CN112022769A - Composition containing epimedium extract and phellodendron amurense extract and application thereof - Google Patents

Composition containing epimedium extract and phellodendron amurense extract and application thereof Download PDF

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CN112022769A
CN112022769A CN202010999980.6A CN202010999980A CN112022769A CN 112022769 A CN112022769 A CN 112022769A CN 202010999980 A CN202010999980 A CN 202010999980A CN 112022769 A CN112022769 A CN 112022769A
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composition
phellodendron amurense
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张贵民
杨鉴
卢小艳
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Lunan Pharmaceutical Group Corp
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
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    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18

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Abstract

The invention relates to the field of cosmetics, in particular to a composition containing epimedium extract and phellodendron amurense extract and application thereof, and specifically relates to application of the composition in preparation of anti-wrinkle skin care products. The invention provides a safe and effective skin care product composition, which takes epimedium extract and phellodendron amurense extract as active ingredients, has obvious oxygen radical scavenging function and antioxidant activity, can reduce the length, the area and the depth of skin wrinkles, improve the collagen level of the skin and has obvious anti-wrinkle effect.

Description

Composition containing epimedium extract and phellodendron amurense extract and application thereof
Technical Field
The invention relates to the field of cosmetics, in particular to a composition containing epimedium extract and phellodendron amurense extract and application thereof, and specifically relates to application of the composition in preparation of anti-wrinkle skin care products.
Background
Wrinkles are the result of skin aging. Skin aging not only directly affects the normal structure and physiological functions of skin tissues, but also indirectly affects the stability of the internal and external environments of the organism, causes imbalance of metabolism in different degrees, and may promote and accelerate aging of the organism, even death.
Skin wrinkles, which are a manifestation of deteriorated skin aging, have recently received increasing attention from beauty-conscious people and medical cosmetologists. At present, a plurality of techniques and methods for removing wrinkles bring good news to beauty lovers, but at the same time, the methods for removing wrinkles are mostly invasive and bring complications such as pigmentation and the like.
With the increasing importance of cosmetic safety, the demand of whitening and caring skin and the understanding of health, cosmetics taking natural plants and Chinese herbal medicines as main components have gradually appeared, and pure natural plant essential oil products are more and more favored by beauty-lovers, and the essence of plants and Chinese herbal medicines is integrated into the cosmetics, so that the natural plant cosmetics not only are combined with the traditional cosmetics and modern cosmetics, but also open up a new territory for the development of national enterprises, and the natural plant cosmetics will become the most important trend for future research and development. In conclusion, in order to solve the problems of poor anti-wrinkle moisturizing curative effect, long service time and large side effect of skin care products on the market, the design of a natural plant skin care product with anti-wrinkle and firming effects is especially necessary.
Disclosure of Invention
The invention provides a safe and effective skin care product composition, which takes epimedium extract and phellodendron amurense extract as active ingredients, has obvious oxygen radical scavenging function and antioxidant activity, can reduce the length, the area and the depth of skin wrinkles, improve the collagen level of the skin and has obvious anti-wrinkle effect. The skin care product composition provided by the invention has good anti-wrinkle effect and is safe to use, the selection of anti-wrinkle people is increased, and the skin care product composition has a good application prospect.
The anti-wrinkle skin care product composition takes epimedium extract and phellodendron amurense extract as active ingredients.
Preferably, the weight ratio of the phellodendron amurense extract to the epimedium extract in the skin care product composition is 1: (0.01-20), and more preferably, the weight ratio of the phellodendron amurense extract to the epimedium extract in the skin care product composition is 1: (0.05-10).
The anti-wrinkle composition contains epimedium extract and phellodendron amurense extract, and the content of total flavonoids in the epimedium is not lower than 50% and the content of aglycon in the epimedium is not lower than 35% by liquid phase detection of the epimedium extract.
The extraction method of the epimedium extract comprises the following steps:
heating icariin and helicase, performing enzymolysis reaction, filtering, adding anhydrous ethanol into the obtained solid, stirring, standing for layering, discarding the solid, concentrating the filtrate under reduced pressure, vacuum filtering, drying the solid, and pulverizing to obtain herba Epimedii extract.
Preferably, icariin and helicase are heated to 40-65 ℃ in a weight ratio of 3-8:1, enzymolysis reaction is carried out for 8-15h, filtration is carried out, the obtained solid is added with absolute ethyl alcohol, stirring is carried out for 1-6h, standing and layering are carried out for 3-8h, the solid is discarded, the filtrate is subjected to reduced pressure concentration and reduced pressure suction filtration, the solid is dried for 5-10h, and crushing is carried out, so as to obtain the epimedium extract.
The liquid phase detection conditions of the epimedium total flavonoids are as follows:
the mobile phase is acetonitrile as a mobile phase A, and water as a mobile phase B; gradient elution, conditions were as follows: 0 → 29min, 25% a; 29 → 30min, 25% A → 41% A; 30 → 55min, 41% A; 55 → 56min, 41% A → 25% A; 56 → 59min, 25% A;
the column temperature is 30 ℃;
the wavelength is 270 nm;
flow rate: 1.0 ml/min.
The liquid phase detection conditions of the icariin are as follows:
liquid phase conditions: the instrument comprises the following steps: agilent 1260;
mobile phase: methanol: 0.1% phosphoric acid water 80: 20;
detection wavelength: 270 nm;
column temperature: 30 ℃;
flow rate: 1.0 ml/min.
The invention relates to an anti-wrinkle composition containing epimedium extract and phellodendron amurense extract, wherein the content of berberine in the phellodendron amurense extract is not lower than 0.5%.
The extraction method of the phellodendron amurense extract comprises the following steps:
pulverizing cortex Phellodendri, soaking in lime water, filtering, adjusting pH, collecting precipitate, washing with water, precipitating with propylene glycol solvent, adjusting to neutrality to obtain cortex Phellodendri extractive solution, concentrating under reduced pressure, vacuum filtering, and drying to obtain cortex Phellodendri extract.
The liquid phase detection conditions of the berberine are as follows:
liquid phase conditions: octadecylsilane chemically bonded silica is used as a filler;
mobile phase: 0.01mol/L ammonium dihydrogen phosphate solution: acetonitrile 75: 25;
detection wavelength: 345 nm.
The anti-wrinkle effect of the skin care product composition is not only obviously superior to the effect of the two components when the two components are used independently, but also superior to the addition of the two effects.
One of the purposes of the invention is to provide a skin care product composition, and the active ingredients of the skin care product composition consist of epimedium extract and phellodendron amurense extract. Through a large number of experiments, the inventor finds that the phellodendron amurense extract and the epimedium extract in the skin care product composition can achieve the synergistic improvement effect of resisting wrinkles. The weight ratio of the phellodendron amurense extract to the epimedium extract in the skin care product composition is 1: (0.01-20), and more preferably, the weight ratio of the phellodendron amurense extract to the epimedium extract in the skin care product composition is 1: (0.05-10).
The active substance components in the skin care product composition comprise 0.1-10% of phellodendron amurense extract and 0.1-10% of epimedium extract by mass percent.
Preferably, the composition also comprises the following components in percentage by mass: 8-15% of grease, 6-20% of humectant, 2-7% of emulsifier, 0.5-2.0% of thickener and the balance of water.
The invention also provides a skin care product containing the skin care product composition, and preferably in the form of the following skin care product: a toner, a skin nutrient solution, a nutrient cream, a massage cream, an essence, a gel cream, a mask, a mascara, a concealer, a lipstick, a lip gloss, or a foundation.
The invention also aims to provide the skin care effect of the skin care product composition, namely the application of the skin care product composition in preparing anti-wrinkle skin care products.
Example 1 of the present invention shows that the composition of the present invention has significant oxygen radical scavenging function and antioxidant activity. Example 2 of the present invention shows that the composition of the present invention can reduce the wrinkle length, wrinkle area, wrinkle depth of the skin, and increase the collagen level of the skin.
The skin care product composition can be clinically used for resisting wrinkles and has a remarkable effect. Clinical trial shows that the anti-wrinkle composition is easy to absorb and good in wrinkle removing effect, fine lines on the face are obviously smoothed after the anti-wrinkle composition is used, and wrinkles are effectively reduced or relieved. The subjects did not have skin allergy, red swelling, and other adverse conditions.
Compared with the prior art, the skin care product composition has the following outstanding advantages in the aspect of anti-wrinkle:
(1) according to the anti-wrinkle composition, the epimedium extract and the phellodendron amurense extract are compounded according to a certain proportion, so that flavonoids of the epimedium extract are combined to promote skin metabolism and the phellodendron amurense extract has an antioxidant effect, aged skin can be repaired in multiple aspects, and a synergistic effect is achieved. Can be applied to the development of anti-wrinkle skin care products.
(2) The invention aims to research a natural anti-wrinkle composition, which can effectively delay aging, is safe and mild, and has no stimulation and side effect on skin.
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FIG. 1 Effect of the compositions of the present invention on photoaging model wrinkle Length
FIG. 2 Effect of the compositions of the present invention on the percent wrinkle area of the photoaging model
FIG. 3 Effect of compositions of the invention on photoaging model wrinkle depth
FIG. 4 Effect of the compositions of the present invention on collagen levels in a model of photoaging
Detailed Description
The present invention will be further described below by way of specific embodiments, but the scope of application of the present invention is not limited to the following examples. Alterations and/or combinations of features of the invention will be apparent to those skilled in the art from the disclosure, spirit and/or scope of the invention, and are intended to be encompassed by the invention.
The raw material sources are as follows:
the epimedium extract is prepared according to the invention.
Phellodendron amurense extract: quzhou City exhibition-macro Biotechnology Ltd.
Formulation example 1
Figure BDA0002693960080000041
Figure BDA0002693960080000051
Formulation example 2
Composition (I) Content (wt%)
Epimedium extract 1.00
Cortex Phellodendri extract 3.00
Glycerol caprylate 0.80
Oil tea seed oil 1.20
Jojoba oil 1.50
Squalane 2.00
Soybean oil 3.00
Sunflower seed oil 0.50
Propylene glycol 3.00
Hyaluronic acid 2.00
Nicotinamide 2.50
Sorbitan fatty acid esters 1.50
Sodium lauryl sulfate 1.00
Xanthan gum 0.50
Cellulose gum 0.20
Purified water Other parts
Total up to 100
Formulation example 3
Figure BDA0002693960080000052
Figure BDA0002693960080000061
Example 1 oxygen radical scavenging functionality of skin care compositions of the present invention
Skin wrinkle formation, hyperpigmentation and skin aging are caused by oxidative stress induced by Reactive Oxygen Species (ROS). Although the skin has a defense mechanism against ROS, excessive exposure to uv light and a polluted environment can lead to oxidative stress, which in turn leads to hyperpigmentation, freckles, dark spots and wrinkle formation. For anti-wrinkle efficacy, oxygen radical scavenging function and antioxidant activity were evaluated.
1.1DPPH method of free radical scavenging assay
To evaluate the anti-oxygen radical efficacy of skin care compositions according to the present invention, a standard method for measuring free radical scavenging, DPPH, was performed.
25.0mg of DPPH was weighed out and diluted with methanol to 1L. Taking 0.2mL of sample solutions of cortex Phellodendri extract, cortex Phellodendri extract and their composition respectively, adding into a tube with plug containing 3.8mL of DPPH methanol solution, and shaking thoroughly. After each test solution reacts with DPPH methanol solution for 30min, the absorbance value at 517nm is detected, and the absorbance Ai of the test solution is measured by taking methanol as a reference. Simultaneously measuring the absorbance Ac of 0.2mL of methanol and 3.8mL of DPPH solution; 0.2mL of phellodendron amurense extract, and absorbance Aj of the composition with 3.8mL of methanol added thereto, respectively. Each group was assayed 3 times in parallel. The oxygen radical clearance was calculated according to the following formula:
K(%)=[1-(Ai-Aj)/Ac]x100%
note: composition 1 group: phellodendron amurense extract: herba Epimedii extract 1: 0.01;
composition 2 group: phellodendron amurense extract: herba Epimedii extract 1: 0.05;
composition 3 group: phellodendron amurense extract: herba Epimedii extract 1: 3;
composition 4 group: phellodendron amurense extract: herba Epimedii extract 1: 10;
composition 5 group: phellodendron amurense extract: herba Epimedii extract at a ratio of 1: 20.
1.2 results of the experiment
TABLE 1 percentage of radical scavenging by compositions to DPPH (%)
Figure BDA0002693960080000071
Experimental results show that the composition has radical scavenging effect obviously superior to that of phellodendron amurense extract group and that of epimedium extract group. The composition 3 group with the dilution factor of 16 has the best effect of scavenging free radicals.
2.1 determination of Total Oxidation resistance
In order to evaluate the antioxidant activity of the skin care composition according to the present invention, an assay using a phosphorus molybdenum complex method was performed.
Sequentially numbering 10mL of graduated test tubes, respectively adding 2.0mL of sample solutions with different concentrations, respectively adding 2.0mL of 0.6mol/L concentrated sulfuric acid, 28mmol/L ammonium molybdate and 4mmol/L sodium phosphate, respectively, uniformly mixing, carrying out water bath at 95 ℃ for 90min, measuring the absorbance at 695nm, carrying out parallel measurement for 3 times at each concentration, and taking the average value. The greater the absorbance, the greater the total antioxidant capacity.
Note: composition 1 group: phellodendron amurense extract: herba Epimedii extract 1: 0.01;
composition 2 group: phellodendron amurense extract: herba Epimedii extract 1: 0.05;
composition 3 group: phellodendron amurense extract: herba Epimedii extract 1: 3;
composition 4 group: phellodendron amurense extract: herba Epimedii extract 1: 10;
composition 5 group: phellodendron amurense extract: herba Epimedii extract at a ratio of 1: 20.
2.2 results of the experiment
TABLE 2 Total antioxidant Capacity of the compositions
Figure BDA0002693960080000072
Figure BDA0002693960080000081
Note: and groupComposition 1 group comparison###P is less than 0.001; compared with composition No. 5&&&P<0.001;
Compared with composition 1¥¥P is less than 0.01; compared with composition No. 5@P<0.05,@@P<0.01;
Compared with composition 3$P<0.05。
Experimental results show that the total antioxidant capacity of each group of the composition is obviously superior to that of a phellodendron amurense extract group and that of an epimedium extract group.
EXAMPLE 2 Effect of the compositions of the present invention on photoaging nude mouse model wrinkles
Facial wrinkles are considered one of the most prominent features of skin aging. Skin aging is generally divided into intrinsic (chronological) aging and extrinsic (photoaging) aging. Extrinsic aging indicates that photoaged skin has rough wrinkles, which are mainly caused by exposure to sunlight including ultraviolet B, while intrinsic aging is caused by genetic factors of aging and forms shallow and smooth wrinkles. A large body of literature demonstrates that aged or wrinkled skin often exhibits loss of skin elasticity and degradation of elastic fibers and collagen. We used measurements of the length, depth and thickness of skin wrinkles and the expression level of collagen fibers to evaluate the anti-wrinkle effect of the test substance.
The experimental scheme is as follows:
the experimental animals are selected from 6-8 weeks old male HR-1 nude mice, and the UVB irradiation conditions are as follows: ultraviolet irradiation was carried out using a UVM-225D Mineralight ultraviolet lamp having an emission wavelength of 302 nm.
And coating the object to be tested while irradiating. The test period was 8 weeks.
Week 1: 60mJ/cm2For 200s, 3 times a week (one minimal erythemal dose);
week 2-3: 120mJ/cm2Lasting for 400s, 3 times a week;
week 4-5: 180mJ/cm2Lasting for 600s, 3 times a week;
week 6-8: 240mJ/cm2Lasting for 800s, 3 times a week;
the day after the experiment, 0.7%Pentobarbital sodium is injected into the abdominal cavity of an anesthetized animal, a skin image of a test area is captured,
Figure BDA0002693960080000082
VL 650 analysis of skin wrinkle depth and length; taking down the skin of the test area, and measuring the thickness of the epidermis by using a microscope with an ocular lens and a micrometer; the other part was fixed in 4% paraformaldehyde, sectioned, observed by Masson staining and counted for collgen expression levels.
Note: composition 1 group: phellodendron amurense extract: herba Epimedii extract 1: 0.01;
composition 2 group: phellodendron amurense extract: herba Epimedii extract 1: 0.05;
composition 3 group: phellodendron amurense extract: herba Epimedii extract 1: 3;
composition 4 group: phellodendron amurense extract: herba Epimedii extract 1: 10;
composition 5 group: phellodendron amurense extract: herba Epimedii extract at a ratio of 1: 20.
The results are shown in FIGS. 1-4.
In figure 1, note that: compared with the normal group***P is less than 0.001; compared with model group#P<0.05,##P<0.01,###P is less than 0.001; 1 ratio of composition
Figure BDA0002693960080000092
In contrast to the composition 3, the composition,&&&p is less than 0.001; compared with composition 5ψP<0.05。
Fig. 1 shows that the skincare composition of phellodendron amurense extract and epimedium extract can reduce the length of skin wrinkles of a photo-oxidation nude mouse model, and the length efficacy of the phellodendron amurense extract and epimedium extract skincare composition for reducing skin wrinkles is obviously superior to that of a phellodendron amurense extract group and that of an epimedium extract group.
FIG. 2 shows: compared with the normal group***P is less than 0.001; compared with model group#P<0.05,##P<0.01,###P is less than 0.001; 1 ratio of composition
Figure BDA0002693960080000091
In contrast to the composition 3, the composition,&&&p is less than 0.001; compared with composition 5ψψP<0.01。
Fig. 2 shows that the skincare composition of phellodendron amurense extract and epimedium extract can reduce the area of skin wrinkles of a photo-oxidation nude mouse model, and the skincare composition of phellodendron amurense extract and epimedium extract has obviously better effect of reducing the area of skin wrinkles than the phellodendron amurense extract group and the epimedium extract group.
FIG. 3 shows: compared with the normal group***P is less than 0.001; compared with model group#P<0.05,##P<0.01,###P is less than 0.001; 1 ratio of composition
Figure BDA0002693960080000093
In contrast to the composition 3, the composition,&&&p is less than 0.001; compared with composition 5ψP<0.05。
Fig. 3 shows that the skincare composition of phellodendron amurense extract and epimedium extract can reduce the depth of skin wrinkles of a photo-oxidation nude mouse model, and the skincare composition of phellodendron amurense extract and epimedium extract has obviously better skin wrinkle reducing effect than the phellodendron amurense extract group and the epimedium extract group.
FIG. 4 shows: compared with the normal group***P is less than 0.001; compared with model group#P<0.05,##P<0.01,###P is less than 0.001; 1 ratio of composition
Figure BDA0002693960080000094
In contrast to the composition 3, the composition,&&&p is less than 0.001; compared with composition 5ψP<0.05,ψψP<0.01。
Fig. 4 shows that the cortex phellodendri extract and herba epimedii extract skin care product composition can improve the skin collagen level of a photooxidation nude mouse model, and the effect of the cortex phellodendri extract and herba epimedii extract skin care product composition on improving the skin collagen level is obviously superior to that of a cortex phellodendri extract group and that of an herba epimedii extract group.
The experimental results show that the anti-wrinkle effect of each group of the composition is obviously superior to that of a phellodendron amurense extract group and that of an epimedium extract group.
Example 3 anti-wrinkle Effect of the anti-wrinkle skin Care article of the present invention
1. General data
50 people of 35-45 years old are selected to participate in the method voluntarily, and healthy women have no wound, no skin disease, no infectious disease and no long-term medicine taking history.
Sex: female, the female is provided with a drug.
Age: 35-45 years old.
2. Treatment course and application method
The course of treatment is as follows: four weeks is a course of treatment.
The using method comprises the following steps: the anti-wrinkle composition of the application formula example 2 is used for 1 time respectively after face cleaning in the morning and evening every day, and is continuously used for eight weeks.
The forehead wrinkles before use were used as a control group, and the forehead wrinkles after eight weeks were used continuously as a sample group.
Anti-wrinkle effect determination criteria:
the effect is excellent: compared with the wrinkle before use, the wrinkle subsides more than 90%, and is obviously improved.
The effect is shown: compared with the wrinkle before use, the wrinkle is removed by 70-90 percent and obviously improved.
The method has the following advantages: wrinkles resolved 30-70% compared to before use, but still a few wrinkles were present, improving.
And (4) invalidation: wrinkles resolved by less than 30% without improvement compared to before use.
3. The anti-wrinkle results are shown in table 2.
The course of treatment is as follows: the treatment course has excellent effect in 12 cases, 20 cases with obvious effect, 11 cases with effect and 7 cases with no effect.
TABLE 3 anti-wrinkle Effect of the anti-wrinkle composition of the present invention
Figure BDA0002693960080000101
4. Conclusion
The anti-wrinkle composition in the formula example 2 has high acceptance, trial volunteers show that the face cream is easy to absorb and has good wrinkle removing effect, fine lines on the face are obviously smoothed after the composition is used for 8 weeks, and wrinkles are effectively reduced or relieved. The subjects did not have skin allergy, red swelling, and other adverse conditions.
The skin care product composition disclosed by the invention has an oxygen radical removing function and antioxidant activity, reduces the length, the area and the depth of wrinkles of the skin, improves the collagen level of the skin, and enables the skin to be smooth, plump, tight and fine.

Claims (10)

1. A composition comprising the following components: phellodendron amurense extract and epimedium extract.
2. The composition of claim 1, wherein the weight ratio of phellodendron amurense extract to epimedium extract is 1: (0.01-20).
3. The composition of claim 2, wherein the weight ratio of phellodendron amurense extract to epimedium extract is 1: (0.05-10).
4. The composition of claim 1, wherein the epimedium extract has a total flavonoids content of not less than 50% and an aglycon content of not less than 35% as determined by liquid phase assay.
5. The composition of claim 1, wherein the content of berberine extract of phellodendron amurense is not less than 0.5%.
6. A skin care composition containing the composition of claim 1, wherein the active substance component and the mass percentage of the skin care composition are 0.1-10% of phellodendron amurense extract and 0.1-10% of epimedium extract.
7. The skin care composition of claim 5, further comprising the following components in mass percent: 8-15% of grease, 6-20% of humectant, 2-7% of emulsifier, 0.5-2.0% of thickener and the balance of water.
8. Use of a composition according to any one of claims 1 to 7 for the preparation of an anti-wrinkle skin care product.
9. The use according to claim 8, wherein the skin care product is in the form of a toner, skin tonic, nourishing cream, massage cream, essence, gel cream, mask, mascara, concealer, lipstick, lip gloss, or foundation.
10. Use according to claim 9, wherein the skin care product is in the form of a lotion, cream or mask.
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