CN112545963A - Composition with whitening effect, whitening compound preparation and preparation method of whitening compound preparation - Google Patents
Composition with whitening effect, whitening compound preparation and preparation method of whitening compound preparation Download PDFInfo
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- CN112545963A CN112545963A CN202011614211.6A CN202011614211A CN112545963A CN 112545963 A CN112545963 A CN 112545963A CN 202011614211 A CN202011614211 A CN 202011614211A CN 112545963 A CN112545963 A CN 112545963A
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- CN
- China
- Prior art keywords
- whitening
- parts
- stirring
- pterostilbene
- composition
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- 230000002087 whitening effect Effects 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 84
- 239000000203 mixture Substances 0.000 title claims abstract description 52
- 150000001875 compounds Chemical class 0.000 title claims abstract description 29
- VLEUZFDZJKSGMX-ONEGZZNKSA-N pterostilbene Chemical compound COC1=CC(OC)=CC(\C=C\C=2C=CC(O)=CC=2)=C1 VLEUZFDZJKSGMX-ONEGZZNKSA-N 0.000 claims abstract description 51
- VLEUZFDZJKSGMX-UHFFFAOYSA-N pterostilbene Natural products COC1=CC(OC)=CC(C=CC=2C=CC(O)=CC=2)=C1 VLEUZFDZJKSGMX-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000463 material Substances 0.000 claims abstract description 43
- 238000003756 stirring Methods 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000012071 phase Substances 0.000 claims abstract description 33
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 229910001868 water Inorganic materials 0.000 claims abstract description 21
- ZGSCRDSBTNQPMS-UJURSFKZSA-N 3-O-Ethylascorbic acid Chemical compound CCOC1=C(O)C(=O)O[C@@H]1[C@@H](O)CO ZGSCRDSBTNQPMS-UJURSFKZSA-N 0.000 claims abstract description 13
- 229940120145 3-o-ethylascorbic acid Drugs 0.000 claims abstract description 12
- 235000020415 coconut juice Nutrition 0.000 claims abstract description 9
- 239000008346 aqueous phase Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 51
- 229920000858 Cyclodextrin Polymers 0.000 claims description 39
- 239000002131 composite material Substances 0.000 claims description 32
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 30
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- 239000000243 solution Substances 0.000 claims description 18
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- 238000000034 method Methods 0.000 claims description 15
- -1 3, 5-dihydroxyphenyl Chemical group 0.000 claims description 14
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 7
- 229940010747 sodium hyaluronate Drugs 0.000 claims description 7
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 claims description 7
- 239000004475 Arginine Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 5
- OWBTYPJTUOEWEK-UHFFFAOYSA-N butane-2,3-diol Chemical compound CC(O)C(C)O OWBTYPJTUOEWEK-UHFFFAOYSA-N 0.000 claims description 5
- 125000002801 octanoyl group Chemical group C(CCCCCCC)(=O)* 0.000 claims description 5
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- 229960004705 kojic acid Drugs 0.000 description 5
- WZNJWVWKTVETCG-UHFFFAOYSA-N kojic acid Natural products OC(=O)C(N)CN1C=CC(=O)C(O)=C1 WZNJWVWKTVETCG-UHFFFAOYSA-N 0.000 description 5
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
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- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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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
- A61K8/60—Sugars; Derivatives thereof
- A61K8/602—Glycosides, e.g. rutin
-
- 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
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
-
- 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
- A61K8/73—Polysaccharides
- A61K8/738—Cyclodextrins
-
- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9794—Liliopsida [monocotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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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
- A61K2800/10—General cosmetic use
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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
- A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Birds (AREA)
- Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Dermatology (AREA)
- Cosmetics (AREA)
Abstract
The application relates to the technical field of skin care products, and particularly discloses a composition with a whitening effect, a whitening compound preparation and a preparation method of the whitening compound preparation. The composition with whitening effect comprises salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut juice according to the weight ratio of (5.8-6.2), (2.8-3.2) and 1. The whitening compound preparation comprises the following components in parts by weight: 58.55-89.35 parts of an aqueous phase material; 1.5-3.5 parts of oil phase materials; 6.8-9.5 parts of composition with whitening effect; 0.497 to 0.85 part of low-temperature material; the preparation method comprises the following steps: mixing the water phase and oil phase, adding the composition with whitening effect and the low temperature material, and stirring. The active ingredient compounding is carried out on various inducers based on a multi-channel whitening mechanism, and the long-acting whitening effect is achieved.
Description
Technical Field
The application relates to the technical field of skin care products, in particular to a composition with a whitening effect, a whitening compound preparation and a preparation method of the whitening compound preparation.
Background
The skin is the largest organ of the human body and is distributed in various parts of the human body. There are many factors that affect the appearance and appeal of skin, such as water tenderness, smoothness, etc., of which the factor of greatest concern or influence is skin pigmentation, i.e., the skin color. The difference of human skin color is mainly influenced by melanin, and the content and distribution of the melanin in the skin determine the color of human skin. Tyrosinase is the rate-limiting enzyme for melanin synthesis, and inhibition of tyrosinase activity is one of the main targets for inhibiting melanin formation. When the body produces excessive melanin, it may cause skin spots or changes in skin color, a condition known as hyperpigmentation.
At present, the conventional external preparations mainly suppress tyrosinase activity and melanocyte activity to solve the pigmentation problem. For example, the external preparation containing hydroquinone, retinoic acid, kojic acid and the like as main components has obvious whitening effect in a short period.
In view of the above-mentioned related art, the pigmentation is multi-causative, and improvement only from tyrosinase and melanocytes fails to achieve a long-lasting whitening effect.
Disclosure of Invention
In order to start from a multi-channel whitening mechanism, active ingredients are compounded according to various inducers, so that the skin care product with long-acting whitening effect is obtained. The application provides a composition with a whitening effect, a whitening compound preparation and a preparation method of the whitening compound preparation.
In a first aspect, the present application provides a composition with whitening effect, which adopts the following technical scheme:
a composition with whitening effect comprises salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut juice, wherein the weight ratio of salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut juice is (5.8-6.2): 2.8-3.2): 1;
the above-mentionedSalidroside-plus is 2- (3, 5-dihydroxyphenyl) ethyl-beta-D-glucoside, and the molecular formula is as follows: c13H18O8The structural formula is as follows:
by adopting the technical scheme, salidroside-plus takes P4HB as a target point, regulates ubiquitination degradation of IRF1 to regulate melanin generation, and simultaneously inhibits inflammatory factor release to resist inflammation, thereby regulating melanin generation from the source. The added pterostilbene inhibits the maturation of tyrosinase, resists inflammation by inhibiting the activation capability of nuclear factor NF-kB, and improves the tolerance of skin and relieves stimulation by reducing oxidative stress reaction. The 3-O-ethyl ascorbic acid ether has better DPPH and ABTS free radical scavenging capacity, can reduce the generated melanin, and has super-strong antioxidation. The organic acid in coconut fruit powder is used for promoting the division of melanocyte, accelerating the transport metabolism of melanosome and having small mild irritation. After the four components are reasonably mixed, the pigmentation can be effectively relieved, the skin color can be uniformly improved, and meanwhile, the used components are mild, have no stimulation and have no stimulation to the skin. Salidroside-plus is preferably used, and has better melanin formation inhibiting ability and can obviously inhibit the generation of melanin compared with salidroside, so that the product has better whitening effect, and meanwhile, the salidroside-plus also has better anti-inflammatory ability.
In a second aspect, the application provides a whitening compound preparation, which adopts the following technical scheme:
a whitening compound preparation comprises the following components in parts by weight:
58.55-89.35 parts of an aqueous phase material;
1.5-3.5 parts of oil phase materials;
6.8-9.5 parts of composition with whitening effect;
0.497-0.85 parts of low-temperature material.
By adopting the technical scheme, the prepared whitening compound preparation provides safe, long-acting and side-effect-free whitening effects through an all-around and multi-path whitening mechanism, and meanwhile, has better stability, cold resistance and heat resistance.
Preferably, the aqueous phase material comprises the following components in parts by weight:
0.15-0.25 part of acrylic acid (ester)/C10-30 alkanol acrylate crosslinked polymer;
55-85 parts of deionized water;
3-3.5 parts of glycerol;
0.05-0.1 part of sodium hyaluronate;
0.35-0.5 part of p-hydroxyacetophenone.
By adopting the technical scheme, glycerin and sodium hyaluronate are used as a humectant to play a role in keeping moisture, and the acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer is a better emulsion stabilizer of the skin care product, so that the stability of the system can be improved. The added p-hydroxyacetophenone as antiseptic is naturally present in stems and leaves of Compositae plants, and has no irritation to skin.
Preferably, the aqueous phase material is prepared by the following steps:
a1, adding acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer into deionized water, and stirring to obtain a first premix;
a2, mixing sodium hyaluronate with glycerol, and stirring to obtain a second premix;
a3, adding p-hydroxyacetophenone into the first premix, heating to dissolve, adding the second premix, and stirring to obtain the water-phase material.
By adopting the technical scheme, the water phase material is prepared by mixing in steps, so that all the components can be fully dissolved and mixed, and the obtained water phase material is uniform in texture and has better moisturizing and hydrating effects.
Preferably, the oil phase material comprises the following components in parts by weight:
0.5-1.5 parts of polydimethylsiloxane;
0.5-1 part of PEG-20 methyl glucose sesquistearate;
0.5-1 part of chinaroot greenbrier seed oil.
Preferably, the oil phase material is prepared by the following steps: heating and dissolving PEG-20 methyl glucose sesquistearate and polydimethylsiloxane, adding white Potentilla chinensis seed oil, stirring and mixing to obtain oil phase material.
By adopting the technical scheme, PEG-20 methyl glucose sesquistearate and polydimethylsiloxane are dissolved and mixed at a proper temperature, and then the white chinaroot herb oil is added and mixed to form an oil phase material. The meadowfoam seed oil contains more than 98% of long-chain fatty acid, has extremely strong stability, increases the stability of oil phase materials, thereby effectively prolonging the quality guarantee period of the whitening composite preparation, and is also an excellent emollient.
Preferably, the low-temperature material comprises the following components in parts by weight:
0.05-0.075 part of caprylyl hydroximic acid;
0.017-0.025 parts of glycerol caprylate;
0.28-0.5 part of methyl propylene glycol;
0.15-0.25 part of arginine.
By adopting the technical scheme, the caprylyl hydroximic acid, the glyceryl caprylate and the methyl propylene glycol have a good stabilizing effect on essence prepared by mixing the water phase material and the oil phase material, the composite preparation can be safely used within a shelf life and has good stability, and the added arginine is used for adjusting the pH value.
In a third aspect, the application provides a preparation method of a whitening compound preparation, which adopts the following technical scheme:
a preparation method of a whitening compound preparation comprises the following steps:
s1, mixing the water phase material and the oil phase material, homogenizing and stirring to obtain essence;
s2, adding the composition with the whitening effect and the low-temperature material into the essence, and stirring to obtain the whitening compound preparation.
By adopting the technical scheme, the preparation method provided by the application is used for compounding multiple inducers influencing pigmentation, the preparation process is safe and effective, the whitening compound preparation can be stably prepared, the process is simple, and the preparation method is suitable for large-scale industrial production.
Preferably, the salidroside-plus and the pterostilbene are pretreated before being added,
the pretreatment process of the salidroside-plus comprises the following steps: dissolving cyclodextrin in water to obtain cyclodextrin saturated solution, setting the dissolving temperature at 40-50 deg.C, adding salidroside-plus into the cyclodextrin saturated solution, stirring for 3-4 hr, filtering, and drying to obtain the final product; the pretreatment process of pterostilbene is as follows: dissolving cyclodextrin in water to obtain cyclodextrin saturated solution, setting the dissolving temperature at 40-50 deg.C, adding pterostilbene into ethanol to obtain pterostilbene ethanol solution, adding pterostilbene ethanol solution into cyclodextrin saturated solution, stirring for 3-4 hr, filtering, and drying.
By adopting the technical scheme, the raw materials are subjected to cyclodextrin coating treatment, so that the solubility of the raw materials is improved, and the utilization rate is improved; the stability of the raw material components is improved; preventing volatile components from being emitted; reducing irritation and toxicity to skin. The salidroside-plus is subjected to cyclodextrin encapsulation treatment, so that the stability of the salidroside-plus can be improved, the salidroside-plus is not easy to separate out, and the salidroside-plus has a slow release effect. The water solubility of pterostilbene is poor, the water solubility of pterostilbene is improved after the pterostilbene is wrapped by cyclodextrin, the pterostilbene is easy to add into products such as skin lotion, emulsion, essence, facial mask, cream and the like, is not easy to separate out, has good stability, and has a slow release effect.
Preferably, in the S1, the mixing temperature is set to 75-85 ℃, the homogenizing rotation speed is set to 5000-6000rpm, and the homogenizing time is set to 5-10 min; in the S2, the stirring temperature is set to 40-45 ℃.
By adopting the technical scheme, the whitening compound preparation is prepared under the condition range, so that the uniform dispersibility of the raw material components in a mixed system is improved, and the prepared whitening compound preparation has a good long-acting whitening effect.
In summary, the present application has the following beneficial effects:
1. the composition with the whitening effect provides the safe, long-acting and non-side effect whitening effect through an all-round and multi-path whitening mechanism, realizes the effective co-dissolution of salidroside PLUS, pterostilbene, 3-O-ethyl ascorbic acid ether and coconut fruit powder, and acts on the whole generation process of melanin, so that the generation of the melanin, the transportation and the metabolism of the melanin are effectively regulated and controlled;
2. according to the application, the salidroside-plus and the pterostilbene are wrapped by the cyclodextrin before mixing by using a cyclodextrin inclusion technology, so that the stability of the salidroside-plus is improved, the salidroside-plus is not easy to precipitate during use, the defect of poor water solubility of the pterostilbene is improved, and the salidroside-plus can be easily added into various skin care products;
3. the preparation method is simple, safe and effective in preparation process, can be used for stably preparing the whitening compound preparation, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a graph showing the results of the first test in the performance test of the present application.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples.
The 3-O-ethyl ascorbyl ether in the examples of the present application was taken from Hubei Xin Mingtai chemical Co., Ltd; pterostilbene was taken from sigma aldrich trade ltd; acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer is obtained from Beijing Huameili biochemical engineering; the glycerol is produced by Baomeile company; sodium hyaluronate is produced biologically in focus; p-hydroxyacetophenone is produced by Dexinxin under the trade name Symsave H; polydimethylsiloxane, manufactured by shin-Etsu corporation of Japan, under the trade name KF-56A-6 CS; PEG-20 methyl glucose sesquistearate is available from Lubrizol under the trade name Glucamate SSE-20; the meadowfoam seed oil is produced by Henry company of Germany; caprylyl hydroximic acid, glyceryl caprylate and methyl propylene glycol are produced by Guangzhou Ezepine Biotechnology, Inc.; arginine is produced by Emei mountain Longteng Biotech limited; the phosphate buffer solution is collected from Nanchang rain and dew experimental equipment, Inc.; trypsin is produced by Solarbio.
The constant temperature heating magnetic stirrer is made by Shanghai Yinying instruments Co., Ltd, and has the model of DF-101S; the microplate reader assay was obtained from the Megastic molecular instruments (Shanghai) Inc. under the model SpectraMax iD 5.
Examples
Example 1: a composition with whitening effect comprises salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut fruit juice. Salidroside-plus is 2- (3, 5-dihydroxyphenyl) ethyl-beta-D-glucoside, and the molecular formula is as follows: c13H18O8The structural formula is as follows:
wherein the weight ratio of salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut juice is 5.8: 5.8: 2.8: 1, and is prepared by the following steps:
s1, stirring and mixing salidroside-plus and pterostilbene for 5min by using a constant-temperature heating magnetic stirrer, wherein the stirring temperature is set to 40 ℃, and the stirring speed is set to 60rpm, so as to obtain a mixture A;
s2, adding 3-O-ethyl ascorbic acid ether and coconut juice into the mixture A, stirring and mixing for 20min, setting the stirring temperature at 60 ℃ and the stirring speed at 120rpm, and discharging.
Example 2: a composition having whitening effects, which is different from example 1 in that the weight ratio of salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut juice in the composition having whitening effects is 6:6:3: 1.
Example 3: a composition having whitening effects, which is different from example 1 in that the weight ratio of salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut juice in the composition having whitening effects is 6.2: 6.2: 3.2: 1.
example 4: a composition having a whitening effect, which is different from example 2 in that salidroside-plus and pterostilbene are both pre-treated before being added in the preparation process of the composition having a whitening effect.
The pretreatment process of salidroside-plus is as follows: dissolving 1.8g of beta-cyclodextrin in 50g of deionized water to prepare a cyclodextrin saturated solution, setting the dissolving temperature to be 40 ℃, adding salidroside-plus into the cyclodextrin saturated solution, stirring for 3 hours at the rotating speed of 220rpm at the temperature of 40 ℃ by using a constant-temperature heating magnetic stirrer, filtering, and drying to obtain the salidroside-plus-cyclodextrin saturated solution.
The pretreatment process of pterostilbene is as follows: dissolving 1.8g of beta-cyclodextrin in 50g of deionized water to prepare a cyclodextrin saturated solution, setting the dissolving temperature at 40 ℃, adding pterostilbene into 10g of 40% ethanol solution to prepare a pterostilbene ethanol solution, adding the pterostilbene ethanol solution into the cyclodextrin saturated solution, stirring for 3 hours at the rotating speed of 220rpm at the temperature of 40 ℃ by using a constant-temperature heating magnetic stirrer, filtering, and drying to obtain the pterostilbene ethanol solution.
Example 5: a composition having a whitening effect, which is different from example 2 in that salidroside-plus and pterostilbene are both pre-treated before being added in the preparation process of the composition having a whitening effect.
The pretreatment process of salidroside-plus is as follows: dissolving 1.8g of beta-cyclodextrin in 50g of deionized water to prepare a cyclodextrin saturated solution, setting the dissolving temperature at 45 ℃, adding salidroside-plus into the cyclodextrin saturated solution, stirring for 3.5 hours at the rotating speed of 220rpm by using a constant-temperature heating magnetic stirrer at the temperature of 45 ℃, filtering, and drying to obtain the salidroside-plus-cyclodextrin saturated solution.
The pretreatment process of pterostilbene is as follows: dissolving 1.8g of beta-cyclodextrin in 50g of deionized water to prepare a cyclodextrin saturated solution, setting the dissolving temperature at 45 ℃, adding pterostilbene into 10g of 40% ethanol solution to prepare a pterostilbene ethanol solution, adding the pterostilbene ethanol solution into the cyclodextrin saturated solution, stirring for 3.5 hours at the rotating speed of 220rpm at the temperature of 45 ℃ by using a constant-temperature heating magnetic stirrer, filtering, and drying to obtain the pterostilbene ethanol-based composite material.
Example 6: a composition having a whitening effect, which is different from example 2 in that salidroside-plus and pterostilbene are both pre-treated before being added in the preparation process of the composition having a whitening effect.
The pretreatment process of salidroside-plus is as follows: dissolving 1.8g of beta-cyclodextrin in 50g of deionized water to prepare a cyclodextrin saturated solution, setting the dissolving temperature to 50 ℃, adding salidroside-plus into the cyclodextrin saturated solution, stirring for 4 hours at the rotation speed of 220rpm at the temperature of 50 ℃ by using a constant-temperature heating magnetic stirrer, filtering, and drying to obtain the salidroside-plus-cyclodextrin saturated solution.
The pretreatment process of pterostilbene is as follows: dissolving 1.8g of beta-cyclodextrin in 50g of deionized water to prepare a cyclodextrin saturated solution, setting the dissolving temperature at 50 ℃, adding pterostilbene into 10g of 40% ethanol solution to prepare a pterostilbene ethanol solution, adding the pterostilbene ethanol solution into the cyclodextrin saturated solution, stirring for 4 hours at the rotation speed of 220rpm at the temperature of 50 ℃ by using a constant-temperature heating magnetic stirrer, filtering, and drying to obtain the pterostilbene ethanol solution.
Example 7: a whitening compound preparation is prepared by the following steps of:
s1, mixing half of the water phase materials with all the oil phase materials at 75 ℃, adding the rest half of the water phase materials, and homogenizing and stirring at 5000rpm for 5min to obtain essence;
s2, sequentially adding the composition with the whitening effect, caprylyl hydroximic acid, glyceryl caprylate and methyl propylene glycol into the essence at 40 ℃, stirring for 10min, then adding arginine, stirring for 5min, and sieving with a 200-mesh sieve to obtain the whitening compound preparation.
Wherein the water phase material is prepared by the following steps:
a1, adding acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer into deionized water, and stirring for 10min to obtain a first premix;
a2, mixing sodium hyaluronate with glycerol, and stirring for 10min to obtain a second premix;
a3, adding p-hydroxyacetophenone into the first premix at 80 deg.C to dissolve, adding the second premix, and stirring for 10min to obtain water phase material.
The oil phase material is prepared by the following steps: dissolving PEG-20 methyl glucose sesquistearate and polydimethylsiloxane at 65 deg.C, adding white Potentilla seed oil, stirring and mixing for 5min to obtain oil phase material.
The composition having a whitening effect was prepared as in example 1.
Examples 8 to 9: a whitening composite preparation, which is different from example 1 in that each component and the corresponding weight thereof are shown in table 1.
TABLE 1 Components and weights (g) of examples 7-9
Example 10: a whitening composite preparation, which is different from example 7 in that the composition having a whitening effect was prepared as in example 2.
Example 11: a whitening composite preparation, which is different from example 7 in that the composition having a whitening effect was prepared as in example 3.
Example 12: a whitening composite preparation, which is different from example 7 in that the composition having a whitening effect was prepared as in example 4.
Example 13: a whitening composite preparation, which is different from example 7 in that the composition having a whitening effect was prepared as in example 5.
Example 14: a whitening composite preparation, which is different from example 7 in that the composition having a whitening effect was prepared as in example 6.
Example 15: a whitening compound preparation, which is different from the whitening compound preparation in the embodiment 1 in that in the preparation process of the whitening compound preparation, the mixing temperature in S1 is set to be 80 ℃, the mean rotating speed is set to be 5500rpm, and the homogenization time is set to be 8 min; the stirring temperature was set to 43 ℃ in S2.
Example 16: a whitening composite preparation, which is different from the whitening composite preparation in the embodiment 1, in the preparation process of the whitening composite preparation, the mixing temperature in S1 is set to be 85 ℃, the mean rotating speed is set to be 6000rpm, and the homogenizing time is set to be 10 min; the stirring temperature was set to 45 ℃ in S2.
Comparative example
Comparative example 1: a composition which differs from example 1 in that the weight ratio of salidroside-plus, 3-O-ethyl ascorbyl ether, pterostilbene and coconut fruit juice in the composition is 7: 6.5: 2: 1.5.
comparative example 2: a composition which differs from example 1 in that the weight ratio of salidroside-plus, 3-O-ethyl ascorbyl ether, pterostilbene and coconut fruit juice in the composition is 4: 3: 6: 1.
comparative example 3: a complex formulation, which is different from example 8 in that salidroside, whose molecular formula is: c14H20O7The structural formula is as follows:
comparative example 4: a composite preparation, which is different from example 8 in that kojic acid is used instead of the composition having a whitening effect during the preparation of the composite preparation.
Comparative example 5: a composite preparation, which is different from example 8 in that the mixing temperature in S1 is set to 60 ℃, the homogenizing speed is set to 4000rpm, and the homogenizing time is set to 3min during the preparation process of the composite preparation; the stirring temperature was set to 35 ℃ in S2.
Comparative example 6: a composite preparation, which is different from example 8 in that the mixing temperature in S1 is set to 90 ℃, the mean rotation speed is set to 6500rpm, and the homogenization time is set to 15min during the preparation process of the composite preparation; the stirring temperature was set to 50 ℃ in S2.
Performance test
Test one:
the compositions prepared in examples 1-6 and comparative examples 1-2 were used as test objects, respectively, and dissolved in deionized water to prepare 10mg/mL of sample solution to be tested.
Setting a control group, wherein in the control group 1, the sample solution to be detected is kojic acid solution of 10 mg/mL;
control group 2: the sample solution to be detected is deionized water.
The test is carried out by selecting human melanocytes, and the human melanocytes are inoculated on a 96-well plate, wherein the plating density is 5000 cells/well. After the cells adhere to the wall, the culture medium is added with nerve factors to induce the generation of the simulated melanin in vivo, and simultaneously UV induces the activation of the melanocytes. Selecting 10 groups of samples, setting 5 times for each group of samples, respectively adding 25 μ L of the sample solution to be tested in examples 1-6, comparative examples 1-2 and control groups 1-2, adding the same sample solution to be tested in the same group, and adding 5% CO at 37 deg.C2The constant temperature and humidity incubator continues to culture for 60 h. The cells were washed with pre-chilled phosphate buffer, then trypsinized, the plates were centrifuged and the supernatant discarded, the cells were lysed with 10% dimethyl sulfoxide in NaOH (1mol/L), and the melanin granules were completely lysed in a 65 ℃ water bath using an microplate reader to detect absorbance at 490 nm. Finally, the melanin content was fed back at this value. The test results are shown in fig. 1.
Referring to fig. 1, the whitening composition prepared in examples 1 to 6 has the best melanin inhibitory activity among human melanocytes, and examples 2 and 5 are the most preferred examples, which illustrate that the preferred weight ratio of salidroside-plus, 3-O-ethyl ascorbate ether, pterostilbene and coconut fruit powder is (5.8-6.2): (2.8-3.2):1, wherein the most preferred weight ratio is 6:6:3: 1. Meanwhile, salidroside-plus and pterostilbene are wrapped by cyclodextrin, so that the melanin inhibitory activity of the composition can be remarkably improved.
And (2) test II:
the compositions prepared in examples 1-6 and comparative examples 1-2 were used as test objects, respectively, and dissolved in deionized water to prepare 10mg/mL of sample solution to be tested.
Setting a control group, wherein in the control group 1, the sample solution to be detected is kojic acid solution of 10 mg/mL;
control group 2: the sample solution to be detected is deionized water.
Mouse melanoma B16 cells were cultured, and when the cells grew to log phase, they were digested with 0.25% trypsin, adjusted to a cell concentration of 5X 105 cells/mL, and seeded in a 96-well plate at 100. mu.L per well. Placing in incubator at 37 deg.C and 5% CO2After culturing for 24 hours under the conditions of (1) and (2), the supernatant was discarded, and the sample solutions to be tested in examples 1 to 6, comparative examples 1 to 2, and control groups 1 to 2 were added. After 72h incubation, the supernatant was discarded, washed 2 times with PBS buffer, 100. mu.L/well fresh medium and 10. mu.L/well CCK-8 solution were added, returned to the cell incubator, and after 1h, A450 was measured. And (3) repeating the holes in each group, wherein the content of the added sample solution to be tested is 10 mu L, 30 mu L and 50 mu L in sequence, the test is repeated for 3 times, and the test result is averaged.
Cell proliferation = (mean absorbance of test sample/mean absorbance of control 2) × 100, and results for each group were averaged and are shown in table 2 below.
As can be seen from the data of table 2, the compositions prepared in examples 1 to 6 are significantly more toxic to cells than comparative examples 1 to 2 and control 1, and thus the whitening composition provided by the present invention has good safety.
TABLE 2 cell proliferation Rate test results
And (3) test III:
the composite preparations obtained in examples 7 to 16 and comparative examples 3 to 6 were used as test objects, each of the examples or comparative examples was sampled 6 times at 50g each time and placed in a clean beaker, 6 samples obtained in the same examples or comparative examples were subjected to stability test under high and low temperature cycles of 25 ℃, 45 ℃, 4 ℃, 18 ℃, 45 ℃ and-18 ℃ and light irradiation, and the stability of the preparations after 30d, 60d and 90d was examined and the examination results were recorded as pass and fail and shown in the following tables 3 and 4.
As can be seen from the test data in tables 3 and 4: the whitening compound preparations prepared in the embodiments 1 to 11 have no phase separation, no change of smell, pH and color after 90 days under the conditions of high and low temperature circulation and illumination at 25 ℃, 45 ℃, 4 ℃, 18 ℃, 45 ℃ and 18 ℃ below zero, and have good stability.
Table 325 ℃, 45 ℃ and 4 ℃ stability test results
TABLE 4-18 deg.C, high and low temperature cycle, stability under illumination test results
And (4) testing:
the composite preparations prepared in example 10, example 13 and comparative example 4 were used as test subjects, 40 qualified volunteers were selected as test subjects to participate in the test by screening questionnaires and preliminary screening of original values of the volunteers, and were randomly divided into 4 groups of 10 subjects. Test samples were randomly distributed by the test staff, one set dispensing the whitening complex formulation prepared in example 10, one set dispensing the whitening complex formulation prepared in example 13, one set dispensing the complex formulation prepared in comparative example 4, and the remaining set using deionized water as a blank. The skin melanin bottom value was measured before applying the skin melanin bottom value on day 1, and then the skin melanin value was measured every 1 week for 4 weeks, and the results of the measurements in the same group were averaged and recorded in the following table 5.
As can be seen from the test data in table 5: the whitening composite preparations prepared in examples 10 and 13 were superior to the composite preparation in comparative example 4, which contains kojic acid as a whitening ingredient, in the effect of significantly improving the skin melanin pigmentation, and the whitening composite preparation of the present application was found to have excellent safety, no sensitization, and irritation by the questionnaire on 20 volunteers who used the whitening composite preparations prepared in examples 10 and 13.
TABLE 5 results of melanin value measurements
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A composition with whitening effect is characterized by comprising salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut juice, wherein the weight ratio of salidroside-plus, 3-O-ethyl ascorbic acid ether, pterostilbene and coconut juice is (5.8-6.2): 2.8-3.2): 1;
the salidroside-plus is 2- (3, 5-dihydroxyphenyl) ethyl-beta-D-glucoside, and the molecular formula is as follows: c13H18O8The structural formula is as follows:
2. a whitening compound preparation comprising the composition with whitening effect of claim 1 is characterized by comprising the following components in parts by weight:
58.55-89.35 parts of an aqueous phase material;
1.5-3.5 parts of oil phase materials;
6.8-9.5 parts of composition with whitening effect;
0.497-0.85 parts of low-temperature material.
3. The whitening composite preparation according to claim 2, wherein the water phase material comprises the following components in parts by weight:
0.15-0.25 part of acrylic acid (ester)/C10-30 alkanol acrylate crosslinked polymer;
55-85 parts of deionized water;
3-3.5 parts of glycerol;
0.05-0.1 part of sodium hyaluronate;
0.35-0.5 part of p-hydroxyacetophenone.
4. The whitening composite preparation according to claim 3, wherein the water-phase material is prepared by the following steps:
a1, adding acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer into deionized water, and stirring to obtain a first premix;
a2, mixing sodium hyaluronate with glycerol, and stirring to obtain a second premix;
a3, adding p-hydroxyacetophenone into the first premix, heating to dissolve, adding the second premix, and stirring to obtain the water-phase material.
5. The whitening composite preparation according to claim 2, wherein the oil phase material comprises the following components in parts by weight:
0.5-1.5 parts of polydimethylsiloxane;
0.5-1 part of PEG-20 methyl glucose sesquistearate;
0.5-1 part of chinaroot greenbrier seed oil.
6. The whitening composite preparation according to claim 5, wherein the oil phase material is prepared by the following steps: heating and dissolving PEG-20 methyl glucose sesquistearate and polydimethylsiloxane, adding white Potentilla chinensis seed oil, stirring and mixing to obtain oil phase material.
7. The whitening composite preparation according to claim 2, wherein the low-temperature material comprises the following components in parts by weight:
0.05-0.075 part of caprylyl hydroximic acid;
0.017-0.025 parts of glycerol caprylate;
0.28-0.5 part of methyl propylene glycol;
0.15-0.25 part of arginine.
8. The method for preparing the whitening composite preparation of any one of claims 2 to 7, characterized by comprising the following steps:
s1, mixing the water phase material and the oil phase material, homogenizing and stirring to obtain essence;
s2, adding the composition with the whitening effect and the low-temperature material into the essence, and stirring to obtain the whitening compound preparation.
9. The method for preparing a whitening composite preparation according to claim 8, characterized in that the salidroside-plus and pterostilbene are both pre-treated before being added,
the pretreatment process of the salidroside-plus comprises the following steps: dissolving cyclodextrin in water to obtain cyclodextrin saturated solution, setting the dissolving temperature at 40-50 deg.C, adding salidroside-plus into the cyclodextrin saturated solution, stirring for 3-4 hr, filtering, and drying to obtain the final product; the pretreatment process of pterostilbene is as follows: dissolving cyclodextrin in water to obtain cyclodextrin saturated solution, setting the dissolving temperature at 40-50 deg.C, adding pterostilbene into ethanol to obtain pterostilbene ethanol solution, adding pterostilbene ethanol solution into cyclodextrin saturated solution, stirring for 3-4 hr, filtering, and drying.
10. The method for preparing a whitening composite preparation according to claim 8, wherein in S1, the mixing temperature is set to 75-85 ℃, the homogenizing rotation speed is set to 5000-6000rpm, and the homogenizing time is set to 5-10 min; in the S2, the stirring temperature is set to 40-45 ℃.
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