CN116440048A - Composite retinol composition and preparation method and application thereof - Google Patents
Composite retinol composition and preparation method and application thereof Download PDFInfo
- Publication number
- CN116440048A CN116440048A CN202310624211.1A CN202310624211A CN116440048A CN 116440048 A CN116440048 A CN 116440048A CN 202310624211 A CN202310624211 A CN 202310624211A CN 116440048 A CN116440048 A CN 116440048A
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- retinol
- parts
- composition
- composite
- skin
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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
- A61K8/96—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
- A61K8/30—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
- A61K8/34—Alcohols
- A61K8/342—Alcohols having more than seven atoms in an unbroken chain
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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
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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
- A61K8/67—Vitamins
- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
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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
- A61K8/73—Polysaccharides
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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
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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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
- A61K8/9706—Algae
- A61K8/9722—Chlorophycota or Chlorophyta [green algae], e.g. Chlorella
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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
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing 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
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
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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
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
Abstract
The invention relates to a compound retinol composition and a preparation method and application thereof, wherein the compound retinol composition comprises hydroxy pinacolone retinoic acid ester, retinol palmitate and bidens pilosa extract.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a composite retinol composition, and a preparation method and application thereof.
Background
The skin gradually enters a natural aging state from about 25 years old, so that whitening and aging resistance becomes the first task of skin care of people, and more whitening and aging resistance products are favored by many consumers. However, the whitening and anti-aging products with strong efficacy inevitably have the problem of strong irritation, and retinol and its derivatives are increasingly applied to whitening and anti-aging skin care products because of their characteristics of improving the state of epidermal cells and being safe and effective.
CN112957276a discloses a multi-effect hydroxypivalone retinoate nanocomposite comprising hydroxypivalone retinoate, nicotinamide, glycyrrhetinic acid, emulsifiers, co-emulsifiers, and polyols. The nanometer composition disclosed by the invention has the advantages that the hydroxy pinacolone retinoic acid ester, nicotinamide and glycyrrhetinic acid are wrapped in the nanometer composition, so that the stability of the functional components is effectively improved. The three functional components of the nano composition are reasonably matched, are synergistic, penetrate through the skin barrier and enter deep skin tissues, improve the bioavailability, increase the anti-aging, acne removing and whitening effects, are mild and free of stimulation to the skin, and can be widely applied to cosmetics.
CN108210362a discloses a technological formula of a VACE essence for removing freckle and whitening. The main components are as follows: retinol palmitate (VA), ascorbyl tetraisopalmitate (VC), tocopheryl acetate (VE), canola oil, silicones, polydimethyl siloxane and other adjunct ingredients. The invention has the advantages that: particularly adopts fat-soluble VC component with extremely high affinity with skin and VA and VE essence, and deeply isolates external environment pollution while fading color spots, resisting allergy and eliminating redness and dark skin, and improves the skin color. The invention adopts the organic silicon as the auxiliary material, so that the essence is fine, smooth and fresh, has good spreadability, is suitable for any skin, and is especially suitable for dry and dull skin.
However, the above products added with retinol have single action path and lack a combination of multiple dimensions, so that it is highly desirable to develop a retinol product with high efficiency and multiple action mechanisms based on the needs and targeting mechanism of consumers to meet the application needs of consumers.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a composite retinol composition, a preparation method and application thereof, and the composite retinol composition can solve the skin problem in a multi-target way by utilizing the combination of different retinol components, thereby meeting the requirements of consumers on whitening, moisturizing and anti-aging.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a complex retinol composition, comprising hydroxy pinacolin retinol, retinol palmitate and bidens pilosa extract.
According to the composition, through the synergistic combination of Hydroxy Pinacolone Retinoate (HPR), retinol palmitate and bidens pilosa extract, on one hand, the composition can stimulate the generation of epidermal keratinocytes, thicken a granular layer, strengthen intercellular adhesion protein deposition, increase the thickness of epidermis, greatly solve the problem of thinning skin due to aging, has the effect of reducing wrinkles, can make the skin smooth and glossy, has enhanced light transmittance, and can make the skin look redder, on the other hand, can interact with fibroblasts of dermis to generate more collagen and elastic fibers, reduce the decomposition and aging of the collagen, and has good supporting effect to enable the skin to be plump, compact and elastic.
The composite retinol composition also comprises bisabolol and/or isosorbide dimethyl ether.
As a preferable technical scheme of the invention, the isosorbide dimethyl ether can promote better mutual solubility of hydroxy pinacolone retinoic acid ester, retinol palmitate and bidens pilosa extract, so that the penetration of active ingredients to epidermis can be increased; the bisabolol can promote the regeneration of cells, has the effects of caring skin and relieving skin, and can improve the transdermal absorption of active ingredients, and the composition can further improve the effects of whitening and brightening skin and resisting aging and removing wrinkles by adding the bisabolol and the isosorbide dimethyl ether.
Preferably, the complex retinol composition comprises hydroxy pinacolin retinoate, retinol palmitate, bidens pilosa extract, bisabolol and isosorbide dimethyl ether.
Preferably, the compound retinol composition comprises 0.1-1 part of hydroxy pinacolone retinoic acid ester, 0.1-1 part of retinol palmitate, 0.1-2 parts of bidens pilosa extract, 0.01-0.5 part of bisabolol and 1-10 parts of isosorbide dimethyl ether according to parts by weight.
The amount of the hydroxy pinacolin retinoic acid ester added in the composite retinol composition of the present invention can be 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts or 0.9 parts, etc.;
the retinol palmitate may be added in an amount of 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts or 0.9 parts, etc.;
the addition amount of the bidens pilosa extract can be 0.2 part, 0.3 part, 0.5 part, 0.7 part, 0.9 part, 1 part, 1.2 part, 1.4 part, 1.6 part or 1.8 part and the like;
the addition amount of the bisabolol may be 0.05 part, 0.1 part, 0.15 part, 0.2 part, 0.25 part, 0.3 part, 0.35 part, 0.4 part, 0.45 part, or the like;
the addition amount of the isosorbide dimethyl ether can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts, etc.
Specific point values in the numerical ranges are selectable, and will not be described in detail here.
In a second aspect, the present invention provides a method for preparing a composite retinol composition as defined in the first aspect, said method comprising mixing and stirring hydroxy pinacolin retinol ester, retinol palmitate and herba Bidentis Bipinnatae extract, homogenizing to obtain said composite retinol composition.
Preferably, the preparation method comprises the steps of stirring and mixing hydroxy pinacolone retinoic acid ester, retinol palmitate, bidens pilosa extract, bisabolol and isosorbide dimethyl ether, and homogenizing to obtain the compound retinol composition.
Preferably, the temperature of the stirring and mixing is 50-60 ℃, for example, 51 ℃, 53 ℃, 55 ℃, 57 ℃, 59 ℃ or the like.
Preferably, the rotation speed of stirring and mixing is 300-400r/min, and can be 310r/min, 330r/min, 350r/min, 370r/min or 390r/min, for example.
Specific point values in the numerical ranges are selectable, and will not be described in detail here.
In a third aspect, the present invention provides the use of a complex retinol composition as defined in the first aspect in cosmetics.
Preferably, the cosmetic comprises any one of essence, essence cream, face cream, facial mask and skin lotion.
Preferably, the mass percentage of the composite retinol composition in the cosmetic is 1-10%, for example, 2%, 3%, 4%, 5%, 6%, 7%, 8% or 9%, etc., and the specific point values in the above numerical ranges are all selectable, and will not be described in detail herein.
In a fourth aspect, the invention provides an essence, which comprises, by weight, 1-10 parts of the composite retinol composition, 1-20 parts of a humectant, 1-10 parts of a skin conditioning agent, 1-3 parts of an antioxidant, 0.1-0.5 part of a thickening agent, 0.01-0.1 part of a solubilizer, 0.01-0.1 part of a chelating agent and 1-90 parts of deionized water.
The adding amount of the compound retinol composition in the essence of the invention can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts, etc.;
the humectant can be added in an amount of 2 parts, 4 parts, 6 parts, 8 parts, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts or the like;
the skin conditioning agent may be added in an amount of 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, or the like;
the antioxidant may be added in an amount of 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, 2.2 parts, 2.4 parts, 2.6 parts, or 2.8 parts, etc.;
the thickener may be added in an amount of 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, or the like;
the amount of the solubilizer added may be 0.02 part, 0.03 part, 0.04 part, 0.05 part, 0.06 part, 0.07 part, 0.08 part, 0.09 part, or the like;
the chelating agent may be added in an amount of 0.02 part, 0.03 part, 0.04 part, 0.05 part, 0.06 part, 0.07 part, 0.08 part, 0.09 part, or the like;
the deionized water may be added in an amount of 5 parts, 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, 90 parts, 95 parts, or the like.
Specific point values in the numerical ranges are selectable, and will not be described in detail here.
Preferably, the humectant comprises any one or a combination of at least two of glycerin, butylene glycol, tremella heteropolysaccharide, trehalose or hydrolyzed sodium hyaluronate.
Preferably, the humectant is a combination of tremella heteropolysaccharide, trehalose and hydrolyzed sodium hyaluronate.
In the invention, when the humectant is the combination of the tremella polysaccharide, the trehalose and the sodium hyaluronate hydrolysate, the moisture content of the cuticle can be further improved, the decomposition and oxidation of collagen in skin are reduced, and the tremella polysaccharide, the trehalose and the sodium hyaluronate hydrolysate have a certain synergistic effect on the effects.
Preferably, the skin conditioner comprises any one or a combination of at least two of argania spinosa kernel oil, bearberry extract or chlorella extract.
Preferably, the skin conditioner is a combination of argania spinosa kernel oil, bearberry extract and chlorella extract.
The skin conditioner disclosed by the invention can enhance skin cell metabolism through the synergistic combination of the argania spinosa kernel oil, the bearberry extract and the chlorella extract, has a good whitening and nourishing effect on skin, and can be matched with other components of the essence to realize synergistic effect, so that the effects of whitening, removing wrinkles and brightening skin color of the essence are further improved.
Preferably, the antioxidant comprises p-hydroxyacetophenone and/or nicotinamide.
Preferably, the chelating agent comprises EDTA-2 sodium.
Preferably, the thickener comprises any one or a combination of at least two of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, carbomer or xanthan gum.
Preferably, the solubiliser comprises polysorbate-20 and/or PEG-40 hydrogenated castor oil.
Preferably, the essence further comprises any one or a combination of at least two of a pH adjustor, a preservative, or a fragrance.
In a fifth aspect, the present invention provides a method for preparing the essence according to the fourth aspect, the method comprising:
(1) Mixing humectant, water, thickener and chelating agent, heating and stirring at 70-80deg.C (such as 75deg.C, 75deg.C or 75deg.C) to obtain water phase solution;
(2) Cooling the aqueous phase liquid obtained in the step (1) to below 50 ℃ (such as 38 ℃, 40 ℃, 42 ℃, 44 ℃, 46 ℃ or 48 ℃ and the like), adding an antioxidant, stirring uniformly, cooling to below 35 ℃ (such as 25 ℃, 28 ℃, 30 ℃, 32 ℃ or 34 ℃ and the like), then sequentially adding the compound retinol composition, the skin conditioning agent and the solubilizer, and stirring uniformly to obtain the skin care product;
preferably, step (2) further comprises adding any one or a combination of at least two of a pH adjuster, preservative or fragrance after adding the solubilizing agent.
Specific point values in the numerical ranges are selectable, and will not be described in detail here.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the composition, through the synergistic combination of Hydroxy Pinacolone Retinoate (HPR), retinol palmitate and bidens pilosa extract, on one hand, the composition can stimulate the generation of epidermal keratinocytes, thicken a granular layer, strengthen intercellular adhesion protein deposition, increase the thickness of epidermis, greatly solve the problem of thinning skin due to aging, has the effect of reducing wrinkles, can make the skin smooth and glossy, has enhanced light transmittance, and can make the skin look redder, on the other hand, can interact with fibroblasts of dermis to generate more collagen and elastic fibers, reduce the decomposition and aging of the collagen, and has good supporting effect to enable the skin to be plump, compact and elastic.
2. The essence disclosed by the invention can increase the nutrition of skin, deeply moisten the skin, and has the effects of resisting aging, removing wrinkles and whitening and brightening the skin through the matching of the functional components.
3. The preparation method of the essence provided by the invention is simple and easy to operate, is easy for industrial mass production, and has excellent practicability.
Detailed Description
In order to further describe the technical means adopted by the present invention and the effects thereof, the following describes the technical scheme of the present invention in combination with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.
The parts by weight of hydroxy pinacolin retinoic acid ester, retinol palmitate, bidens pilosa extract and bisabolol are calculated by the actual content of functional components contained in the commercial raw materials, and any one or a combination of at least two of solvents, fillers, diluents, stabilizers, pH regulators, antibacterial agents, antioxidants and impurities within the allowable range are also optionally contained in the commercial raw materials.
The following examples and comparative examples relate to the following partial materials and brand information:
the remaining materials can be used as long as they are purchased from a regular dealer.
Example 1
The present example provides a complex retinol composition prepared by the following preparation method: 0.5 part of hydroxy pinacolone retinoic acid ester, 0.5 part of retinol palmitate, 1 part of bidens pilosa extract, 0.3 part of bisabolol and 5 parts of isosorbide dimethyl ether are stirred and mixed at 55 ℃ and 350r/min, and the mixture is homogenized to obtain the composite retinol composition.
Example 2
The present example provides a complex retinol composition prepared by the following preparation method: 1 part of hydroxy pinacolone retinoic acid ester, 0.3 part of retinol palmitate, 1.5 parts of bidens pilosa extract, 0.1 part of bisabolol and 8 parts of isosorbide dimethyl ether are stirred and mixed at 50 ℃ and 300r/min, and the mixture is homogenized to obtain the compound retinol composition.
Example 3
The present example provides a complex retinol composition prepared by the following preparation method: 0.3 part of hydroxy pinacolone retinoic acid ester, 1 part of retinol palmitate, 0.5 part of bidens pilosa extract, 0.5 part of bisabolol and 3 parts of isosorbide dimethyl ether are stirred and mixed at 50 ℃ and 300r/min, and the mixture is homogenized to obtain the composite retinol composition.
Example 4
This example provides a composite retinol composition which differs from example 1 only in that no isosorbide dimethyl ether is added during the preparation process, the remaining components and the addition amounts remain unchanged, and the preparation method is described with reference to example 1.
Example 5
This example provides a composite retinol composition which differs from example 1 only in that bisabolol is not added during the preparation process, and the remaining components and addition amounts remain unchanged, and the preparation method is described with reference to example 1.
Comparative example 1
This example provides a combination retinol composition which differs from example 1 only in that no hydroxy pinacolin retinoic acid ester is added during the preparation process, the reduced amount is distributed to retinol palmitate and bidens pilosa extract in parts ratio, and the rest components and the added amount are kept unchanged, and the preparation method is described in example 1.
Comparative example 2
This example provides a complex retinol composition which differs from example 1 only in that no retinol palmitate is added during the preparation process, the reduced amount is distributed to hydroxy pinacolin retinol and bidens pilosa extract in parts ratio, and the rest components and the added amount remain unchanged, and the preparation method is described in example 1.
Comparative example 3
This comparative example provides a complex retinol composition which differs from example 1 only in that no herba Bidentis Bipinnatae extract is added during the preparation, the reduced amount is distributed to hydroxy pinacolin retinoic acid ester and retinol palmitate in parts ratio, and the rest components and addition amounts remain unchanged, and the preparation method is described in example 1.
Application example 1
The application example provides an essence, which comprises the following formula:
the preparation method comprises the following steps:
(1) Mixing humectant, water, thickener and chelating agent, heating and stirring at 75deg.C to obtain water phase solution;
(2) Cooling the aqueous phase liquid obtained in the step (1) to 40 ℃, adding an antioxidant, stirring uniformly, cooling to below 30 ℃, and then sequentially adding the composite retinol composition, the skin conditioning agent and the solubilizer, and stirring uniformly to obtain the skin care product.
Application examples 2 to 5
The present application example provides four kinds of essence, the formulation of which is different from that of application example 1 only in that the composite retinol composition of example 1 is replaced by the composite retinol compositions of examples 2 to 5 with the same addition amount, and other conditions are kept unchanged, and the preparation method is referred to application example 1.
Application example 6
The present application example provides an essence whose formulation differs from application example 1 only in that the skin conditioner does not include a skin conditioner, its reduction is complemented by deionized water, and other conditions remain unchanged. The preparation method is described in application example 1.
Application example 7
The application example provides an essence, and the formula of the essence is different from that of application example 1 only in that the skin conditioner does not comprise chlorella extract, and the reduction amount of the chlorella extract is distributed into the argania spinosa kernel oil and the bearberry extract according to the part ratio, and other conditions are kept unchanged. The preparation method is described in application example 1.
Application example 8
The application example provides an essence, and the formula of the essence is different from that of application example 1 only in that the skin conditioner does not comprise the argania spinosa kernel oil, and the reduction amount of the argania spinosa kernel oil is distributed into chlorella extract and bearberry extract according to the part ratio, and other conditions are kept unchanged. The preparation method is described in application example 1.
Application example 9
The application example provides an essence, and the formula of the essence is different from that of application example 1 only in that the skin conditioner does not comprise bearberry extract, and the reduction amount of bearberry extract is distributed into argania spinosa kernel oil and chlorella extract according to the part ratio, and other conditions are kept unchanged. The preparation method is described in application example 1.
Application example 10
The application example provides an essence, and the formula of the essence is different from that of the application example 1 only in that the humectant does not comprise tremella heteromeric polysaccharide, and the reduced amount of tremella heteromeric polysaccharide is distributed into trehalose and hydrolyzed sodium hyaluronate according to the part ratio, and other conditions are kept unchanged. The preparation method is described in application example 1.
Application example 11
The application example provides an essence, and the formula of the essence is different from that of the application example 1 only in that the humectant does not comprise trehalose, and the reduced amount of the trehalose is distributed into tremella polysaccharide and hydrolyzed sodium hyaluronate in parts by weight, and other conditions are kept unchanged. The preparation method is described in application example 1.
Application example 12
The application example provides an essence, and the formula of the essence is different from that of the application example 1 only in that the humectant does not comprise hydrolyzed sodium hyaluronate, and the reduced amount of the hydrolyzed sodium hyaluronate is distributed into tremella polysaccharide and trehalose in parts by weight, and other conditions are kept unchanged. The preparation method is described in application example 1.
Comparative application examples 1 to 3
The present application example provides three kinds of essences, the formulation of which is different from that of application example 1 only in that the complex retinol composition of example 1 is replaced with the complex retinol compositions of comparative examples 1-3 with the same addition amount, respectively, and the other conditions are kept unchanged. The preparation method is described in application example 1.
Comparative application example 4
The present application example provides a essence whose formulation differs from that of application example 1 only in that it does not contain the component of the composite retinol composition, its reduction is complemented by water, and other conditions remain unchanged. The preparation method is described in application example 1.
Test example 1: in vitro cell tyrosinase inhibition assay
1.1 sample preparation
The compositions of examples 1-5 and comparative examples 1-3 were diluted to a concentration of 0.45mg/ml in serum-free medium;
1.2 cell culture
The melanoma cells of the mice B16 grow to a fusion state, are digested by pancreatin-EDTA for 5min, are blown and dispersed, the cell suspension is sucked into a centrifuge tube, the centrifugation is carried out for 5min by using a centrifuge at 1000r/min, the supernatant is discarded, and the culture medium is added to prepare the cell suspension. The cells are treated with a culture mediumThe suspension was diluted to a certain concentration. Inoculating logarithmic phase B16 cells into 96-well plate with cell density of 7X10 4 cfu/ml, 100. Mu.L per well, was plated and labeled on the top of the cell plate. Culturing was performed in an incubator for 24 hours.
The supernatant was carefully aspirated from the cell plates after 24h incubation, and the plates were divided into a blank group, a positive control group, and a sample group. Adding prepared samples into a sample group, adding culture solution containing alpha-arbutin into a positive control group, and adding serum-free culture medium without medicines into a blank group. The addition amount is 100 mu L/hole, 4 compound holes are made for each concentration, and after the addition, the mixture is placed into an incubator for culturing for 72 hours.
1.3 intracellular tyrosinase inhibition assay
The cell plates after 72h incubation were discarded, 150. Mu.L of 1% Triton X-100 solution was added to each well, rapidly frozen at-80℃for 30min, then thawed at room temperature to completely disrupt the cells, pre-warmed at 37℃for 5min, then 60. Mu.L of 0.5% L-DOPA solution was added, reacted at 37℃for 2h, and the absorbance (OD) was measured at 490nm in an ELISA reader. And calculating the inhibition rate of tyrosinase activity.
Tyrosinase activity inhibition ratio (%) = (1-sample average absorbance value/blank average absorbance value) ×100%. The results are shown in Table 1.
Test example 2: test for inhibiting melanin in zebra fish embryo
2.1 sample preparation
The compositions of examples 1-5 and comparative examples 1-3 were directly dissolved with fish embryo culture to prepare test solutions at a concentration of 1 mg/ml.
2.2 cultivation and detection
Healthy zebra fish embryos are selected and cultured at 28 ℃ for 6-8 hours after fertilization at a density of not more than 1 fish embryo in 200 mu L of fish embryo culture solution. The 96-well plates were divided into 3 groups, which were a blank control group (fish embryo culture solution), a positive control group (phenylthiourea working solution) and a test substance group (test substance), respectively, and the corresponding fish embryo culture solutions were added. Subsequently, 24 fish embryos are randomly selected from X3 groups to 96-well plates, placed in a constant temperature oven at 28+ -1deg.C and cultured until 48+ -1 h after fertilization. Covering the fish embryo with 2-4% methyl cellulose, and photographing the fish embryo under a stereo microscope according to uniform photographing parameters. The head and yolk back regions of each fish embryo are marked by analysis software, then the average measured intensity in the column of measurement is selected, and the average signal intensity in the test result is selected as the melanin signal intensity. The melanin inhibition rate was calculated.
Zebra fish embryo melanin inhibition rate = [ (normal zebra fish embryo melanin level-sample treatment group zebra fish embryo melanin level) ×100/(normal zebra fish embryo melanin level-positive control group zebra fish embryo melanin level) ]%. The results are shown in Table 1.
TABLE 1
| Test sample | Intracellular tyrosinase inhibition% | Zebra fish embryo melanin inhibiting rate% |
| Example 1 | 39.23 | 40.86 |
| Example 2 | 38.47 | 39.15 |
| Example 3 | 39.09 | 38.28 |
| Example 4 | 35.42 | 34.76 |
| Example 5 | 36.26 | 35.91 |
| Comparative example 1 | 30.15 | 28.54 |
| Comparative example 2 | 29.73 | 29.45 |
| Comparative example 3 | 30.82 | 28.29 |
The data of examples 1-3 show that the intracellular tyrosinase inhibition rate of the composite retinol composition provided by the invention is 38.47-39.23%, and the melanin inhibition rate of the zebra fish embryo is 38.28-40.86%, which shows that the composition has remarkable effects of whitening, resisting aging and protecting skin of human body; as can be seen from a comparison of example 1 with comparative examples 1-3, the intracellular tyrosinase inhibition rate of the composition and the melanin inhibition rate of the zebra fish embryos were significantly reduced when any one of hydroxy pinacolin retinoate, retinol palmitate and bidens pilosa extract was absent from the composition.
Test example 3 anti-wrinkle efficacy test
The anti-wrinkle efficacy test was performed on the essences provided in application examples 1 to 12 and the essences provided in comparative application examples 1 to 4, as follows:
(1) Promoting elastin production test: human fibroblasts are inoculated on a 96-well plate according to the density of 20000 cells per well, a culture medium is added, the culture is carried out for 24 hours in a 37 ℃ incubator, after the cells are attached, a new culture medium is replaced, samples of application examples 1-12 and comparative application examples 1-4 are respectively added (the final concentration of the samples is controlled to be 50 mg/mL), a 20mmol/L PBS solution is used as a blank control, and then the culture is carried out for 2 days in the 37 ℃ incubator;
(2) Clinical anti-wrinkle efficacy test: 160 volunteers 18-55 years old with healthy skin were selected, randomly divided into 16 groups of 5 men and 5 women, and the facial crease marks of the subjects were obtained by using silicone, and then the essences of application examples 1-12 and comparative application examples 1-4 were applied to the facial crease of the subjects 2 times daily for 56 consecutive days, respectively. The wrinkle marks of the test sites of the subjects after 28 days and 56 days of treatment were obtained, and the wrinkle depths were measured by a confocal microscope. The percentage of reduction in wrinkle depth after 28 days and 56 days of treatment was calculated;
the specific test results are shown in table 2:
TABLE 2
As shown in the test data of Table 2, the essence disclosed by the invention can promote the expression of elastin, and the expression level of elastin is more than 5.6; after 28 days of use, the wrinkle depth reduction value reaches more than 12.9%, and after 56 days, the wrinkle depth reduction value reaches more than 20.6%, which shows that the components of the essence supplement each other, and the essence has a synergistic effect, can promote the synthesis and repair of collagen and fibronectin, improve the crack symptoms and further lighten fine lines; but also can tighten skin and repair skin fine lines. From application examples 10 to 12, it is known that when any one of tremella hetero polysaccharide, trehalose and hydrolyzed sodium hyaluronate is absent in the moisturizer, the expression of elastin of the essence is negatively affected.
Test example 4 anti-aging and brightening Effect test
The anti-aging and brightening effects of the essences provided in application examples 1 to 9 and the essences provided in comparative application examples 1 to 4 were tested as follows:
130 skin-healthy 18-55 year old volunteers were selected and randomly divided into 13 groups of 5 men and 5 women, each group was used 1 time a day in the morning and evening for 4 weeks with the samples of application examples 1-9 and comparative application examples 1-4, respectively, on the face.
(1) The skin melanin content changes before and after application of the mask composition to the subject were evaluated using a skin red melanin tester (Hexameter MX 18). The measurement range of the instrument used is 0-999, the higher the measurement value, the higher the melanin content in the skin. The reduction of melanin of the front and rear facial skin of a subject using the mask composition prepared by the invention;
(2) VISIA skin analysis evaluation: after the faces of the tested volunteers are cleaned, the faces are shot by a VISIA face image analyzer, detection data of pigment spots, textures and wrinkles of the faces are analyzed, and the higher the numerical value is, the more obvious the pigment spots and textures are represented. After a treatment course is finished, comparing the information obtained by the VISIA facial image analyzer with the information before treatment, and analyzing the improvement condition of facial pigment spots, textures and wrinkles of the tested volunteers, wherein p is less than 0.02, and the method has statistical significance;
(3) Lightening efficacy: the skin color of the test volunteers before and after treatment were tested with skin color difference tester (probe CL400 and multi-probe skin test system MPA 10), respectively, and ITA ° was calculated. The test conditions were constant temperature and humidity environment at 22℃and 50% humidity.
The specific test results are shown in table 3:
TABLE 3 Table 3
As can be seen from the test data in Table 3, the comparison of the VISIA test results before and after the treatment revealed that the subjects had a melanin reduction of 54% or more, a pigmentation mark reduction of 20% or more, a texture reduction of 23% or more, and a lightening effect of 25% or more, using the essence provided in application examples 1 to 3. Therefore, the essence has the effects of reducing melanin generation and brightening skin, can reduce skin fine lines and improve rough skin, and can be used for solving the problems that the types of skin conditioning agents have influence on the whitening effect and the wrinkle improvement effect of the essence as shown in application examples 7-9; as is clear from comparative application example 4, when the composite retinol composition of the present invention is absent in the essence, it has a significant negative effect on whitening the essence and improving wrinkles.
Test example 5: safety evaluation experiment
The essence provided in application examples 1-12 was tested for safety performance as follows:
protein denaturation experiment:
diluting the sample with PBS solution to 10g/L, adding 200 μl of the above red blood cell suspension into 10mL of the diluted solution, taking distilled water as blank control, 1mg/mL Sodium Dodecyl Sulfate (SDS) solution as positive control, gently mixing, incubating at 37deg.C for 30min, centrifuging at 2000r/min for 10min, collecting supernatant, and measuring absorbance A at 540nm and 575nm with spectrophotometer 540 And A 575 Calculating a protein denaturation index (D) according to the following formula;
wherein R is 1 Control group a =blank 575 Blank group A 540 ，R 2 Experimental group a 575 Experimental group A 540 ，R 3 Positive control group a = 575 Positive control group A 540 。
Evaluating the irritation of the sample to be tested according to the L/D value, wherein the L/D value is HD 50 The erythrocyte hemolysis assay stimulation fractionation criteria are shown in Table 4 below:
TABLE 4 Table 4
| L/D | Grading |
| >100 | No irritation |
| 10<L/D≤100 | Microstimulation |
| 1<L/D≤10 | Mild irritation |
| 0.1<L/D≤1 | Moderate irritation |
The test results are shown in table 5 below:
TABLE 5
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The safety performance test shows that the essence prepared by the application examples 1-12 is mild, has no stimulation and is safer and more reliable.
The applicant states that the present invention is illustrated by the above examples as a complex retinol composition, as well as the preparation method and application thereof, but the present invention is not limited to the above examples, i.e. it is not meant that the present invention must be practiced in dependence upon the above examples. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Claims (10)
1. A complex retinol composition, wherein said complex retinol composition comprises hydroxy pinacol retinol, retinol palmitate and bidens pilosa extract.
2. The composite retinol composition as defined in claim 1, wherein the composite retinol composition further comprises bisabolol and/or dimethyl isosorbide ether;
preferably, the complex retinol composition comprises hydroxy pinacolin retinoate, retinol palmitate, bidens pilosa extract, bisabolol and isosorbide dimethyl ether.
3. The composite retinol composition as defined in claim 1 or 2, wherein said composite retinol composition comprises, in weight parts, 0.1-1 part of hydroxy pinacolone retinol, 0.1-1 part of retinol palmitate, 0.1-2 parts of bidens pilosa extract, 0.01-0.5 part of bisabolol and 1-10 parts of isosorbide dimethyl ether.
4. A method of preparing a complex retinol composition as defined in any one of claims 1-3, wherein said preparation method comprises: mixing hydroxy pinacolone retinoate, retinol palmitate and herba Bidentis Bipinnatae extract under stirring, and homogenizing to obtain the composite retinol composition.
5. The method for preparing a composite retinol composition as defined in claim 4, wherein said method comprises mixing hydroxy pinacolin retinol ester, retinol palmitate, bidens pilosa extract, bisabolol and isosorbide dimethyl ether under stirring, homogenizing to obtain said composite retinol composition;
preferably, the temperature of the stirring and mixing is 50-60 ℃;
preferably, the rotation speed of stirring and mixing is 300-400r/min.
6. Use of the complex retinol composition as defined in any one of claims 1-3 in cosmetics;
preferably, the cosmetic comprises any one of essence, essence cream, face cream, facial mask and skin lotion;
preferably, the mass percentage of the composite retinol composition in the cosmetic is 1-10%.
7. An essence, characterized in that the essence comprises, by weight, 1-10 parts of the compound retinol composition as defined in any one of claims 1-3, 1-20 parts of a humectant, 1-10 parts of a skin conditioning agent, 1-3 parts of an antioxidant, 0.1-0.5 part of a thickening agent, 0.01-0.1 part of a solubilizer, 0.01-0.1 part of a chelating agent and 1-90 parts of deionized water.
8. The concentrate of claim 7, wherein the humectant comprises any one or a combination of at least two of glycerin, butylene glycol, tremella isopolysaccharide, trehalose, or hydrolyzed sodium hyaluronate;
preferably, the humectant is a combination of tremella heteropolysaccharide, trehalose and hydrolyzed sodium hyaluronate;
preferably, the skin conditioner comprises any one or a combination of at least two of argania spinosa kernel oil, bearberry extract or chlorella extract;
preferably, the skin conditioner is a combination of argania spinosa kernel oil, bearberry extract and chlorella extract.
9. The concentrate of claim 7 or 8, wherein the antioxidant comprises p-hydroxyacetophenone and/or nicotinamide;
preferably, the chelating agent comprises EDTA-2 sodium;
preferably, the thickener comprises any one or a combination of at least two of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, carbomer or xanthan gum;
preferably, the solubiliser comprises polysorbate-20 and/or PEG-40 hydrogenated castor oil;
preferably, the essence further comprises any one or a combination of at least two of a pH adjustor, a preservative, or a fragrance.
10. The process for preparing the serum according to any one of claims 7 to 9, characterized in that it comprises:
(1) Mixing humectant, water, thickener and chelating agent, heating and stirring at 70-80deg.C to obtain water phase solution;
(2) Cooling the aqueous phase liquid obtained in the step (1) to below 50 ℃, adding an antioxidant, uniformly stirring, cooling to below 35 ℃, sequentially adding a composite retinol composition, a skin conditioning agent and a solubilizer, and uniformly stirring to obtain the aqueous phase liquid;
preferably, step (2) further comprises adding any one or a combination of at least two of a pH adjuster, preservative or fragrance after adding the solubilizing agent.
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| CN117205103A (en) * | 2023-10-07 | 2023-12-12 | 诺德溯源(广州)生物科技有限公司 | Plant A alcohol-containing tightening and anti-aging composition suitable for sensitive muscles and application thereof |
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