阅读说明：本技术 一种水溶性防晒乳液及其制备方法 (Water-soluble sunscreen emulsion and preparation method thereof ) 是由 郑影 于 2021-04-01 设计创作，主要内容包括：本发明属于化学和日化产品技术领域,公开了一种水溶性防晒乳液,包含原花青素提取物、防晒剂、乳化剂、防腐剂、稳定剂和助剂。原花青素提取物主要以蓝莓、葡萄籽、枸杞为原料制得,原花青素对紫外线(UV)280nm处有强吸收作用,可以抑制紫外线直射皮肤过程,因此原花青素提高了防晒乳液的防晒效果,使得该防晒乳液的SPF值高达45-60,另外,本发明还公开了该防晒乳液的制备方法。由于原花青素表面含有大量的羟基,能与乳液中的极性成分形成氢键,在防晒乳液中结合稳固,加上羟基具有亲水性,吸水和保湿性能优异,因此,添加了原花青素的防晒乳液具有较好的水溶性和明显的保湿效果。(The invention belongs to the technical field of chemical and daily chemical products, and discloses a water-soluble sunscreen emulsion which comprises a proanthocyanidin extract, a sunscreen agent, an emulsifier, a preservative, a stabilizer and an auxiliary agent. The procyanidin extract is mainly prepared from blueberry, grape seeds and medlar serving as raw materials, and has a strong absorption effect on Ultraviolet (UV) rays at 280nm and can inhibit ultraviolet rays from directly irradiating the skin, so that the procyanidin improves the sun-screening effect of the sun-screening emulsion, and the SPF value of the sun-screening emulsion is up to 45-60. The proanthocyanidin surface contains a large amount of hydroxyl groups, so that hydrogen bonds can be formed with polar components in the emulsion, the proanthocyanidin surface can be firmly combined in the sunscreen emulsion, and the hydroxyl groups have hydrophilicity and excellent water absorption and moisture retention performances, so that the sunscreen emulsion added with the proanthocyanidin has better water solubility and obvious moisture retention effect.)

1. The water-soluble sunscreen emulsion is characterized by comprising procyanidin extract, a sunscreen agent, an emulsifier, a preservative, a stabilizer and an auxiliary agent.

2. The water-soluble sunscreen emulsion according to claim 1, comprising the following components in weight percent: 5-30% of procyanidine extract, 5-20% of auxiliary agent consisting of aloe gel, 5-10% of glycerol, 5-10% of vaseline and 0.5-3% of fat-soluble vitamin, 0.2-2% of zinc oxide as sun-protecting agent, 1-5% of stearic acid as stabilizer, 0.05-2% of glyceryl stearate as emulsifier, 0.04-0.1% of ethylhexyl salicylate as preservative and the balance of deionized water.

3. The water-soluble sunscreen emulsion of claim 1 wherein said sunscreen agent is one or more of procyanidins, zinc oxide, titanium dioxide, methoxycinnamates, salicylates.

4. The water-soluble sunscreen emulsion according to claim 2, wherein the fat-soluble vitamin is one or more of vitamin A, vitamin C, and vitamin E.

5. A water-soluble sunscreen emulsion according to claim 1 or claim 3 wherein the emulsifier is one or more of glyceryl stearate and lecithin, in an amount of 0.01% to 5% by weight.

6. A water-soluble sunscreen emulsion according to claim 2 or claim 3 wherein the zinc oxide is nano zinc oxide having a particle size of 10-40 nm.

7. A water-soluble sunscreen emulsion according to any of claims 1 to 4 wherein the preservative is any one of caprylyl glycol and ethylhexyl salicylate, in an amount of 0.1% to 2% by weight.

8. The water-soluble sunscreen emulsion according to claim 1, wherein said procyanidin extract is obtained by the steps of:

(1) pretreatment of

Mixing the raw materials such as natural plants including blueberries, grape seeds and lycium ruthenicum in a mass ratio of 3-5:2-4:3-5, washing the raw material mixture for a plurality of times, squeezing and filtering to obtain stock solution, drying, crushing, sieving filter residues, adding water, stirring, squeezing and centrifuging to obtain mixed solution A obtained by mixing supernatant and the stock solution;

(2) polyphenol extraction

Adding water and a certain amount of complex enzyme into the precipitate obtained after the mixed solution is centrifuged, adjusting Ph3.0-5.0, performing enzymolysis at 30-50 ℃ for 2-3h, performing stirring, enzyme deactivation, filtration, squeezing and centrifugation, extracting in an extraction device, repeating the steps for many times, and separating to obtain a mixed solution B;

mixing the mixed solution A and the mixed solution B to obtain mixed solution C;

(3) concentrating and drying

Concentrating the mixed solution C with a concentrator, and drying with a low-temperature vacuum drier to obtain polyphenol and procyanidin extract.

9. A process for preparing a water-soluble sunscreen emulsion according to any of claims 1 to 4, characterized in that the water-soluble sunscreen emulsion is produced by the following steps:

(1) preparing water phase by mixing procyanidin extract, emulsifier, zinc oxide and deionized water, heating for dissolving, and stirring to obtain mixture E;

(2) preparation of oil phase: mixing stearic acid, vaseline, glycerol, fat-soluble vitamins and a preservative, heating for dissolving, and uniformly stirring to obtain a mixture F;

(3) and mixing the mixture E and the mixture F, stirring uniformly, heating for dissolving, preserving heat, homogenizing under high pressure, and cooling to room temperature to obtain the water-soluble sunscreen emulsion.

10. A method of forming a water-soluble sunscreen emulsion as claimed in claim 9 wherein: in the mixing step of preparation, heating and dissolving at 60-80 ℃, preserving heat for 1 hour, homogenizing for 5-15 minutes under 10-30 MPa high pressure and 3000-4000rpm, repeatedly homogenizing for 1-3 times, and cooling to room temperature to obtain the product.

Technical Field

The invention belongs to the technical field of chemical and daily chemical products, and relates to a water-soluble sunscreen emulsion and a preparation method thereof, in particular to a sunscreen emulsion containing procyanidin extract and a preparation method thereof.

Background

The skin diseases caused by ultraviolet rays will be increasingly developed as people age. The short-term effect caused by ultraviolet radiation is mainly manifested as sunburn and suntan, erythema can be generated after the skin absorbs the ultraviolet radiation for 2-24 hours by the optically active substance, edema, blister and desquamation are accompanied, serious even systemic symptoms appear, various color spots can be caused by long-term exposure of the skin, and serious diseases such as skin cancer can be caused. Skin aging phenomena such as skin dryness, sagging, drooping and wrinkles can also be caused due to factors such as solar irradiation and age.

CN202010455788 discloses a whitening sun-screening emulsion containing natural plant sun-screening components and a preparation method thereof, wherein the sun-screening emulsion comprises the following raw materials in parts by weight: 3-5 parts of ethylhexyl methoxycinnamate, 3-5 parts of ethylhexyl salicylate, 3-5 parts of bis-ethylhexyloxyphenol methoxyphenyl triazine, 10-20 parts of octocrylene, 10-20 parts of plant extract, 3-5 parts of ethylhexyl triazone, 3-5 parts of ultraviolet absorbent, 3-5 parts of humectant, 5-10 parts of whitening agent, 3-5 parts of phenoxyethanol, 3-5 parts of triethanolamine, 1-3 parts of thickener and 3-5 parts of water. However, most of chemical sunscreen creams achieve the purpose of sunscreen by utilizing the characteristic of absorbing ultraviolet rays, and convert the ultraviolet rays into molecular vibration energy or heat energy to achieve the effect of sunscreen, but the long-term use of the chemical sunscreen creams causes skin problems such as large pores, dry skin and the like.

CN 201910049375 discloses a sunscreen emulsion with moisturizing effect and a preparation method thereof, wherein the sunscreen emulsion comprises the following raw materials by mass percent: 2.5-3.5% of garlic bulb extract, 0.8-1.6% of amur cork tree bark extract, 0.5-1.5% of raspberry extract, 4.8-5.2% of cetostearyl alcohol, 1.8-3.8% of tetrahydrocurcumin, 8.5-9.5% of glycerol, 3.5-5.5% of methyl p-hydroxybenzoate, 2.5-5.5% of acrylic acid (ester)/acrylamide copolymer, 2.5-3.5% of cetearyl glucoside, 1.6-1.8% of hydrogenated lecithin, 0.12-0.18% of sodium alginate, 0.01-0.03% of essence, 0.02-0.05% of antioxidant, 0.1-0.2% of preservative and the balance of deionized water. This sunscreen lotion with effect of moisturizing has excellent result of use, but this sunscreen lotion utilizes oily ingredient or thickener to adjust sunscreen lotion's fusion degree, lead to sunscreen lotion's water sense not clear mildly, it is comparatively greasy, bring discomfort for the user, can not realize giving first place to natural plant sunscreen composition, and the cooperation is whitened sunscreen composition, make sunscreen lotion's sunscreen effect obtain the promotion of very big degree, can not reach through the harmonious cooperation with natural plant composition and organic synthesis sunscreen composition, make sunscreen lotion can carry out sun-proof purpose for a long time, thereby it is unfavorable to use sunscreen lotion to people to sun-block. There is a need to develop an anti-aging sunscreen lotion that can achieve sunscreen effects and is also water-soluble.

Disclosure of Invention

The invention aims to provide a water-soluble sunscreen emulsion and a preparation method thereof, wherein the sunscreen emulsion contains an extract of procyanidine, the defects that the existing sunscreen emulsion is single in ultraviolet absorption wavelength, the safety of the reused sunscreen emulsion is problematic, and the antioxidant effect is lacked are overcome, and the procyanidine is prepared from natural plants, is safe and reliable and has no side effect.

In addition, another object of the present invention is to provide the moisturizing effect of the water-soluble sunscreen emulsion, wherein the proanthocyanidin has a molecular structure containing a large amount of hydrophilic phenolic hydroxyl groups, which can strongly bind to water molecules to retain moisture, and can form a complex with proteins, polypeptides, polysaccharides, polyols, lipids, etc., which are excellent moisturizing factors per se. The procyanidin has the moisturizing function also reflected in the inhibition effect on hyaluronidase, so the sunscreen emulsion added with procyanidin has good water solubility and deep moisturizing effect.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows:

a water-soluble sunscreen lotion contains procyanidin 10-40% by weight of the total lotion.

The water-soluble sunscreen emulsion also contains an emulsifier, stearic acid, a preservative, zinc oxide, fat-soluble vitamins, a preservative, glycerol, vaseline, deionized water and the like.

The sunscreen agent is one or more of procyanidine, zinc oxide, titanium dioxide, methoxy cinnamate and salicylate.

The emulsifier is one or more of glycerol stearate and lecithin, and the content of the emulsifier is 0.01-5% of the total weight.

The water-soluble sunscreen emulsion also contains a preservative which is any one of caprylyl glycol and ethylhexyl salicylate, and the content of the preservative is 1% -3%.

More preferably, the water-soluble sunscreen emulsion further comprises zinc oxide.

More preferably, the zinc oxide is nano zinc oxide, the particle size is 10-40nm, and the content of the nano zinc oxide is 0.2-2% of the total weight of the sunscreen emulsion. Nano zinc oxide is a broad-spectrum inorganic ultraviolet screening agent, and is increasingly used due to its effective screening, safety and antibacterial properties against UVA.

The invention further provides a preparation method of the water-soluble sunscreen emulsion, which comprises the following steps:

(1) pretreatment of

Mixing natural plants such as blueberries, grape seeds, black Chinese wolfberry and the like with a certain mass, washing the raw material mixture for a plurality of times, squeezing and filtering to obtain stock solution, drying, crushing, sieving, adding water, stirring, squeezing and centrifuging filter residues to obtain mixed solution A obtained by mixing supernatant and the stock solution.

(2) Polyphenol extraction

Adding water and a certain amount of complex enzyme into the precipitate after the mixed solution is centrifuged, adjusting Ph3.0-5.0, performing enzymolysis at 30-50 ℃ for 2-3h, performing stirring, enzyme deactivation, filtration, squeezing and centrifugation, extracting in an extraction device, repeating the steps for many times, and separating to obtain a mixed solution B.

And mixing the mixed solution A and the mixed solution B to obtain mixed solution C.

(3) Concentrating and drying

Concentrating the mixed solution C with a concentrator, and drying with a low-temperature vacuum drier to obtain polyphenol and procyanidin extract.

(4) Preparation of Water-soluble sunscreen emulsions

The raw materials for preparing the beverage comprise, by mass, 5-30% of procyanidine extract, 5-20% of aloe gel, 1-5% of stearic acid, 0.01-5% of emulsifier, 0.04-0.1% of preservative, 0.2-0.5% of zinc oxide, 0.5-3% of fat-soluble vitamin, 0.1-2% of preservative, 5-10% of glycerol, 5-10% of vaseline and 30-80% of deionized water.

The water phase is prepared by mixing procyanidin extract, emulsifier, zinc oxide and deionized water, heating to dissolve, and stirring to obtain mixture E.

Preparation of oil phase: mixing stearic acid, vaseline, glycerol, fat-soluble vitamins and preservative, heating for dissolving, and stirring uniformly to obtain a mixture F.

And mixing the mixture E and the mixture F, uniformly stirring, heating and dissolving at 60-80 ℃, preserving heat for 1 hour, homogenizing for 5-15 minutes at the rotating speed of 3000-4000rpm under the high pressure of 10MPa, repeatedly homogenizing for 3 times, and cooling to room temperature to obtain the water-soluble sunscreen emulsion.

Compared with the prior art, the technical scheme of the invention at least has the following beneficial effects:

(a) good water solubility and safety

The sunscreen emulsion containing the procyanidin extract is prepared from natural plants, and procyanidin has a polyhydroxy structure, so that the sunscreen emulsion has good water solubility and is evaluated through safety. The water-soluble sunscreen emulsion has strong permeability and is not heavy, and is suitable for various skin types. The procyanidine extract adopted by the sunscreen emulsion is prepared by extracting natural plants such as blueberries, grape seeds, black Chinese wolfberry and the like, and is safe, reliable and free of side effects.

(b) Effective sun protection

Specific experiments in the examples show that the sunscreen emulsion containing the procyanidin extract can effectively prevent ultraviolet rays in sunlight from irradiating human skin to cause skin damage. Procyanidin has strong absorption effect on Ultraviolet (UV) at 280 nm. Ultraviolet irradiation of skin can induce lipid peroxide generation, and procyanidin can inhibit the process, which indicates that procyanidin extracted from natural plants can relieve sun damage to a certain extent.

(c) Antioxidant effect

The water-soluble sunscreen emulsion containing procyanidin prepared by the invention has strong oxidation resistance. Procyanidin is a polyphenol compound, contains a large amount of active phenolic hydroxyl, releases hydrogen ions after being oxidized in vivo, competitively combines with active oxygen free radicals to achieve the effect of removing free radicals, and also competitively combines with oxides to protect lipid from being oxidized and block free radical chain reaction, free radicals generated after reaction can generate a polymer with a catechin and pyrogallol structure through nucleophilic addition reaction, and the polymer still has strong antioxidant activity.

In summary, in the technical scheme of the invention, the proanthocyanidin extract is prepared by selecting natural plants such as blueberries, grape seeds and medlar, extracting, concentrating and drying the natural plants to prepare the proanthocyanidin extract into the sunscreen emulsion, and on the basis of effective broad-spectrum ultraviolet absorption for sunscreen, the sunscreen emulsion can remove free radicals, relieve cell oxidative damage and relieve UVA-mediated apoptosis and becomes a safe and effective sunscreen product through a safety evaluation test.

Detailed Description

Blank control

The blank sample was a Biore style SPF50 sunscreen available from the market.

Example one

The embodiment provides a water-soluble sunscreen emulsion and a preparation method thereof, wherein procyanidin extracted from a natural plant mixture is mainly added into the sunscreen emulsion, and the preparation method comprises the following specific steps:

a water-soluble sunscreen emulsion comprises the following raw materials in percentage by weight: 30% of procyanidin extract, 20% of aloe gel, 5% of stearic acid, 0.5% of emulsifier, 0.05% of preservative ethylhexyl salicylate, 0.2% of zinc oxide, 3% of fat-soluble vitamin, 10% of glycerol, 10% of vaseline and the balance of deionized water.

(1) Preparing a proanthocyanidin extract: firstly, pretreatment is carried out: mixing and crushing blueberries, grape seeds and medlar in a mass ratio of 5:4:5, squeezing to obtain a stock solution, adding water into filter residues, and squeezing to obtain a mixed solution; and secondly, extracting essential oil: supercritical CO₂Extracting to obtain essential oil; and (3) adding water again for extraction: adding water and complex enzyme, stirring,Inactivating enzyme, filtering, squeezing again, centrifuging, repeating for several times, and mixing the obtained extractive solutions to obtain polyphenol stock solution mixed extractive solution; finally, ethanol extraction is carried out: adding ethanol, stirring, squeezing, filtering, repeating for several times to obtain procyanidin stock solution mixed extractive solution, concentrating, and drying to obtain procyanidin extract.

(2) And preparing the water phase, namely mixing the procyanidin extract, the emulsifier, the zinc oxide and deionized water according to the proportion, heating to dissolve, and uniformly stirring to obtain a mixture A.

(3) Preparation of oil phase: mixing stearic acid, vaseline, glycerol, fat-soluble vitamins and preservative in the above proportion, heating to dissolve, and stirring uniformly to obtain a mixture B.

And mixing the mixture A and the mixture B, stirring uniformly, heating to dissolve at 80 ℃, preserving heat for 1 hour, homogenizing at the rotation speed of 4000rpm under the high pressure of 10MPa for 15 minutes, repeatedly homogenizing for 3 times, and cooling to room temperature to obtain the water-soluble sunscreen emulsion.

Example two

The embodiment provides a water-soluble sunscreen emulsion and a preparation method thereof, wherein procyanidin extracted from a natural plant mixture is mainly added into the sunscreen emulsion, and the preparation method comprises the following specific steps:

the water-soluble sunscreen emulsion comprises the following raw materials in percentage by weight: 15% of procyanidin extract, 15% of aloe gel, 3% of stearic acid, 3% of emulsifier, 0.1% of preservative caprylyl glycol, 0.5% of zinc oxide, 3% of fat-soluble vitamin, 5% of glycerol, 5% of vaseline and the balance of deionized water.

(1) Preparing a proanthocyanidin extract: firstly, pretreatment is carried out: mixing and crushing blueberries, grape seeds and medlar in a mass ratio of 4:3:4, squeezing to obtain a stock solution, adding water into filter residues, and squeezing to obtain a mixed solution; and secondly, extracting essential oil: supercritical CO₂Extracting to obtain essential oil; and (3) adding water again for extraction: adding water and complex enzyme, stirring, inactivating enzyme, filtering, squeezing, centrifuging, repeating for several times, and mixing the obtained extractive solutions to obtain polyphenol stock solution mixed extractive solution; finally, ethanol extraction is carried out: adding ethanol, stirring, squeezing, filtering, and repeating for several timesAnd then, obtaining the procyanidine stock solution mixed extract, and concentrating and drying to obtain the procyanidine extract.

(2) And preparing the water phase, namely mixing the procyanidin extract, the emulsifier, the zinc oxide and deionized water according to the proportion, heating to dissolve, and uniformly stirring to obtain a mixture A.

(3) Preparation of oil phase: mixing stearic acid, vaseline, glycerol, fat-soluble vitamins and preservative in the above proportion, heating to dissolve, and stirring uniformly to obtain a mixture B.

Mixing the mixture A and the mixture B, stirring uniformly, heating to dissolve at 75 ℃, preserving heat for 1 hour, homogenizing for 5 minutes at the rotating speed of 3000 under the high pressure of 10MPa, repeatedly homogenizing for 3 times, and cooling to room temperature to obtain the water-soluble sunscreen emulsion.

EXAMPLE III

The embodiment provides a water-soluble sunscreen emulsion and a preparation method thereof, wherein procyanidin extracted from a natural plant mixture is mainly added into the sunscreen emulsion, and the preparation method comprises the following specific steps:

the water-soluble sunscreen emulsion comprises the following raw materials in percentage by weight: 10% of procyanidin extract, 20% of aloe gel, 5% of stearic acid, 3% of emulsifier, 0.1% of preservative caprylyl glycol, 0.5% of zinc oxide, 3% of fat-soluble vitamin, 5% of glycerol, 5% of vaseline and the balance of deionized water.

(1) Preparing a proanthocyanidin extract: firstly, pretreatment is carried out: mixing and crushing blueberries, grape seeds and medlar in a mass ratio of 3:2:3, squeezing to obtain a stock solution, adding water into filter residues, and squeezing to obtain a mixed solution; and secondly, extracting essential oil: supercritical CO₂Extracting to obtain essential oil; and (3) adding water again for extraction: adding water and complex enzyme, stirring, inactivating enzyme, filtering, squeezing, centrifuging, repeating for several times, and mixing the obtained extractive solutions to obtain polyphenol stock solution mixed extractive solution; finally, ethanol extraction is carried out: adding ethanol, stirring, squeezing, filtering, repeating for several times to obtain procyanidin stock solution mixed extractive solution, concentrating, and drying to obtain procyanidin extract.

(2) And preparing the water phase, namely mixing the procyanidin extract, the emulsifier, the zinc oxide and deionized water according to the proportion, heating to dissolve, and uniformly stirring to obtain a mixture A.

(3) Preparation of oil phase: mixing stearic acid, vaseline, glycerol, fat-soluble vitamins and preservative in the above proportion, heating to dissolve, and stirring uniformly to obtain a mixture B.

Mixing the mixture A and the mixture B, stirring uniformly, heating to dissolve at 75 ℃, preserving heat for 1 hour, homogenizing for 10 minutes at 3000 rpm under 10MPa high pressure, repeatedly homogenizing for 3 times, and cooling to room temperature to obtain the water-soluble sunscreen emulsion.

Comparative example

The comparative example provides a water-soluble sunscreen emulsion, which is different from the first example in that procyanidin is not added in the sunscreen agent, the content of zinc oxide is increased to 5%, and the content of other components and the preparation method are the same as the first example.

And (4) testing the moisturizing effect: when the moisturizing effect of the cosmetic is judged, a single application test which is finished in a short time is suitably performed for a tester with the same skin type. The samples of examples one and two were applied at a uniform application density for 1 short time, gently tapped until absorbed, and the moisture content of the stratum corneum and the moisture loss of the epidermis through the skin before and after application were measured at different times to analyze the moisturizing effect. The test results are as follows:

the water-soluble sunscreen emulsion can permanently moisten and effectively moisturize the skin, and is proved to be capable of keeping the skin moisture value of the sunscreen emulsion of the embodiment 1, the embodiment 2 and the embodiment 3 higher than that of a blank control group after the sunscreen emulsion of the embodiment 1, the embodiment 2 and the embodiment 3 is used for 20 hours.

Sun protection factor SPF value test: the film similar to skin tissue is placed into an irradiation box simulating sunlight for irradiation, the performance change of the film after irradiation is observed, and the sun protection factor SPF value and the PA value are tested, wherein the specific numerical values are shown in the following table:

the test results show that the sunscreen performance of example 1 is better than that of comparative example, example 2 and example 3, and the matching of the components in example 1 shows that the components cooperate with each other to achieve synergistic interaction, so that the sunscreen function of the sunscreen emulsion can be further promoted and enhanced.

The water-soluble sunscreen emulsion is characterized by comprising the following components in percentage by weight: 5-30% of procyanidine extract, 5-20% of auxiliary agent consisting of aloe gel, 5-10% of glycerol, 5-10% of vaseline and 0.5-3% of fat-soluble vitamin, 0.2-2% of zinc oxide as sun-protecting agent, 1-5% of stearic acid as stabilizer, 0.05-2% of glyceryl stearate as emulsifier, 0.04-0.1% of ethylhexyl salicylate as preservative and the balance of deionized water.

The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments, and therefore, any simple modifications or equivalent changes made to the above embodiments according to the technical spirit of the present invention still fall within the scope of the technical solution of the present invention.