (en) | Ultraviolet light-resistant composition and container therefor | |
| CN105560086A (en) | Pure natural multiple-effect nourishing sunscreen cream containing peony seed oil and preparation method thereof | |
| CN101381529B (en) | Anti-ultraviolet radiation nano cerium-tin oxidate aqueous slurry and preparation method thereof | |
| JP3530052B2 (en) | Surface-treated powder having a surface coated with a transparent oily film containing titanium oxide and a method for producing the same, and a skin composition, a paint composition, a resin composition, and a container containing the same | |
| KR102386598B1 (en) | An ultraviolet screening dispersion comprising alkane-based oil as a dispersion medium and a cosmetic composition containing the same | |
| JP7188447B2 (en) | Electromagnetic wave absorber, sunscreen, optical component, glasses, and method for producing electromagnetic wave absorber | |
| TW201125960A (en) | Clay mineral with intercalated UV absorber and cosmetic containing the same | |
| Li et al. | Fabrication of CeO2/CaO nanocomposite as ultraviolet screening agent and its application in sunscreen |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication |