CN112402291A - Composite wall material particle coated with fat-soluble sunscreen agent, preparation method and application - Google Patents
Composite wall material particle coated with fat-soluble sunscreen agent, preparation method and application Download PDFInfo
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/65—Characterized by the composition of the particulate/core
- A61K2800/652—The particulate/core comprising organic material
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Abstract
The invention discloses a composite wall material particle coated with a fat-soluble sun-screening agent, a preparation method and application thereof in a sun-screening cosmetic. The raw materials comprise alcohol soluble protein, cellulose, fat-soluble sun-screening agent, solubilizer, emulsifier, acid, alkali and deionized water. The preparation method comprises the following steps: stirring and dissolving cellulose in a solubilizer, then adding a fat-soluble sun-screening agent, and fully stirring and dissolving to obtain an oil phase; dissolving prolamine in ethanol solution, adding alkali, stirring, dissolving completely, mixing with oil phase, mixing with water phase composed of acid, emulsifier and deionized water, homogenizing, and drying. Compared with the sunscreen agent particle coated by a single alcohol soluble protein serving as a wall material, the composite particle prepared by the invention is more stable and has good mechanical property, and can be uniformly dispersed in water, thereby solving the problems of skin irritation caused by a chemical sunscreen agent, dissolution and dispersion of the chemical sunscreen agent, nondegradable property of the sunscreen agent-coated particle, pollution to marine biological environment and the like.
Description
Technical Field
The invention relates to a coated sun-screening agent, in particular to a liposoluble chemical sun-screening agent particle coated by taking alcohol-soluble protein and cellulose as wall materials, a preparation method thereof and application thereof in sun-screening products, belonging to the technical field of cosmetic processing.
Background
In recent years, sun protection has become a hot spot, wherein chemical sunscreens are attracting attention, and there are more and more solutions to the problems of instability of chemical sunscreens, skin irritation, etc., and the coating technology can effectively solve such problems. However, the particles prepared by the synthetic materials such as polyethylene, polymethyl methacrylate and the like which are used as coating materials at present have nondegradable property, and the plastic particles are almost less than 2 mm, so that the product containing the plastic particles is not easy to filter down after being used, can be directly discharged into rivers, lakes and seas, finally flows into the sea, is swallowed by marine organisms, and enters human bodies through food chains, thereby causing serious harm to the environment and the health of the human bodies.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing sunscreen agent has the technical problem of great irritation.
In order to solve the technical problem, the invention provides a composite wall material particle coated with a fat-soluble sun-screening agent, which is characterized in that raw materials comprise 0.4-0.8 part of alcohol-soluble protein, 0.3-0.6 part of cellulose, 1.3-3.5 parts of the fat-soluble sun-screening agent, 4-10 parts of solubilizer, 0.1-3 parts of emulsifier, 0.02-0.1 part of acid, 0.02-0.1 part of alkali and deionized water in parts by weight.
Preferably, the prolamin is at least one of hordein, zein, hordein and soyamin.
Preferably, the cellulose is ethyl cellulose, propyl cellulose or a mixture of the two.
Preferably, the fat-soluble sunscreen agent is at least one of octyl methoxycinnamate, diethylamino oxybenzoyl hexyl benzoate, benzophenone-3, homosalate and avobenzone.
Preferably, the emulsifier is any one or a mixture of two of a plasma anionic emulsifier and a nonionic emulsifier; the emulsifier is at least one of tween80, span 80, Brij721, Brij72, glyceryl stearate, sodium stearyl glutamate, sodium lauryl sulfate and sodium cetearyl sulfate.
Preferably, the solubilizer is absolute ethyl alcohol.
Preferably, the acid is citric acid; the alkali is at least one of sodium hydroxide, potassium hydroxide and triethanolamine.
The invention also provides a preparation method of the composite wall material particle coated with the fat-soluble sun-screening agent, which is characterized by comprising the following steps:
step 1): in a water bath kettle at the temperature of 40-50 ℃, cellulose is stirred and dissolved in a solubilizer, then a fat-soluble sun-screening agent is added, and the oil phase is obtained after full stirring and dissolution;
step 2): dissolving prolamin in 70-90 vol% ethanol solution, adding alkali, stirring, and dissolving completely;
step 3): mixing the oil phase obtained in the step 1) with the solution obtained in the step 2), and uniformly stirring;
step 4): sequentially adding acid and an emulsifier into deionized water, stirring, and fully dissolving to obtain a water phase;
step 5): slowly adding the water phase obtained in the step 4) into the mixture obtained in the step 3) for homogenization;
step 6): and (3) drying the emulsion obtained in the step 5) to obtain the composite wall material particles coated with the fat-soluble sun-screening agent.
Preferably, the rotation speed of the stirring in the step 1), the step 2), the step 3) and the step 4) is 400-600 r/min; the specific steps of homogenizing in the step 5) are as follows: shearing for 10-15 minutes by a homogenizer with the rotation speed of 13000-25000rpm, and then carrying out high-pressure homogenization under the pressure of 16-26 kpsi; and the drying in the step 6) adopts normal-temperature air drying, freeze drying or spray drying.
The invention also provides application of the composite wall material particle coated with the fat-soluble sun-screening agent in sun-screening cosmetics.
The wall material used in the invention is a natural component, is safe and green, has biodegradability, and the strength of the wall material of the sun-screening particles coated by the natural composite wall material taking the alcohol soluble protein and the cellulose as the wall material is superior to that of the wall material of the sun-screening particles coated by the single alcohol soluble protein as the wall material, and has high mechanical strength and excellent performance, and can be well dispersed in a water phase system. The preparation method of the coated sun-screening agent uses the methods of phase inversion emulsification and pH value adjustment, can greatly reduce the use of ethanol in industry, improves the production safety, and is more environment-friendly.
Compared with the prior art, the invention has the beneficial effects that:
the alcohol soluble protein and cellulose natural composite wall material is coated with the fat soluble sun-screening agent, so that the obtained sun-screening particles have good biocompatibility and are easy to degrade, the dispersibility of the chemical sun-screening agent in water is increased, the irritation of the chemical sun-screening agent to skin is reduced, and compared with the single alcohol soluble protein used as the wall material coated sun-screening agent, the particles are more stable, the mechanical strength is high, and the sun-screening performance is superior.
The preparation method of the invention utilizes the phase inversion emulsification and the pH value adjustment, can greatly reduce the use of ethanol in industry, improves the safety, and is more environment-friendly.
The invention is exemplified by its application in sunscreen skin care cosmetics such as creams, lotions, etc., but is not limited to its application in other color cosmetic products.
Drawings
FIG. 1 is a transmission electron microscope image of A-Plus sunscreen-coated microparticles prepared in example 1;
FIG. 2 is a graph of the particle size distribution of microparticles coated with A-Plus sunscreen prepared in example 3;
FIG. 3 is a test chart of sunscreen obtained in example 4.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
A particle coated with an A-Plus sun-screening agent comprises the following raw materials in parts by weight:
anhydrous ethanol: 4.00 parts; ethyl cellulose: 0.5 part; octyl methoxycinnamate: 0.5 part; diethylaminohydroxybenzoylbenzoic acid hexyl ester: 0.5 part; zein: 0.7 part; sodium lauryl sulfate: 0.1 part; citric acid: 0.05 part; sodium hydroxide: 0.05 part; deionized water was added to 100 parts.
The preparation process comprises the following specific steps:
1) in a water bath kettle at 50 ℃, ethyl cellulose is stirred and dissolved in 2.37 parts of absolute ethyl alcohol, then octyl methoxycinnamate and diethylamino hydroxybenzoyl hexyl benzoate are added, and an oil phase is obtained after full stirring and dissolution;
2) preparing 1.63 parts of absolute ethyl alcohol into an 80% ethanol solution in volume concentration, and sequentially dissolving zein and sodium hydroxide in the 80% absolute ethyl alcohol solution;
3) respectively dissolving sodium dodecyl sulfate and citric acid in deionized water to obtain a water phase;
4) adding the oil phase in the step 1) into the solution in the step 2), fully mixing, slowly adding the water phase in the step 3) into the oil phase, shearing for 10 minutes under a homogenizer, and then homogenizing under high pressure under a high-pressure micro-jet homogenizer;
5) and (3) performing rotary evaporation on the emulsion obtained in the step 4), removing ethanol, and performing spray drying to obtain particles coated with diethylamino hydroxybenzoyl hexyl benzoate (A-Plus) sunscreen, wherein the particle size is 452nm, and the embedding rate of the A-Plus is 15.75%.
Example 2
A particle coated with an A-Plus sun-screening agent comprises the following raw materials in parts by weight:
anhydrous ethanol: 4.00 parts; ethyl cellulose: 0.5 part; octyl methoxycinnamate: 0.5 part; diethylaminohydroxybenzoylbenzoic acid hexyl ester: 2 parts of (1); zein: 0.7 part; tween 80: 3 parts of a mixture; citric acid: 0.08 part; sodium hydroxide: 0.08 part; deionized water was added to 100 parts.
The preparation process comprises the following specific steps:
1) in a water bath kettle at 50 ℃, ethyl cellulose is stirred and dissolved in 2.37 parts of absolute ethyl alcohol, then octyl methoxycinnamate and diethylamino hydroxybenzoyl hexyl benzoate are added, and an oil phase is obtained after full stirring and dissolution;
2) preparing 1.63 parts of absolute ethyl alcohol into an 80% ethanol solution in volume concentration, and sequentially dissolving zein and sodium hydroxide in the 80% absolute ethyl alcohol solution;
3) respectively dissolving sodium dodecyl sulfate and citric acid in deionized water to obtain a water phase;
4) adding the oil phase in the step 1) into the solution in the step 2), fully mixing, slowly adding the water phase in the step 3) into the oil phase, shearing for 10 minutes under a homogenizer, and then homogenizing under high pressure under a high-pressure micro-jet homogenizer;
5) and (3) performing rotary evaporation on the emulsion obtained in the step 4), removing ethanol, and performing spray drying to obtain particles coated with diethylamino hydroxybenzoyl hexyl benzoate (A-Plus) sunscreen, wherein the particle size is 650nm, and the embedding rate of the A-Plus is 34.8%.
Example 3
A particle coated with an A-Plus sun-screening agent comprises the following raw materials in parts by weight:
anhydrous ethanol: 4.00 parts; ethyl cellulose: 0.25 part; octyl methoxycinnamate: 0.5 part; diethylaminohydroxybenzoylbenzoic acid hexyl ester: 1 part; zein: 0.75 part; tween 80: 3 parts of a mixture; citric acid: 0.02 part; sodium hydroxide: 0.02 part; deionized water was added to 100 parts.
The preparation process comprises the following specific steps:
1) in a water bath kettle at 50 ℃, ethyl cellulose is stirred and dissolved in 2.37 parts of absolute ethyl alcohol, then octyl methoxycinnamate and diethylamino hydroxybenzoyl hexyl benzoate are added, and an oil phase is obtained after full stirring and dissolution;
2) preparing 1.63 parts of absolute ethyl alcohol into an 80% ethanol solution in volume concentration, and sequentially dissolving zein and sodium hydroxide in the 80% absolute ethyl alcohol solution;
3) dissolving sodium dodecyl sulfate and citric acid in deionized water to obtain a water phase;
4) adding the oil phase in the step 1) into the solution in the step 2), fully mixing, slowly adding the water phase in the step 3) into the oil phase, shearing for 10 minutes under a homogenizer, and then homogenizing under high pressure under a high-pressure micro-jet homogenizer;
5) performing rotary evaporation on the emulsion obtained in the step 4), removing ethanol, and performing freeze drying to obtain microparticles coated with diethylamino hydroxybenzoyl hexyl benzoate (A-Plus) sunscreen agent, wherein the particle size is 569.25nm, and the embedding rate of the A-Plus is 26.9%.
Comparative example 1
A particle only using zein as a wall material to coat an A-Plus sun-screening agent comprises the following raw materials in parts by weight:
anhydrous ethanol: 4 parts of a mixture; octyl methoxycinnamate: 0.5 part; diethylaminohydroxybenzoylbenzoic acid hexyl ester: 0.5 part; zein: 0.7 part; sodium lauryl sulfate: 0.1 part; citric acid: 0.05 part; sodium hydroxide: 0.05 part; deionized water was added to 100 parts.
The preparation process comprises the following specific steps:
1) adding octyl methoxycinnamate and diethylamino hydroxybenzoyl hexyl benzoate into 2.37 parts of absolute ethyl alcohol in a water bath kettle at 50 ℃, and fully stirring and dissolving to obtain an oil phase;
2) preparing 1.63 parts of absolute ethyl alcohol into an 80% ethanol solution in volume concentration, and sequentially dissolving zein and sodium hydroxide in the 80% absolute ethyl alcohol solution;
3) respectively dissolving sodium dodecyl sulfate and citric acid in deionized water to obtain a water phase;
4) adding the oil phase in the step 1) into the solution in the step 2), fully mixing, slowly adding the water phase in the step 3) into the oil phase, shearing for 10 minutes under a homogenizer, and then homogenizing under high pressure under a high-pressure micro-jet homogenizer;
5) and (3) performing rotary evaporation on the emulsion obtained in the step 4), removing ethanol, and performing spray drying to obtain the microparticles which are not coated with the diethylamino hydroxybenzoyl hexyl benzoate (A-Plus) sun-screening agent.
Example 4
Sunscreen emulsion was prepared from the a-Plus sunscreen-coated microparticles obtained in example 1, consisting of the following raw materials in parts by weight:
phase A:
phase B:
5 parts of glycerin
0.2 portion of xanthan gum
Deionized water to 100 parts by weight
And C phase:
2.98 parts of microparticles coated with A-Plus sunscreen
10 portions of deionized water
The preparation process comprises the following specific steps:
the first step is as follows: accurately weighing each component in the phase A, putting the components in a beaker A, and fully stirring and dissolving the components in a water bath at the temperature of 80-90 ℃;
the second step is that: accurately weighing a certain amount of deionized water in a beaker B, and dissolving the rest components in the beaker B in the deionized water;
the third step: slowly mixing the phase A and the phase B, and homogenizing for 3-5 minutes by using a homogenizer with the rotating speed r being 13000 rpm;
the fourth step: and (3) uniformly dispersing the phase C components in deionized water, adding the phase C components into the cream prepared in the third step at the temperature of lower than 50 ℃, and fully stirring to obtain the sunscreen cream containing the A-Plus sunscreen particles.
Comparative example 2
The emulsion without the sun-screening agent comprises the following raw materials in parts by weight:
phase A:
phase B:
5 parts of glycerin
0.2 portion of xanthan gum
Deionized water is added into the cream by weight of 100 parts
The preparation process comprises the following specific steps:
the first step is as follows: accurately weighing each component in the phase A, putting the components in a beaker A, and fully stirring and dissolving the components in a water bath at the temperature of 80-90 ℃;
the second step is that: accurately weighing a certain amount of deionized water in a beaker B, and dissolving the rest components in the beaker B in the deionized water;
the third step: slowly mixing the phase A and the phase B, and homogenizing for 3-5 minutes by using a homogenizer with the rotating speed r being 13000 rpm; cooling and fully stirring.
Comparative example 3
The emulsion added with the free sun-screening agent comprises the following raw materials in parts by weight:
phase A:
phase B:
5 parts of glycerin
0.2 portion of xanthan gum
Deionized water is added into the cream by weight of 100 parts
The preparation process comprises the following specific steps:
the first step is as follows: accurately weighing each component in the phase A, putting the components in a beaker A, and fully stirring and dissolving the components in a water bath at the temperature of 80-90 ℃;
the second step is that: accurately weighing a certain amount of deionized water in a beaker B, and dissolving the rest components in the beaker B in the deionized water;
the third step: slowly mixing the phase A and the phase B, and homogenizing for 3-5 minutes by using a homogenizer with the rotating speed r being 13000 rpm; cooling and fully stirring.
And (3) testing the sun protection effect: the sunscreen creams of example 4, comparative example 2 and comparative example 3 were subjected to in vitro sunscreen testing using an SPF-290AS instrument and the results are shown in table 1.
TABLE 1
| SPF | PFA | |
| Example 4 | 4.29 | 2.93 |
| Comparative example 2 | 1.01 | 1 |
| Comparative example 3 | 2.86 | 2.33 |
As can be seen from Table 1, the A-Plus coated particles (wherein the mass of the A-Plus, the mass of MC80 and the total mass of the sunscreen cream are 1.24%) have the best sunscreen effect when added into the cream in a very small amount, and are superior to sunscreen creams containing the A-Plus (uncoated) which accounts for 0.62% of the total mass of the sunscreen cream, because zein is used as a wall material to form a transparent and glossy film, so that the transparent and glossy effect is better, and the sunlight protection can be effectively carried out on the skin by increasing the dosage of the sunscreen agent particles for embedding the A-Plus.
Claims (10)
1. The composite wall material particle coated with the fat-soluble sun-screening agent is characterized in that raw materials comprise, by weight, 0.4-0.8 part of prolamin, 0.3-0.6 part of cellulose, 1.3-3.5 parts of the fat-soluble sun-screening agent, 4-10 parts of solubilizer, 0.1-3 parts of emulsifier, 0.02-0.1 part of acid, 0.02-0.1 part of alkali and deionized water.
2. The lipid-soluble sunscreen coated composite wall material microparticle of claim 1, wherein said prolamin is at least one of hordein, zein, hordein and soyamin.
3. The lipid-soluble sunscreen coated composite wall material particle as claimed in claim 1, wherein the cellulose is ethyl cellulose, propyl cellulose or a mixture of the ethyl cellulose and the propyl cellulose.
4. The lipid-soluble sunscreen coated composite wall material microparticle of claim 1 wherein the lipid-soluble sunscreen is at least one of octyl methoxycinnamate, diethylamino oxybenzoyl hexyl benzoate, benzophenone-3, homosalate and avobenzone.
5. The lipid-soluble sunscreen coated composite wall material particle as claimed in claim 1, wherein the emulsifier is any one or a mixture of two of a plasma anionic emulsifier and a nonionic emulsifier; the emulsifier is at least one of tween80, span 80, Brij721, Brij72, glyceryl stearate, sodium stearyl glutamate, sodium lauryl sulfate and sodium cetearyl sulfate.
6. The lipid-soluble sunscreen coated composite wall material particle as claimed in claim 1, wherein the solubilizer is absolute ethyl alcohol.
7. The lipid-soluble sunscreen coated composite wall material particle as claimed in claim 1, wherein the acid is citric acid; the alkali is at least one of sodium hydroxide, potassium hydroxide and triethanolamine.
8. The method for preparing the lipid-soluble sunscreen coated composite wall material particle as claimed in any one of claims 1 to 7, wherein the method comprises the following steps:
step 1): in a water bath kettle at the temperature of 40-50 ℃, cellulose is stirred and dissolved in a solubilizer, then a fat-soluble sun-screening agent is added, and the oil phase is obtained after full stirring and dissolution;
step 2): dissolving prolamin in 70-90 vol% ethanol solution, adding alkali, stirring, and dissolving completely;
step 3): mixing the oil phase obtained in the step 1) with the solution obtained in the step 2), and uniformly stirring;
step 4): sequentially adding acid and an emulsifier into deionized water, stirring, and fully dissolving to obtain a water phase;
step 5): slowly adding the water phase obtained in the step 4) into the mixture obtained in the step 3) for homogenization;
step 6): and (3) drying the emulsion obtained in the step 5) to obtain the composite wall material particles coated with the fat-soluble sun-screening agent.
9. The method for preparing the lipid-soluble sunscreen composite wall material particle as claimed in claim 8, wherein the rotation speeds of the stirring in the steps 1), 2), 3) and 4) are all 400-600 r/min; the specific steps of homogenizing in the step 5) are as follows: shearing for 10-15 minutes by a homogenizer with the rotation speed of 13000-25000rpm, and then carrying out high-pressure homogenization under the pressure of 16-26 kpsi; and the drying in the step 6) adopts normal-temperature air drying, freeze drying or spray drying.
10. Use of the coated fat-soluble sunscreen composite wall material microparticle of any one of claims 1-7 in sunscreen cosmetics.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116270261A (en) * | 2023-03-21 | 2023-06-23 | 上海应用技术大学 | Composite wall material sun-screening particles coated with sun-screening agent and preparation method and application thereof |
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