CN111603396B - Poly natural polyphenol type sunscreen gel and preparation method thereof - Google Patents
Poly natural polyphenol type sunscreen gel and preparation method thereof Download PDFInfo
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- CN111603396B CN111603396B CN202010537797.4A CN202010537797A CN111603396B CN 111603396 B CN111603396 B CN 111603396B CN 202010537797 A CN202010537797 A CN 202010537797A CN 111603396 B CN111603396 B CN 111603396B
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- 230000000475 sunscreen effect Effects 0.000 title claims abstract description 84
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
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- SWUARLUWKZWEBQ-VQHVLOKHSA-N phenethyl caffeate Chemical compound C1=C(O)C(O)=CC=C1\C=C\C(=O)OCCC1=CC=CC=C1 SWUARLUWKZWEBQ-VQHVLOKHSA-N 0.000 claims abstract description 100
- SWUARLUWKZWEBQ-UHFFFAOYSA-N phenylethyl ester of caffeic acid Natural products C1=C(O)C(O)=CC=C1C=CC(=O)OCCC1=CC=CC=C1 SWUARLUWKZWEBQ-UHFFFAOYSA-N 0.000 claims abstract description 92
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/042—Gels
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/66—Enzymes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Birds (AREA)
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- Dispersion Chemistry (AREA)
- Chemical & Material Sciences (AREA)
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- Cosmetics (AREA)
Abstract
The invention discloses a poly natural polyphenol type sunscreen gel, which comprises caffeic acid phenethyl ester nano particles and a gel substrate; the gel substrate is a mixture of polyvinyl alcohol and water; the mass percentage of the poly caffeic acid phenethyl ester nano particles in the gel substrate is 1-12%. The invention also discloses a preparation method of the poly natural polyphenol type sunscreen gel. The poly caffeic acid phenethyl ester nano particles in the sun-proof gel have good oxidation resistance, high stability and low blood toxicity; the preparation method is green, simple and convenient, has no complex synthetic preparation process, and the raw materials are all natural extraction/purification raw materials.
Description
Technical Field
The invention relates to the field of cosmetics, in particular to a poly natural polyphenol type sunscreen gel and a preparation method thereof.
Background
The skin is the first barrier for blocking external bacteria, viruses, dust and other substances, and after the skin is excessively exposed to ultraviolet rays, epidermal cells can be damaged, tyrosinase is activated, melanin synthesis is accelerated, the moisturizing function of the skin is damaged, the skin becomes dry, elastic fibers in a dermis layer are damaged, fine wrinkles are generated, and the skin is further inflamed and burned under strong irradiation. Ultraviolet light is a generic term for radiation in the electromagnetic spectrum having wavelengths from 100-400 nm. The ultraviolet light can be divided into UVA (320-400nm), UVB (280-320nm) and UVC (200-280nm) according to the wavelength. UVC hardly reaches the ground surface due to the blocking and absorption of the ozone layer, but UVA and UVB can reach the ground surface through the atmospheric layer to cause certain damage to human skin. UVB can reach the dermis layer, and damage such as sunburn and erythema is caused to the skin; UBAs are capable of penetrating the dermis, damaging cellular DNA, collagen damage, accelerating skin aging, and in some cases, becoming pigmented skin cancers, and the like.
The current commercial sunscreen product concept involves physical and chemical sunscreens, wherein the physical sunscreen gel atomic particles are in the form of a sheet that when applied to the face reflect sunlight like a mirror to achieve the sunscreen goal. However, physical sunscreen products have many limitations, such as the moisturizing effect may be less natural for darker people; the texture is drier, and the skin is not moistened for people with drier skin; is not suitable for whole body sun protection; and make-up removal products must be used to assist in removal. The chemical sunscreen gel is a transparent substance which can absorb ultraviolet rays to convert the ultraviolet rays into molecular vibration energy or heat energy to achieve the sunscreen effect by utilizing the principle of absorbing ultraviolet rays, but the sunscreen strength of the chemical sunscreen products on the market is low at present, and the ideal effect is achieved by continuously supplementing sunscreen. Ordinary chemical sunscreen has a large burden on skin and is easy to cause skin allergy, and the chemical sunscreen agent is reported to cause coral larvae in the sea and destroy the biological diversity of the sea.
The natural extract is used as a piece of ultraviolet-resistant light for animals and plants in nature, wherein a large amount of polyphenols have excellent ultraviolet absorption capacity and free radical scavenging capacity, but because the natural extract has low stability and can penetrate skin quickly, a stable and efficient ultraviolet protective layer is difficult to form on the skin, and the further application of the natural extract in the sunscreen market is limited. Therefore, the natural polyphenol sunscreen gel based on the natural extract has the advantages of strong stability, small irritation, high safety and good protection effect, and has higher market application value.
Disclosure of Invention
In order to solve the above-mentioned disadvantages of the related art, the present invention provides a novel sunscreen gel based on propolis extract and a method for preparing the same.
The invention relates to a poly natural polyphenol type sunscreen gel and a preparation method thereof, which are realized by the following technical scheme:
a poly natural polyphenol sunscreen gel comprises caffeic acid phenethyl ester nanoparticles and a gel substrate;
the mass percentage of the poly caffeic acid phenethyl ester nano particles in the gel substrate is 1-12%.
Further, the gel substrate is a mixture of polyvinyl alcohol and water, and the mass percentage of the polyvinyl alcohol in the water is 5% -10%.
Furthermore, the particle size of the poly caffeic acid phenethyl ester nano particles is 100-200 nm.
A method for preparing a poly natural polyphenol sunscreen gel, comprising:
and 5, mixing the poly-caffeic acid phenethyl ester nano particles with a gel substrate to ensure that the mass percentage of the poly-caffeic acid phenethyl ester nano particles in the gel substrate is 1-12%, thus obtaining the poly-natural polyphenol type sunscreen gel.
Further, the solution A is obtained by dissolving caffeic acid phenethyl ester in a mixed solution of water and ethanol which are uniformly mixed according to a volume ratio of 3: 1-3: 2.
Further, the solution B is obtained by dissolving horseradish peroxidase in deionized water.
Further, the concentration of the caffeic acid phenethyl ester in the solution A is 0.5 mg/mL-4 mg/mL.
Further, the concentration of the horseradish peroxidase in the solution B is 0.5-1 mg/mL.
Furthermore, the addition amount of the 30% aqueous hydrogen peroxide solution in the step 3 is 0.2-4 muL/mL.
Further, the polymerization reaction time is 2-12 h.
Compared with the prior art, the invention has the following beneficial effects:
1) the sun-screening gel is different from the traditional inorganic and organic sun-screening agents, natural polyphenol micromolecule caffeic acid phenethyl ester is subjected to macro-molecular preparation of a nano material, a chemical layer has a large number of conjugated structures to absorb ultraviolet rays, and a physical layer can reflect and shield the ultraviolet rays;
2) the poly caffeic acid phenethyl ester nano particles in the sun-proof gel have good anti-oxidation capability, high stability and low blood toxicity;
3) the preparation method is green, simple and convenient, has no complex synthetic preparation process, and the raw materials are all natural extraction/purification raw materials.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1 is a scanning electron micrograph of poly (phenethyl caffeate) nanoparticles prepared in example 19;
FIG. 2 shows the UV-absorbing properties of poly (phenylethyl caffeate) nanoparticles prepared in example 19;
FIG. 3 shows the preparation of poly (caffeic acid phenethyl ester) nanoparticles with radical scavenging ability as described above;
FIG. 4 is a graph of the broad spectrum of ultraviolet absorbance and the corresponding calculated SPF values for the poly natural polyphenol sunscreen gels of examples 1-8 when applied at a thickness of 15 μm;
FIG. 5 is the skin penetration of the poly natural polyphenol sunscreen gel of example 8;
FIG. 6 is a section of experimental skin from a mouse sun screen.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure. The principles of operation not described in detail in the present invention are well known in the art and the common general knowledge in the field, and should be known to those skilled in the art.
Example 1
This example provides a poly natural polyphenol sunscreen gel comprising caffeic acid phenethyl ester nanoparticles and a gel base; the mass percentage of the poly caffeic acid phenethyl ester nano particles in the gel substrate is 0%.
Further, the gel substrate is a mixture of polyvinyl alcohol and water, and the mass percentage of the polyvinyl alcohol in the water is 5%.
Further, the particle size of the poly caffeic acid phenethyl ester nano particles is 100 nm.
Example 2
This example provides a sunscreen gel of the poly-natural polyphenol type.
This example differs from example 1 in that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 1%.
Example 3
This example provides a sunscreen gel of the poly-natural polyphenol type.
This example differs from example 1 in that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base was 2%.
The mass percentage of the polyvinyl alcohol in the water is 6%.
Example 4
This example provides a sunscreen gel of the poly-natural polyphenol type.
This example differs from example 1 in that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base was 4%.
The mass percentage of the polyvinyl alcohol in the water is 7%.
Example 5
This example provides a sunscreen gel of the poly-natural polyphenol type.
This example differs from example 1 in that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base was 6%.
The mass percentage of the polyvinyl alcohol in the water is 8%.
Example 6
This example provides a sunscreen gel of the poly-natural polyphenol type.
This example differs from example 1 in that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base was 8%.
The mass percentage of the polyvinyl alcohol in the water is 9%.
Example 7
This example provides a sunscreen gel of the poly-natural polyphenol type.
This example differs from example 1 in that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 10%.
The mass percentage of the polyvinyl alcohol in the water is 10%.
Example 8
This example provides a sunscreen gel of the poly-natural polyphenol type.
This example differs from example 1 in that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base was 12%.
The mass percentage of the polyvinyl alcohol in the water is 10%.
Example 9
This example is a method for preparing poly (phenethyl caffeate).
Wherein the mass ratio of the caffeic acid phenethyl ester to the horseradish peroxidase is 1500: 1;
the volume ratio of water to ethanol is 3: 1.67;
the concentration of the caffeic acid phenethyl ester in the solution A is 2.14 mg/mL;
the concentration of the horseradish peroxidase in the solution B is 1 mg/mL;
the preparation method of the poly caffeic acid phenethyl ester nano particle of the embodiment is specifically carried out in the following way:
and 4, after the polymerization reaction is finished, removing alcohol solvent in the reaction liquid through a rotary evaporator to obtain poly-caffeic acid phenethyl ester nanoparticles, and freeze-drying the poly-caffeic acid phenethyl ester nanoparticles into dry powder for later use.
Further, the amount of the 30% aqueous hydrogen peroxide solution added in step 3 was 1.4. mu.L/mL of the reaction solution.
Example 10
This example is a method for preparing poly (phenethyl caffeate).
This example differs from example 1 in that:
the mass ratio of caffeic acid phenethyl ester to horseradish peroxidase is 1000: 1;
the volume ratio of water to ethanol is 3: 1;
the concentration of caffeic acid phenethyl ester in the solution A is 2.5 mg/mL;
the concentration of the horseradish peroxidase in the solution B is 0.75 mg/mL;
the preparation method of the poly caffeic acid phenethyl ester nano particle of the embodiment is specifically carried out in the following way:
and 3, mixing the solution A and the solution B, adding 30% aqueous hydrogen peroxide to obtain a reaction solution, and stirring for 2 hours at normal temperature.
Further, the amount of the 30% aqueous hydrogen peroxide solution added in step 3 was 0.2. mu.L/mL.
Example 11
This example is a method for preparing poly (phenethyl caffeate).
This example differs from example 1 in that:
the mass ratio of caffeic acid phenethyl ester to horseradish peroxidase is 2000: 1;
the volume ratio of water to ethanol is 3: 1;
the concentration of caffeic acid phenethyl ester in the solution A is 0.5 mg/mL;
the concentration of the horseradish peroxidase in the solution B is 0.5 mg/mL;
the preparation method of the poly caffeic acid phenethyl ester nano particle of the embodiment is specifically carried out in the following way:
and 3, mixing the solution A and the solution B, adding 30% aqueous hydrogen peroxide to obtain a reaction solution, and stirring for 7 hours at normal temperature.
Furthermore, the addition amount of the 30% aqueous hydrogen peroxide solution in the step 3 is 0.2-4 muL/mL.
Example 12
This example is a method for preparing poly (phenethyl caffeate).
This example differs from example 1 in that:
the mass ratio of caffeic acid phenethyl ester to horseradish peroxidase is 3000: 1;
the volume ratio of water to ethanol is 3: 2;
the concentration of the caffeic acid phenethyl ester in the solution A is 4 mg/mL;
the concentration of the horseradish peroxidase in the solution B is 1 mg/mL;
the preparation method of the poly caffeic acid phenethyl ester nano particle of the embodiment is specifically carried out in the following way:
and 3, mixing the solution A and the solution B, adding 30% aqueous hydrogen peroxide to obtain a reaction solution, and stirring for 12 hours at normal temperature.
Furthermore, the addition amount of the 30% aqueous hydrogen peroxide solution in the step 3 is 0.2-4 muL/mL.
Example 13
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 9 are mixed with a 5% polyvinyl alcohol aqueous solution of a gel substrate, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel substrate is 1%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 14
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 9 are mixed with a 6% polyvinyl alcohol aqueous solution of a gel substrate, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel substrate is 2%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 15
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 9 are mixed with a 7% polyvinyl alcohol aqueous solution of a gel base, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 4%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 16
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 9 are mixed with 8% polyvinyl alcohol aqueous solution of a gel base, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 6%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 17
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 9 are mixed with 9% polyvinyl alcohol aqueous solution of a gel base, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 8%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 18
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 9 are mixed with 10% polyvinyl alcohol in the gel base, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 10%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 19
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 9 are mixed with 10% polyvinyl alcohol in the gel base, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 12%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 20
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 10 are mixed with 10% polyvinyl alcohol in the gel base, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 12%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 21
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 11 are mixed with 10% polyvinyl alcohol in the gel base, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 12%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Example 22
This example provides a method for preparing a sunscreen gel of the poly-natural polyphenol type.
The poly (phenethyl caffeate) nanoparticles prepared in the example 12 are mixed with 10% polyvinyl alcohol in the gel base, so that the mass percentage of the poly (phenethyl caffeate) nanoparticles in the gel base is 12%, and the poly (natural polyphenol) sunscreen gel of the example is obtained.
Experimental part
1. Experimental Material
Caffeic acid phenethyl ester (99%) was purchased from Annaiji chemical, peroxidase (HRP, >300 units/mg) in horseradish from Allatin industries, Inc. (Shanghai, China), 2, 2-diphenyl-1 picrylhydrazine (DPPH, 95%) was purchased from AlfaAesar. Polyvinyl alcohol (pvc-124, viscosity: 54-66 mPas) and absolute ethyl alcohol were provided by Kolon chemical (Chengdu, China).
Ultraviolet light transparent quartz plates (45 mm. times.12.5 mm. times.1.2 mm) were purchased from the Darmoniaceae (Chinese Wuxi).
Animal experiments were performed following the national institutes of health laboratory guidelines for animal care and use, and were approved by the ethical committee of the western hospital, university of sichuan, using female Balb/c mice, 8 weeks old, supplied by medo mada, and were raised for 12 hours in a light/dark cycle.
The instrument comprises: novanano SEM 450 scanning electron microscope, kwl-4a spin coater PerkinElmer Lambda 35 ultraviolet spectrophotometer, Xenogen IVIS-200 in vivo imaging System, UV lamp, skin mirror.
2. Experimental methods
(1) Scanning electron microscope for poly caffeic acid phenethyl ester nano particles
Scanning Electron Microscope (SEM) images are of mica substrates obtained on a Nova nano SEM 450 microscope.
A powder sample of poly (phenethyl caffeate) nanoparticles prepared in example 9 was prepared into a 10mg/mL aqueous suspension and dropped on a mica substrate, and the substrate was rotated by a spin coater at kwl-4a to remove excess suspension. The samples were completely dried under vacuum before testing. And (5) carrying out scanning electron microscope imaging on the sample after spraying gold for 30 s. As shown in fig. 1, the morphology and particle size of the nanoparticles can be observed.
(2) UV absorption of poly (phenethyl caffeate) nanoparticles
50 micrograms of the poly (phenethyl caffeate) nanoparticles prepared in example 9 were added into 1mL of an aqueous solution and sufficiently dispersed by ultrasound to obtain a 50 micrograms/mL aqueous solution, and then the absorbance of the aqueous solution was measured by a Perkinelmer Lambda 35 ultraviolet-visible spectrophotometer. The measured spectral range was 250-800nm and the slit width was 2 nm.
(3) Free radical scavenging activity of poly (caffeic acid phenethyl ester) nanoparticles
The free radical scavenging activity of the poly (phenethyl caffeate) nanoparticles was determined by 2, 2-Diphenylpicrylhydrazine (DPPH) assay.
The specific operation is as follows:
subsequent testing was performed using fresh ethanol solution of DPPH as probe.
The DPPH solution was added to the petri dish, and then different masses of the poly (phenethyl caffeate) nanoparticles prepared in example 9 were added to prepare different concentrations of the solutions, namely 50/33.3/20/10 micrograms of the solutions per milliliter of DPPH.
It is noted that each sample was tested in a volume of 3ml, a final concentration of 0.1mM DPPH, and the scavenging activity of the nanoparticles was evaluated by measuring the change in absorbance at 517nm after mixing with the DPPH solution.
One sample spot was taken every 5 minutes for a total of 30 minutes.
(4) In-vitro method for detecting ultraviolet absorption capacity of poly natural polyphenol type sunscreen gel
The poly natural polyphenol type sunscreen gels of examples 1 to 8, i.e., poly natural polyphenol type sunscreen gels having a mass concentration of 0%, 1%, 2%, 3%, 4%, 6%, 8%, 10%, 12% of poly phenethylcaffeate nanoparticles, which are respectively designated as Hydrogel-0, Hydrogel-1, Hydrogel-2, Hydrogel-3, Hydrogel-4, Hydrogel-5, Hydrogel-6, Hydrogel-7, were coated and left to air-dry for 20min to form a sunscreen film of 15 μm thickness, the ultraviolet absorption spectrum of the sample was measured using an ultraviolet spectrophotometer, and the SPF value thereof was calculated according to the formula
Wherein S (lambda) is the spectral irradiance of the earth sunlight under certain conditions (40 degrees north latitude, 20 degrees solar zenith angle and 0.305cm ozone layer thickness mid-summer noon sunshine), and E (lambda) is the relative effective coefficient of the ultraviolet ray with the wavelength of lambda nm generating the tardive erythema on the human skin.
The ultraviolet absorption capacity test method refers to a paper Skin segmentation-implanted polypoamine Sunscreens published by advanced Function Materials in 2018, and the paper proves that the in vitro test SPF value is similar to the result of the human test SPF when the thickness is 15 mu m.
(5) Evaluation of skin penetration Properties of sunscreen gels
For skin permeation studies, two groups of fresh porcine skin samples of the same area (1.5 x 1.5cm) were prepared.
The phenethyl caffeate small molecules connected with the FITC fluorescent probe and the poly natural polyphenol type sun-proof gel of the embodiment 8 are smeared on the surface of a skin sample, the dosage of the small molecules is 2mg per square centimeter, after incubation for 6 hours in a humidity chamber at 37 ℃, each skin sample is washed 3 times with 30ml of PBS, and the small molecules are cut into 10 mu m pieces which are fixed on a slide glass and then frozen for 30 minutes. Residual FITC fluorescence values in the pig skin were compared by fluorescence microscopy imaging.
(6) Comparative test
The dorsal skin of Balb/c mice was divided into four parts, each 1 x 1.5cm, and then washed with 70% alcohol.
The method is divided into four groups: control group (blank group, No uv irradiation), No protection group (No Sunscreen gel applied, direct uv irradiation), Sunscreen group (uv irradiation after applying a commercial Sunscreen gel) and Hydrogel-7 group (uv irradiation after applying the poly natural polyphenol type Sunscreen gel of example 8 of the present application); PBS was also used as control condition and tinfoil shielding as normal condition.
Then 1060mJ cm at UVB-2The skin marker area was irradiated for 15 minutes (peak at 313 nm). The mice were kept in individual cages until they were observed to wake up. After 3 days of uv irradiation, the mice were then sacrificed and the dorsal skin was excised for tissue staining.
3. Results of the experiment
(1) Scanning electron microscope for poly caffeic acid phenethyl ester nano particles
The result of fig. 1 shows that according to the above preparation method, spherical nanoparticle material with uniform particle size and regular morphology can be prepared, and the particle size of the spherical nanoparticle material is about 150 nm.
(2) UV absorption of poly (phenethyl caffeate) nanoparticles
The result of FIG. 2 shows that, at a detection concentration of 50 micrograms per milliliter, the nanoparticles have good ultraviolet absorption capacity at 290-400 nm, and the absorbance can reach up to 1.5.
(3) Free radical scavenging activity of poly (caffeic acid phenethyl ester) nanoparticles
The results in FIG. 3 show that the DPPH radical scavenging ability of the particles is proportional to the concentration, and 90% clearance is rapidly achieved at a concentration of 50. mu.g/mL.
(4) And (3) detecting the ultraviolet absorption capacity of the poly natural polyphenol type sunscreen gel by an in vitro method.
The results in fig. 4 show that the poly natural polyphenol sunscreen gel of the present invention has strong uv absorption capability, and the uv absorption capability is stronger when the addition amount of the particles is larger, and the poly natural polyphenol sunscreen gel of example 8 can reach the calculated SPF of 70+ when the addition amount is 12%.
(5) Evaluation of skin penetration Properties of sunscreen gels
FIG. 5 shows the results of the three upper images, from left to right, of an electron micrograph, a fluorescence electron micrograph, and two overlaid images of the skin tissue section coated with the caffeic acid phenethyl ester small molecule connected with the FITC fluorescent probe, which show that the caffeic acid phenethyl ester small molecule of the FITC fluorescent probe permeates into the skin;
the electron microscope image, the fluorescence electron microscope image and the two images displayed in an overlapped manner of the following three images, from left to right, of the skin tissue section smeared with the poly natural polyphenol type sunscreen gel of the embodiment 8 connected with the FITC fluorescent probe show that almost all the poly natural polyphenol type sunscreen gel of the embodiment 8 of the invention is remained on the surface of the skin, which proves that the poly natural polyphenol type sunscreen gel has low transdermal capacity and is safer.
The simple natural polyphenol micromolecule caffeic acid phenethyl ester is very easy to be permeated through the skin, and the sunscreen gel taking the poly caffeic acid phenethyl ester nano particles as the main material can be retained on the surface of the skin almost without transdermal effect, so that the sunscreen gel has better human body safety.
(6) Comparative test
As shown in fig. 6, HE staining results showed that the unprotected sample was significantly damaged, and visible are polymorphonuclear leukocyte-containing intracorneal and subcorneal fissures and mildly edematous keratotic fragments of the epidermis, consistent with the changes in sun damaged pathological tissue, as shown in the second row of the first panel of fig. 6.
Interestingly, in skin areas protected by ordinary sun protection, subtle responses to uv damage occurred, e.g., significant thickening of the epidermis, especially the acanthocyte layer with slight cuticle loss and keratoses, as shown in the third panel of fig. 6.
Meanwhile, the results of the sunscreen hydrogel of the present invention covering the skin (as shown in the fourth panel of the first row of fig. 6) are almost the same as the control group (as shown in the first panel of the first row of fig. 6) without uv irradiation, again demonstrating that the sunscreen hydrogel has a good protective effect. Similarly, three-color staining detected that the skin thickening and dermal superficial edema were more pronounced in the sunscreen gel group, collagen fiber disorder, than in the sunscreen gel of the present invention and the sunless control group. . Taken together, these results demonstrate that the product has better performance than other products in reducing uv damage as verified by animal testing.
The results in fig. 6 show that the sunscreen gel of the present invention has better skin protection effect compared to the common commercial sunscreen gel, and the skin samples protected by the sunscreen gel have a more similar appearance state to the control group skin without being irradiated by ultraviolet light.
Claims (9)
1. A preparation method of a poly natural polyphenol type sunscreen gel is characterized in that the poly natural polyphenol type sunscreen gel comprises poly caffeic acid phenethyl ester nano particles and a gel substrate;
the mass percentage of the poly caffeic acid phenethyl ester nano particles in the gel substrate is 1-12%.
The preparation method comprises the following steps:
step 1, preparing a solution A, wherein the solution A is a water-alcohol solution of caffeic acid phenethyl ester;
step 2, preparing a solution B, wherein the solution B is an aqueous solution of horseradish peroxidase;
step 3, mixing the solution A and the solution B according to the mass ratio of caffeic acid phenethyl ester to horseradish peroxidase of 1000: 1-3000: 1, adding 30% aqueous hydrogen peroxide to obtain a reaction solution, and stirring at normal temperature to perform polymerization reaction;
step 4, after the polymerization reaction is finished, removing alcohol solvent in reaction liquid through a rotary evaporator to obtain poly-caffeic acid phenethyl ester nano particles, and freeze-drying the poly-caffeic acid phenethyl ester nano particles into dry powder;
and 5, mixing the poly-caffeic acid phenethyl ester nano particles with a gel substrate to ensure that the mass percentage of the poly-caffeic acid phenethyl ester nano particles in the gel substrate is 1-12%, thus obtaining the poly-natural polyphenol type sunscreen gel.
2. The method according to claim 1, wherein the gel substrate is a mixture of polyvinyl alcohol and water, and the mass percentage of the polyvinyl alcohol in the water is 5-10%.
3. The method according to claim 1, wherein the poly (phenethylcaffeate) nanoparticles have a particle size of 100-200 nm.
4. The method for preparing poly natural polyphenol-type sunscreen gel according to claim 1, wherein the solution A is obtained by dissolving caffeic acid phenethyl ester in a mixed solution of water and ethanol which are uniformly mixed according to a volume ratio of 3: 1-3: 2.
5. The method of claim 1, wherein said solution B is obtained by dissolving horseradish peroxidase in deionized water.
6. The method of claim 1, wherein the concentration of caffeic acid phenethyl ester in solution a is 0.5mg/mL to 4 mg/mL.
7. The method of claim 5, wherein the concentration of horseradish peroxidase in solution B is 0.5-1 mg/mL.
8. The method of claim 5, wherein the amount of 30% aqueous hydrogen peroxide added in step 3 is 0.2-4 μ L/mL.
9. The method of claim 1, wherein the polymerization reaction time is 2-12 hours.
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