CN112294706B - Moisturizing composition and preparation method and application thereof - Google Patents

Moisturizing composition and preparation method and application thereof Download PDF

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CN112294706B
CN112294706B CN201910704724.7A CN201910704724A CN112294706B CN 112294706 B CN112294706 B CN 112294706B CN 201910704724 A CN201910704724 A CN 201910704724A CN 112294706 B CN112294706 B CN 112294706B
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weight
parts
sodium
stirring
moisturizing
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CN112294706A (en
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孟宏
刘盼玉
曲召辉
刘有停
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Nutri Woods Bio Tech Beijing Co ltd
Taihe Kangmei Beijing Research Institute of Traditional Chinese Medicine Co Ltd
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Taihe Kangmei Beijing Research Institute of Traditional Chinese Medicine Co Ltd
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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
    • A61K8/9717—Rhodophycota or Rhodophyta [red algae], e.g. Porphyra
    • 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
    • A61K8/345—Alcohols containing more than one hydroxy group
    • 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
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/42—Amides
    • 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
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • 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
    • A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4906—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
    • A61K8/4913—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom having five membered rings, e.g. pyrrolidone carboxylic acid
    • 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
    • A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
    • A61K8/4946—Imidazoles or their condensed derivatives, e.g. benzimidazoles
    • 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
    • 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
    • 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
    • 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
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/88—Polyamides
    • 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
    • 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

Abstract

The invention provides a composition with long-acting moisturizing effect, a preparation method and application thereof, wherein the moisturizing composition comprises the following components: glycerin, carrageen crispa, sodium polyglutamate, sodium hyaluronate, L-serine, sodium pyrrolidone carboxylate, betaine and a pH regulator. 0.001 to 40wt% of glycerin, and/or 0.01 to 5wt% of the carrageen crispus, and/or 0.01 to 5wt% of the sodium polyglutamate, and/or 0.01 to 5wt% of the sodium hyaluronate, and/or 0.01 to 2wt% of the L-serine, and/or 0.001 to 15wt% of the sodium pyrrolidone carboxylate, and/or 0.001 to 15wt% of the betaine, and/or 0.001 to 5wt% of the pH adjusting agent, based on the total weight of the moisturizing composition. Experiments prove that the moisturizing composition has a long-acting moisturizing effect, good stability and skin feel and wide application prospect in the field of skin care products.

Description

Moisturizing composition and preparation method and application thereof
Technical Field
The invention relates to the field of skin care, and particularly relates to a composition with a moisturizing effect, and a preparation method and application thereof.
Background
The moisture absorption performance and the moisture retention capacity of the skin are caused by the fact that the natural moisture retention factors are contained in the surface layer of the skin, but the lipid barrier on the surface layer of the skin is damaged due to various reasons such as environment, the natural moisture retention factors are easy to lose, and the phenomena of dryness and desquamation of the skin are caused.
Aiming at the problem, a plurality of moisturizing skin care products achieve an instant moisturizing effect by adding a moisturizing agent, but as time increases, most of the moisturizing agent directly applied runs off and is not fully utilized, so that the moisturizing effect of the product is quickly and obviously reduced, most moisturizing products cannot achieve long-acting moisturizing, a certain moisturizing effect can be achieved only by frequently using the moisturizing products, and the moisturizing cost is greatly improved. In addition, although various components such as L-serine and sodium pyrrolidone carboxylate can be used as natural moisturizing factors, the combination of the components cannot achieve a good synergistic effect.
In order to reduce the loss of moisturizing components and improve the moisturizing effect, the existing moisturizing products mostly adopt macromolecular substances such as sodium hyaluronate or cellulose to form films to achieve the moisturizing effect, but the fact proves that most of the existing moisturizing products can only achieve the short-term moisturizing effect, and long-acting moisturizing is difficult to achieve. Although macromolecular substances can be compounded for use, the mixed system is usually unstable, the viscosity of the system is high, and the application effect is poor. Therefore, few people in the market prepare moisturizing preparations by compounding various macromolecular carriers.
How to obtain a product with strong stability and long-acting moisturizing effect becomes the key point of research and development in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a composition containing a macromolecular compound and having a long-acting moisturizing effect, and provides a preparation method and application of the moisturizing composition. According to the invention, a plurality of macromolecules and moisturizing components are compounded to obtain the moisturizing composition with strong stability, good skin feel and strong slow-release effect, so that the problem that micromolecular moisturizing agents such as natural moisturizing factors are difficult to play a long-acting moisturizing effect on the surface of skin is solved.
In order to achieve the purpose, the invention idea is as follows: the molecular structure of the Chondrus crispus has half ester type sulfate radical, and the side chain of the poly-sodium glutamate contains a large amount of carboxyl which can interact with amino acid components. The polyglutamic acid sodium, the carrageen crispa and the sodium hyaluronate can form a stable net structure in a water environment, can be used as a carrier to contain various substance components, and can act on skin by combining with humectant components, so that the long-acting moisturizing effect is achieved.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a long-lasting moisturizing composition comprising: glycerin, carrageen crispa, sodium polyglutamate, sodium hyaluronate, L-serine, sodium pyrrolidone carboxylate, betaine and a pH regulator.
According to some preferred embodiments of the present invention, the glycerol is 0.001 to 40wt%, and/or the Chondrus crispus is 0.01 to 5wt%, and/or the sodium polyglutamate is 0.01 to 5wt%, and/or the sodium hyaluronate is 0.01 to 5wt%, and/or the L-serine is 0.01 to 2wt%, and/or the sodium pyrrolidone carboxylate is 0.001 to 15wt%, and/or the betaine is 0.001 to 15wt%, and/or the pH adjusting agent is 0.001 to 5wt%, based on the total weight of the composition of the present invention.
According to some preferred embodiments of the invention the sodium polyglutamate has a molecular weight of 50 Da or more, for example in the range of 50-300 Da, such as 50 Da, 80 Da, 100 Da, 150 Da, 250 Da, etc.
According to some preferred embodiments of the invention the Chondrus crispus has a molecular weight ≧ 80 ten thousand Da, such as in the range of 80-600 ten thousand Da, such as 100 ten thousand Da, 150 ten thousand Da, 200 ten thousand Da, 500 ten thousand Da, etc.
According to some preferred embodiments of the invention, the sodium hyaluronate has a molecular weight of 5 ten thousand Da or more, for example, it may be in the range of 5 to 250 ten thousand Da, such as 50 ten thousand Da, 100 ten thousand Da, 150 ten thousand Da, 190 ten thousand Da, etc.
According to a more preferred embodiment of the invention, the molecular weight of the sodium polyglutamate is 100-150 ten thousand Da.
According to a more preferred embodiment of the present invention said Chondrus crispus has a molecular weight of 150-250 ten thousand Da.
According to a more preferred embodiment of the present invention, the molecular weight of the sodium hyaluronate is 100-.
According to some embodiments of the present invention, the pH adjusting agent may be L-glutamic acid, or other pH adjusting agents conventional in the art, such as citric acid, sodium hydroxide, and the like, without being particularly limited.
According to some preferred embodiments of the present invention, the moisturizing composition further comprises: one or more of L-proline, L-glutamic acid, urea, trehalose and allantoin. The components are added to achieve a synergistic effect, so that a better moisturizing effect can be obtained.
Preferably, the L-proline is 0.01-2wt%, and/or the L-glutamic acid is 0.001-0.3wt%, and/or the urea is 0.001-20wt%, and/or the trehalose is 0.001-10wt%, and/or the allantoin is 0.001-0.5wt%, based on the total weight of the moisturizing composition.
Further preferably, the moisturizing composition further comprises water and a preservative. Preservatives conventional in the art may be used in the moisturizing composition of the present invention, and are not particularly limited.
In some embodiments of the invention, the preservative used is phenoxyethanol/ethylhexyl glycerol or caprylyl glycol. Further, the preservative is used in an amount of less than or equal to 1wt% based on the total weight of the moisturizing composition.
According to the present invention, the sodium polyglutamate is 0.01 to 5wt% based on the total weight of the moisturizing composition of the present invention, for example, 0.01%, 0.02%, 0.03%, 0.05%, 0.06%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.5%, 1.6%, 1.8%, 2%, 2.1%, 2.2%, 2.5%, 2.7, 2.9%, 3%, 3.3%, 3.5%, 3.6%, 3.7%, 3.9%, 4%, 4.1%, 4.2%, 4.3%, 4.6%, 4.8%, 5%, and specific points between the above values are not exhaustive and are not limited to the present invention and specific points included in the range are not included for brevity. Preferably, the content of the sodium polyglutamate is 0.01-3wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the carrageen crispa is 0.01 to 5wt% based on the total weight of the moisturizing composition of the present invention, for example, 0.01%, 0.02%, 0.03%, 0.05%, 0.06%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.5%, 1.6%, 1.8%, 2%, 2.1%, 2.2%, 2.5%, 2.7, 2.9%, 3%, 3.3%, 3.5%, 3.6%, 3.7%, 3.9%, 4%, 4.1%, 4.2%, 4.3%, 4.6%, 4.8%, 5%, and specific points between the above values are not exhaustive and for brevity and the invention is not intended to be limited to the list and specific points included in the scope are not included. Preferably, the content of the Chondrus crispus is 0.1-5wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the sodium hyaluronate is 0.01 to 5wt%, for example, 0.01%, 0.02%, 0.03%, 0.05%, 0.06%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.5%, 1.6%, 1.8%, 2%, 2.1%, 2.2%, 2.5%, 2.7, 2.9%, 3%, 3.3%, 3.5%, 3.6%, 3.7%, 3.9%, 4%, 4.1%, 4.2%, 4.3%, 4.6%, 4.8%, 5% based on the total weight of the moisturizing composition of the present invention, and specific points between the above values are not limited to the extent and are not included in the range for brevity. Preferably, the content of the sodium hyaluronate is 0.01-3wt% based on the total weight of the moisturizing composition.
According to the present invention, the glycerin may be 0.001 to 40wt% based on the total weight of the moisturizing composition of the present invention, for example, 0.001%, 0.002%, 0.004%, 0.01%, 1%, 2%, 3%, 4%, 5%, 6%, 10%, 12%, 14%, 15%, 16%, 18%, 19%, 20%, 21%, 22%, 24%, 25%, 27%, 28%, 30%, 31%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, and specific values therebetween are not intended to be limited by space and for brevity, and the present invention is not exhaustive list of specific values included in the ranges. Preferably, the glycerin is contained in an amount of 15 to 35wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the L-serine is 0.01 to 2wt% based on the total weight of the moisturizing composition of the present invention, for example, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, and 2%, and specific points between the above values are not exhaustive and for the sake of brevity, and the present invention does not list the specific points included in the range. Preferably, the L-serine is used in an amount of 0.5 to 1.5wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the sodium pyrrolidone carboxylate is 0.001 to 15wt% based on the total weight of the moisturizing composition of the present invention, for example, 0.001%, 0.005%, 0.01%, 0.03%, 0.05%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.3%, 1.5%, 1.8%, 1.9%, 2%, 2.5%, 3%, 4%, 4.2%, 4.5%, 4.6%, 4.7%, 5%, 5.5%, 5.8%, 6%, 6.5%, 7%, 7.2%, 7.5%, 7.8%, 8%, 9%, 9.4%, 9.5%, 9.8%, 10%, 11%, 13%, 15%, and specific points between the above values are included in the present invention, and specific points between the above values are not included in the present invention, for brevity and for the sake of brevity and the present invention is not limited to the recited range. Preferably, the sodium pyrrolidone carboxylate is 0.5 to 8wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the betaine may be 0.001 to 15wt% based on the total weight of the moisturizing composition of the present invention, for example, 0.001%, 0.01%, 0.03%, 0.05%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.2%, 1.3%, 1.5%, 1.8%, 1.9%, 2%, 2.5%, 3%, 4%, 4.2%, 4.5%, 4.6%, 4.7%, 5%, 5.5%, 5.8%, 6%, 6.5%, 7%, 7.2%, 7.5%, 7.8%, 8%, 9%, 9.4%, 9.5%, 9.8%, 10%, 11%, 12%, 13%, 14%, 15%, and specific points between the above values are included in the present invention, and specific points between the above values are not included in the present invention, for brevity and for the sake of brevity and the present invention is not limited to the recited ranges. Preferably, the betaine is present in an amount of 0.5 to 8wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the pH adjusting agent is 0.001 to 5wt% based on the total weight of the moisturizing composition of the present invention, for example, 0.001%, 0.005%, 0.006%, 0.008%, 0.009%, 0.01%, 0.02%, 0.03%, 0.05%, 0.06%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.5%, 1.6%, 1.8%, 2%, 2.1%, 2.2%, 2.5%, 2.7, 2.9%, 3%, 3.3%, 3.5%, 3.6%, 3.7%, 3.9%, 4%, 4.1%, 4.2%, 4.3%, 4.6%, 4.8%, 5%, and specific points between the above-mentioned values, preferably, the pH adjusting agent is 0.1 to 5wt% based on the total weight of the moisturizing composition of the present invention, preferably, the pH adjusting agent is 0.001 to 5wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the L-proline is 0.01 to 2wt%, based on the total weight of the moisturizing composition of the present invention, and may be, for example, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, and 2%, and specific points between the above values, which are not intended to be exhaustive and for the sake of brevity, and the present invention does not list the specific points included in the range. Preferably, the L-proline is used in an amount of 0.1 to 1wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the L-glutamic acid is 0.001 to 0.3wt% based on the total weight of the moisturizing composition of the present invention, for example, 0.001%, 0.005%, 0.006%, 0.008%, 0.009%, 0.01%, 0.1%, 0.15%, 0.16%, 0.18%, 0.19%, 0.2%, 0.21%, 0.22%, 0.23%, 0.24%, 0.25%, 0.26%, 0.27%, 0.28%, 0.29%, and 0.3%, and specific points between the above values are not exhaustive list of the specific points included in the range for the sake of space and brevity. Preferably, the L-glutamic acid is used in an amount of 0.01 to 0.2wt% based on the total weight of the moisturizing composition of the present invention.
According to the invention, the urea may be present at 0.001-20wt%, for example 0.001%, 0.003%, 0.01%, 0.03%, 0.05%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.3%, 1.5%, 1.8%, 1.9%, 2%, 2.5%, 3%, 4%, 4.2%, 4.5%, 4.6%, 4.7%, 5%, 5.5%, 5.8%, 6%, 6.5%, 7%, 7.2%, 7.5%, 7.8%, 8%, 8.5%, 8.7%, 8.8%, 9%, 9.4%, 9.5%, 9.8%, 10%, 11%, 11.2%, 11.4%, 11.6%, 11.8%, 12%, 12.12%, 13.5%, 13.7%, 8.8%, 8%, 8.8%, 9.8%, 9.4%, 9.5%, 9.8%, 10%, 10.8%, 11.2%, 11.6%, 11.8%, 12%, 12.12%, 14.12%, 14.5%, 14.15.15.5%, 16%, 16.15.15%, 16%, 16.5%, 16%, 16.5%, 16%, 16.8%, 16%, 1.5%, 1.8%, 6%, 1.8%, 1.5%, 1.8%, 6%, 1.8%, 6%, 1.8%, 6%, 1.6%, 6%, 1.6%, 1.9.6%, 1.6%, 1.9%, 6%, 1.9.9.6%, 16%, 6%, 4%, 1.6%, 1.9.9.9.6%, 6%, 1.9.9.9.6%, 1.6%, 1.9%, 1.6%, 6%, 1.6%, 16%, 6%, 16%, 1.6%, 16%, 1.6%, 16%, 6%, 1.6%, 6%, 4%, 1.6%, 6%, 1.6%, 16%, 6%, 16%, 17.2%, 17.4%, 17.6%, 17.8%, 18%, 18.2%, 18.3%, 18.6%, 18.8%, 19%, 19.2%, 19.4%, 19.6%, 19.8%, 20%, and specific points between the above values, to the extent that space is limited and for the sake of brevity, the invention is not intended to be exhaustive of the specific points included in the recited ranges. Preferably, the urea is present in an amount of 0.001 to 10wt%, based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the trehalose is 0.001 to 10wt% based on the total weight of the moisturizing composition of the present invention, for example, may be 0.001%, 0.005%, 0.01%, 0.03%, 0.05%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.2%, 1.3%, 1.5%, 1.8%, 1.9%, 2%, 2.5%, 3%, 4%, 4.2%, 4.5%, 4.6%, 4.7%, 5%, 5.5%, 5.8%, 6%, 6.5%, 7%, 7.2%, 7.5%, 7.8%, 8%, 8.2%, 8.4%, 8%, 8.6%, 8.8%, 9%, 9.4%, 9.5%, 9.8%, 10%, and specific points between the above mentioned values are not included in the present invention and specific points between the above mentioned points are not included for brevity and for the sake of brevity and clarity. Preferably, the trehalose is 0.5 to 8wt% based on the total weight of the moisturizing composition of the present invention.
According to the present invention, the allantoin is 0.001 to 0.5wt%, for example, 0.001%, 0.005%, 0.006%, 0.008%, 0.009%, 0.1%, 0.15%, 0.16%, 0.18%, 0.19%, 0.2%, 0.21%, 0.22%, 0.25%, 0.28%, 0.29%, 0.3%, 0.35%, 0.38%, 0.4%, 0.45%, and 0.5% based on the total weight of the moisturizing composition of the present invention, and specific points between the above-mentioned values are not exhaustive list of the specific points included in the range, limited to space and for the sake of brevity. Preferably, the allantoin is 0.05 to 0.3wt% based on the total weight of the moisturizing composition of the present invention.
Further preferably, the moisturizing composition further comprises a preservative. The preservative is a conventional preservative in the field, and can be added and used in a proper amount according to the cosmetic use specification, preferably phenoxyethanol/ethylhexyl glycerol and/or caprylyl glycol.
Preferably, the preservative is present in an amount of 0.001 to 1wt%, based on the total weight of the composition of the present invention.
In a second aspect, the present invention provides a method for preparing the moisturizing composition, comprising the steps of:
1) adding sodium polyglutamate, Chondrus crispus and sodium hyaluronate into glycerol, stirring, adding into water, and heating to 70-90 deg.C to dissolve to obtain a first solution;
2) Adding L-serine into the first solution obtained in the step 1) for dissolving, adding a pH regulator to regulate the pH to 4.5-5.5, and stirring to obtain a second solution;
3) stirring and dissolving betaine and sodium pyrrolidone carboxylate, and adding the solution into the second solution obtained in the step 2).
Preferably, the moisturizing composition further comprises step 4): cooling the mixture obtained in the step 3) to below 40 ℃, adding urea and a preservative, stirring, filtering and discharging.
According to some preferred embodiments of the present invention, the moisturizing composition is prepared by a method comprising the steps of:
1) adding sodium polyglutamate, Chondrus crispus and sodium hyaluronate into glycerol, stirring, adding into water, and heating to 70-90 deg.C to dissolve to obtain a first solution;
2) adding L-serine and L-proline into the first solution obtained in the step 1) for dissolving, adding L-glutamic acid or other pH regulators to adjust the pH to 4.5-5.5, and stirring to obtain a second solution;
3) stirring and dissolving betaine, sodium pyrrolidone carboxylate, trehalose and allantoin, and adding into the second solution obtained in the step 2).
Preferably, the moisturizing composition further comprises step 4): cooling the mixture obtained in the step 3) to below 40 ℃, adding urea and a preservative, stirring, filtering and discharging.
The inventor tests that the heating step 1) and the pH adjusting step 2) are necessary in the preparation method of the invention, and the heating temperature and the pH value directly influence the form and the moisturizing effect of the moisturizing composition.
According to the invention, the sodium polyglutamate, the rugose carrageenan and the sodium hyaluronate are compounded to form a space net structure, and the space net structure has a loose porous structure. Amino acid has two groups of amino and carboxyl, is an ampholyte, and can react with different ionic substances due to the special structure of the ampholyte. By adjusting the pH value of the system, the system is lower than the isoelectric point of amino acid, the amino group on the amino acid has positive charge, and can simultaneously react with half ester sulfate group on the Chondrus crispus and carboxyl group on the polyglutamic acid, so that the amino acid is changed from being simply dissociated in a net structure to be tightly connected on a macromolecular structure, and a stable carrier structure is formed. Meanwhile, various small molecular moisturizers added in addition can be loaded on the carrier network structure, can be brought to the skin surface by the macromolecular carrier, and are slowly released, so that the synergistic effect is achieved, and the long-acting moisturizing effect is achieved.
Preservatives conventional in the art may be used in the present invention and are not particularly limited. In some embodiments of the invention, the preservative used is phenoxyethanol/ethylhexyl glycerol or caprylyl glycol; the preservative is used in an amount of 1wt% or less based on the total weight of the moisturizing composition.
In a third aspect, the present invention provides a long-acting moisturizing composition of the first aspect or a long-acting moisturizing composition obtained by the preparation process of the second aspect, wherein the long-acting moisturizing composition is applied to a skin care product.
Compared with the prior art, the invention has the beneficial effects that at least:
(1) the stable carrier structure of the composition can slowly release the loaded micromolecule humectant for a long time, fully exerts the moisturizing effect of the humectant and plays a remarkable and lasting moisturizing role;
(2) the components of the composition are synergistic, and the water replenishing and locking functions are obviously enhanced;
(2) the composition of the present invention gives a good feeling in use.
Drawings
FIG. 1 is a 100 XSEM image of a sample of the composition of example 1;
FIG. 2 is a photograph showing the water absorption effect of a sample of the composition of example 1;
FIG. 3 shows the results of the 48h mean change rate of skin moisture content over time for the samples according to Experimental group 1; according to the result that the change rate of the mean value of the skin moisture content of 48h of the sample of the experimental group 2 changes along with the time; according to the result that the change rate of the mean value of the skin moisture content of 48h of the sample of the experimental group 3 changes along with the time;
FIG. 4 shows the results of the change in skin moisture content over time for 48h of samples according to the experimental group; according to the result of the change of the skin moisture content of the sample 48h in the control group 1 along with the time; according to the result that the skin moisture content of the sample of the control group 2 changes with time within 48 h; according to the result that the skin moisture content of the sample of the control group 3 changes with time within 48 h; according to the result that the skin moisture content of the sample of the control group 4 changes with time within 48 h; according to the result that the skin moisture content of the sample of the control group 5 changes with time within 48 h; according to the result that the skin moisture content of the sample of the control group 6 changes with time within 48 h;
Fig. 5 shows sensory evaluation results of the experimental groups; sensory evaluation results of control 1; sensory evaluation results of control 2; sensory evaluation results of control 3.
The specific implementation mode is as follows:
to further illustrate the technical means and effects of the present invention, the present invention is further described with reference to the following examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. The examples, which are not specifically shown for the specific methods, are all routine in the art or according to the product specifications. The reagents or apparatus used are conventional products commercially available from normal sources, not indicated by the manufacturer.
Table 1 raw materials supplier list
Figure 897915DEST_PATH_IMAGE001
TABLE 2 Instrument information List
Figure 205269DEST_PATH_IMAGE002
Example 1: preparation of long-acting moisturizing composition
1) Adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) Weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding the obtained solution in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octyl glycol, stirring uniformly, filtering and discharging.
Example 2: preparation of long-acting moisturizing composition
1) Adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding into the solution obtained in the step 2);
4) Cooling to below 40 ℃, adding 0.4 weight part of preservative octyl glycol, stirring uniformly, filtering and discharging.
Example 3: preparation of Long-acting moisturizing composition
1) Adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 40 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine and 6 parts by weight of sodium pyrrolidone carboxylate, and adding the mixture into the solution obtained in the step 2), stirring and dissolving;
4) cooling to below 40 ℃, adding 0.4 weight part of preservative octyl glycol, stirring uniformly, filtering and discharging.
Example 4: preparation of long-acting moisturizing composition
1) Adding 0.3 part by weight of sodium polyglutamate (with a molecular weight of 50 ten thousand Da), 2 parts by weight of Chondrus crispus (with a molecular weight of 80 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (with a molecular weight of 50 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at a stirrer rotating speed of 300r/min, and simultaneously heating to 85 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) Weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding the obtained solution in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Example 5: preparation of long-acting moisturizing composition
1) Adding 0.3 part by weight of sodium polyglutamate (molecular weight of 150 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 150 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 150 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 75 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding the obtained solution in the step 2);
4) Cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Example 6: preparation of long-acting moisturizing composition
1) Adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 150 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 150 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding the obtained solution in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Example 7: preparation of long-acting moisturizing composition
1) Adding 0.3 part by weight of sodium polyglutamate (molecular weight of 80 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 85 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) Weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding the obtained solution in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Example 8: preparation of long-acting moisturizing composition
1) Adding 1 weight part of sodium polyglutamate (molecular weight is 50 ten thousand Da), 0.01 weight part of Chondrus crispus (molecular weight is 200 ten thousand Da) and 1 weight part of sodium hyaluronate (molecular weight is 100 ten thousand Da) into 15 weight parts of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 2 parts by weight of L-serine and 2 parts by weight of L-proline, adding into the medium obtained in the step 1), dissolving, adding L-glutamic acid, adjusting the pH value to 4.5-5.5, and uniformly stirring at a stirrer rotating speed of 300 r/min;
3) weighing 10 parts by weight of betaine, 10 parts by weight of sodium pyrrolidone carboxylate, 10 parts by weight of trehalose and 0.5 part by weight of allantoin, stirring and dissolving, and adding into the solution obtained in the step 2);
4) Cooling to below 40 ℃, adding 20 parts by weight of urea and 0.3 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Example 9: preparation of long-acting moisturizing composition
1) Adding 0.2 part by weight of sodium polyglutamate (with the molecular weight of 250 ten thousand Da), 5 parts by weight of Chondrus crispus (with the molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (with the molecular weight of 100 ten thousand Da) into 40 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1 part by weight of L-serine and 0.5 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of 300r/min of a stirrer;
3) weighing 5 parts by weight of betaine, 5 parts by weight of sodium pyrrolidone carboxylate, 10 parts by weight of trehalose and 0.1 part by weight of allantoin, stirring and dissolving, and adding into the solution obtained in the step 2);
4) cooling to below 40 ℃, adding 10 parts by weight of urea and 0.3 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Example 10: preparation of long-acting moisturizing composition
1) Adding 0.2 weight part of sodium polyglutamate (molecular weight of 100 ten thousand Da), 1 weight part of Chondrus crispus (molecular weight of 100 ten thousand Da) and 0.1 weight part of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 20 weight parts of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 75 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) Weighing 0.01 part by weight of L-serine and 0.5 part by weight of L-proline, adding into the solution obtained in the step 1), dissolving, adding L-glutamic acid, adjusting the pH value to 4.5-5.5, and uniformly stirring at a stirrer rotating speed of 300 r/min;
3) weighing 5 parts by weight of betaine, 5 parts by weight of sodium pyrrolidone carboxylate, 5 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding the mixture into the solution obtained in the step 2);
4) cooling to below 40 ℃, adding 5 parts by weight of urea and 0.5 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Example 11: preparation of long-acting moisturizing composition
1) Adding 2 parts by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 500 ten thousand Da) and 2 parts by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 40 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 85 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1 part by weight of L-serine, 0.01 part by weight of L-proline and 0.1 part by weight of L-glutamic acid, adding into the solution obtained in the step 1) for dissolving, adding citric acid and sodium hydroxide to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 5 parts by weight of betaine, 3 parts by weight of sodium pyrrolidone carboxylate, 5 parts by weight of trehalose and 0.1 part by weight of allantoin, stirring and dissolving, and adding the mixture into the solution obtained in the step 2);
4) Cooling to below 40 deg.C, adding urea 10 weight parts and antiseptic phenoxyethanol/ethylhexyl glycerol 0.5 weight parts, stirring, filtering, and discharging.
Example 12: preparation of long-acting moisturizing composition
1) Adding 1 weight part of poly-sodium glutamate (molecular weight 100 ten thousand Da), 1 weight part of Chondrus crispus (molecular weight 80 ten thousand Da) and 1 weight part of sodium hyaluronate (molecular weight 100 ten thousand Da) into 10 weight parts of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 70 ℃ until the solution is completely dissolved;
2) weighing 1.5 parts by weight of L-serine, 1 part by weight of L-proline and 0.1 part by weight of L-glutamic acid, adding into the solution obtained in the step 1) for dissolving, adding citric acid and sodium hydroxide to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 5 parts by weight of betaine, 5 parts by weight of sodium pyrrolidone carboxylate, 0.5 part by weight of trehalose and 0.1 part by weight of allantoin, stirring and dissolving, and adding into the solution obtained in the step 2);
4) cooling to below 40 deg.C, adding 5 weight parts of urea and 0.3 weight part of antiseptic phenoxyethanol/ethylhexyl glycerol, stirring, filtering, and discharging.
Example 13: preparation of long-acting moisturizing composition
1) Adding 0.01 weight part of sodium polyglutamate (molecular weight of 100 ten thousand Da), 3 weight parts of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.01 weight part of sodium hyaluronate (molecular weight of 5 ten thousand Da) into 8 weight parts of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 90 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 0.8 part by weight of L-serine, 1.8 parts by weight of L-proline and 0.1 part by weight of L-glutamic acid, adding into the solution obtained in the step 1), dissolving, adding citric acid and sodium hydroxide to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 0.2 part by weight of sodium pyrrolidone carboxylate, 1 part by weight of trehalose and 0.01 part by weight of allantoin, stirring and dissolving, and adding into the solution obtained in the step 2);
4) cooling to below 40 deg.C, adding 1 weight part of urea and 0.3 weight part of antiseptic phenoxyethanol/ethylhexyl glycerol, stirring, filtering, and discharging.
Example 14: preparation of long-acting moisturizing composition
1) Adding 0.01 weight part of sodium polyglutamate (molecular weight is 80 ten thousand Da), 3 weight parts of Chondrus crispus (molecular weight is 80 ten thousand Da) and 0.01 weight part of sodium hyaluronate (molecular weight is 50 ten thousand Da) into 8 weight parts of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 85 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) Weighing 0.8 part by weight of L-serine, 1.8 parts by weight of L-proline and 0.1 part by weight of L-glutamic acid, adding into the solution obtained in the step 1), dissolving, adding citric acid and sodium hydroxide to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 0.2 part by weight of sodium pyrrolidone carboxylate, 1 part by weight of trehalose and 0.01 part by weight of allantoin, stirring and dissolving, and adding the mixture into the solution obtained in the step 2);
4) cooling to below 40 deg.C, adding 1 weight part of urea and 0.3 weight part of antiseptic phenoxyethanol/ethylhexyl glycerol, stirring, filtering, and discharging.
Example 15: preparation of long-acting moisturizing composition
1) Adding 0.01 weight part of sodium polyglutamate (molecular weight is 50 ten thousand Da), 3 weight parts of Chondrus crispus (molecular weight is 80 ten thousand Da) and 0.01 weight part of sodium hyaluronate (molecular weight is 190 ten thousand Da) into 8 weight parts of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 85 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 0.8 part by weight of L-serine, 1.8 parts by weight of L-proline and 0.1 part by weight of L-glutamic acid, adding into the solution obtained in the step 1), dissolving, adding citric acid and sodium hydroxide to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) Weighing 4 parts by weight of betaine, 0.2 part by weight of sodium pyrrolidone carboxylate, 1 part by weight of trehalose and 0.01 part by weight of allantoin, stirring and dissolving, and adding into the solution obtained in the step 2);
4) cooling to below 40 ℃, adding 1 part of urea and 0.3 part of preservative phenoxyethanol/ethylhexyl glycerol by weight, stirring uniformly, filtering and discharging.
Example 16 preparation:
1) adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding the obtained solution in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea, stirring uniformly, filtering and discharging.
Example 17 preparation:
1) adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, and stirring at the rotating speed of 300r/min by using a stirrer;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the solution obtained in the step 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding the obtained solution in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Comparative example 1 preparation:
1) adding 2 parts by weight of Chondrus ocellatus (molecular weight 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by a stirrer, and simultaneously heating to 80 ℃ until the solution is completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the mixed solution obtained in the step 1), dissolving, adding L-glutamic acid, adjusting the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) Weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding into the mixed solution obtained in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Comparative example 2 preparation:
1) adding 0.3 part by weight of sodium polyglutamate (with a molecular weight of 100 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (with a molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerol, stirring and dispersing uniformly, adding into water, stirring at a stirrer rotating speed of 300r/min, and simultaneously heating to 80 ℃ until complete dissolution;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the mixed solution obtained in the step 1), dissolving, adding L-glutamic acid, adjusting the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding into the mixed solution obtained in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octyl glycol, stirring uniformly, filtering and discharging.
Comparative example 3 preparation:
1) Adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da) and 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by a stirrer, and heating to 80 ℃ until the solution is completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the mixed solution obtained in the step 1), dissolving, adding L-glutamic acid, adjusting the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding into the mixed solution obtained in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Comparative example 4 preparation:
1) adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) Weighing 4 parts by weight of betaine, 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding into the mixed solution obtained in the step 2);
3) cooling to below 40 ℃, adding 0.4 weight part of preservative octyl glycol, stirring uniformly, filtering and discharging.
Comparative example 5 preparation:
1) adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the system 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 6 parts by weight of sodium pyrrolidone carboxylate, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding into the mixed solution obtained in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
Comparative example 6 preparation:
1) Adding 0.3 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 2 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da) into 35 parts by weight of glycerin, stirring and dispersing uniformly, adding into water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) weighing 1.2 parts by weight of L-serine and 0.6 part by weight of L-proline, adding into the system 1) for dissolving, adding L-glutamic acid to adjust the pH value to 4.5-5.5, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
3) weighing 4 parts by weight of betaine, 4 parts by weight of trehalose and 0.2 part by weight of allantoin, stirring and dissolving, and adding into the mixed solution obtained in the step 2);
4) cooling to below 40 ℃, adding 8 parts by weight of urea and 0.4 part by weight of preservative octylene glycol, stirring uniformly, filtering and discharging.
First, the preparation process is optimized
The researchers of the invention study the preparation process of the moisturizing composition, and the preparation process is the same as that of the example 1 except that the temperature is different. The effect of different temperatures (normal temperature, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 95 ℃) on the performance of the moisturizing composition is compared and researched.
Product status and stability observations of the compositions prepared at different temperatures are given in the following table:
Figure 188268DEST_PATH_IMAGE003
From the above experimental results, it is understood that when the heating temperature is lower than 60 ℃, the obtained composition is poor in stability, uniformity and the like, and that the stability and the product state are good at 70 ℃ or higher. The stability, uniformity, fluidity, moldability and other properties of the composition have great influence on the performance of the carrier, and the heating temperature is preferably higher than 70 ℃ in the preparation process of the composition. In addition, although the solution is soluble at 95 ℃, on the one hand, the solution is prone to yellowing when heated at high temperatures for a long time, and on the other hand, the high temperatures cause energy waste for industrial production. Therefore, the preparation temperature of the moisturizing composition is preferably controlled to be 70-90 ℃.
Second, efficacy test
Composition space network-sustained release structure basis test
Experiment 1 Electron microscope Observation
The moisturizing composition prepared in example 1 was dried and observed under a Scanning Electron Microscope (SEM).
As can be seen from fig. 1, the composition prepared in example 1 forms a dense spatial network structure which increases the specific surface area of the entire composition and can adsorb and hold a variety of material components, confirming that the moisturizing composition of the present invention has a sustained release structural basis.
Experiment 2 Water absorption experiment
The experimental method comprises the following steps:
the composition prepared in example 1 was lyophilized, and then left to stand at room temperature to observe the state of water absorption, as shown in fig. 2a and 2b, which are the states of the samples after standing for 0min and 140min, respectively.
Comparing fig. 2a and fig. 2b, it can be seen that after standing for 0 and 140min at room temperature after freeze-drying, the sample largely absorbs water from the solid network structure and becomes liquid. The moisturizing composition disclosed by the invention is proved to have a strong water absorption effect, can continuously supply water to the surface of skin, and has a good water replenishing capacity.
(II) product Condition Observation of moisturizing composition
The product state and stability of the compositions prepared in the examples and comparative examples are observed, and the tested samples and the observed results are shown in the following table:
TABLE 4
Figure 849056DEST_PATH_IMAGE004
According to the observation results, the examples 1 to 4 and the comparative examples 1 to 6 have proper viscosity, good transparency, fine texture, proper fluidity and good film forming property, and are suitable for being applied to the field of skin care products.
The sample of example 16 is easily contaminated by microorganisms (becoming cloudy the next day), resulting in poor product stability; the example 17 shows that the preparation process of the sample is different from that of the example 1, the obtained composition has poor uniformity and stability, a transparent granular substance is separated out after the standing time is slightly long, and the long-time slow release basis is not provided, so that the heating process in the preparation process of the composition plays an important role in the performance of the product.
The inventor observes that the product state and stability of other embodiments achieve the same results as those of embodiment 1, and the observation results are not shown one by one in space limitation.
(III) moisturizing composition Long-acting moisturizing experiment for 48 hours
The moisturizing compositions prepared in examples 1 to 3 were formulated into emulsion formulations to be subjected to human moisturizing effect evaluation experiments, and the rate of change in skin moisture content of subjects after application of the moisturizing compositions was measured. The emulsion formulation and experimental methods are as follows:
experimental group 1: phase C moisturizing composition 5wt% of the composition prepared in example 1 was added;
experimental group 2: phase C moisturizing composition 5wt% of the composition prepared in example 2 was added;
experimental group 3: phase C moisturizing composition 5wt% of the composition prepared in example 3 was added.
Table 3 sensory evaluation experiment emulsion formula table
Figure 115959DEST_PATH_IMAGE006
The preparation process of the emulsion comprises the following steps:
(1) preparing in advance: the E-phase sodium hydroxide was prepared in advance as a 10% aqueous solution.
(2) Adding carbomer 940 into water for soaking phase A, and rapidly stirring to completely hydrate carbomer 940;
(3) adding the B phase KELTROL CG-T into pentanediol, stirring uniformly, slowly adding water, and stirring uniformly;
(4) adding the phase B and the phase C into the phase A, uniformly stirring, and heating the mixture to 80-85 ℃ for later use;
(5) uniformly mixing the phase D raw materials, and heating to 80-85 ℃ for later use;
(6) homogenizing phase A (3000 rpm), adding phase D into phase A, and homogenizing for 5 min;
(7) Stirring for half an hour at the temperature of 80-85 ℃;
(8) stirring and cooling, adding phase E at 50-55 deg.C, neutralizing until pH is 6.3-6.8, and stirring;
(9) adding the F-phase raw material at the temperature of below 45 ℃, and uniformly stirring;
the experimental method comprises the following steps: the test sample is smeared on the forearm, and the skin moisture content of the test sample is respectively measured after 4h, 8h, 24h and 48h before the test sample is used by the test subject.
As can be seen from the results in FIG. 3, the skin moisture content of the subjects was significantly increased after the samples of the experimental groups 1 to 3 were used, which indicates that the moisturizing composition of the present invention has a good moisturizing effect. At the same time. The moisturizing effect of the sample in the example 1 is slightly higher than that of the sample in the examples 2 and 3, and the moisturizing performance of the composition is improved by adding auxiliary moisturizing ingredients such as trehalose and allantoin.
(IV) 48h Long-acting moisturizing comparative experiment
The moisturizing compositions prepared in example 1 and comparative examples 1 to 6 were formulated into emulsion formulations to measure the average skin moisture content, and the emulsion formulation tables and experimental methods were as described in (iii).
The experimental samples were as follows:
experimental groups: phase C moisturizing composition 5wt% of the composition prepared in example 1 was added;
control group 1: phase C moisturizing composition 5wt% of the composition prepared in comparative example 1 was added;
control group 2: phase C moisturizing composition 5wt% of the composition prepared in comparative example 2 was added;
Control group 3: phase C moisturizing composition 5wt% of the composition prepared in comparative example 3 was added;
control group 4: phase C moisturizing composition 5wt% of the composition prepared in comparative example 4 was added;
control group 5: phase C moisturizing composition 5wt% of the composition prepared in comparative example 5 was added;
control group 6: phase C moisturizing composition 5wt% was added to prepare a composition of comparative example 6.
The experimental method comprises the following steps: the product was applied to the forearm, and the average skin moisture content was measured before and after application for 4h, 8h, 24h, and 48h, respectively, with the results shown in fig. 4.
As can be seen from fig. 4, the moisture content of the moisturizing composition samples of the experimental group (example 1) after 4h, 8h, 24h and 48h are obviously higher than that of the control groups 1 to 6, indicating that the moisturizing composition of the present invention has long-acting moisturizing effect. Meanwhile, the moisturizing effect of the control group 4-6 is obviously lower than that of the experimental group, and the control group 4-6 cannot achieve the long-acting moisturizing effect, so that the addition of amino acid, betaine, sodium pyrrolidone carboxylate and the like in the moisturizing composition improves the moisturizing effect of the composition.
(V) sensory evaluation experiment:
in the sensory evaluation experiment, screening, grouping training, test result investigation and the like of volunteers are strictly carried out according to the flow of sensory evaluation, and the volunteers can be grouped after qualified tissue grouping training.
Sensory evaluation samples: 15wt% of the composition of the example or the comparative example and the balance of water are mixed evenly to obtain a tested sample.
Experimental groups: 15wt% composition prepared in example 1 + balance water;
control group 1: 15wt% sample of the composition prepared in comparative example 1 + balance water;
control group 2: 15wt% comparative example 2 a sample of the composition + balance water was prepared;
control group 3: 15wt% comparative example 3 a sample of the composition was prepared + the balance water.
The experimental method comprises the following steps: the tested product is smeared on the surface of the skin, so that the use feeling of the tested product is graded by the moistening feeling, the soft feeling, the moistening feeling after absorption, the film forming property and the slippery feeling of a test person, wherein the use feeling of the tested product is best by 5, the use feeling of the tested product is evaluated by 0, and the result is shown in figure 5:
as can be seen from FIG. 5, the samples of the experimental group all had a higher feeling of use than the control group. The moisturizing composition has the effect of improving skin feel, so that the skin is moisturized, tender and smooth.
The control groups 1-3 are the compositions which lack sodium hyaluronate, sodium polyglutamate and carrageen crispus respectively, and the lack of macromolecular substances of the compositions not only has influence on the moisture retention performance, but also has great influence on the moistening feeling, the smooth feeling and the like of the compositions.
In conclusion, the moisturizing composition disclosed by the invention has the beneficial effects that the small molecular humectant slowly releases and synergizes through the synergistic effect of the sodium polyglutamate, the carrageen abomasum and the sodium hyaluronate and is compounded with other small molecular humectant amino acids, betaine and the like, so that the long-acting moisturizing effect is realized, the moisturizing composition has good usability and wide application prospects in skin care products.

Claims (5)

1. A moisturizing composition comprising glycerin, carrageen crispa, sodium polyglutamate, sodium hyaluronate, L-serine, sodium pyrrolidone carboxylate, betaine, and a pH adjusting agent;
based on the total weight of the moisturizing composition, the glycerin is 0.001-40wt%, the carrageen crispa is 0.01-5wt%, the sodium polyglutamate is 0.01-5wt%, the sodium hyaluronate is 0.01-5wt%, the L-serine is 0.01-2wt%, the sodium pyrrolidone carboxylate is 0.001-15wt%, the betaine is 0.001-15wt%, and the pH regulator is 0.001-5 wt%;
the molecular weight of the sodium polyglutamate is 100-150 ten thousand Da, the molecular weight of the Chondrus crispus is 150-250 ten thousand Da, and the molecular weight of the sodium hyaluronate is 100-150 ten thousand Da.
2. The moisturizing composition of claim 1, further comprising one or more of L-proline, L-glutamic acid, urea, trehalose, and allantoin.
3. The moisturizing composition of claim 2, wherein the L-proline is 0.01 to 2wt%, the L-glutamic acid is 0.001 to 0.3wt%, the urea is 0.001 to 20wt%, the trehalose is 0.001 to 10wt%, and the allantoin is 0.001 to 0.5wt%, based on the total weight of the composition.
4. A method for preparing the moisturizing composition of claim 1, comprising the step 1): adding sodium polyglutamate, Chondrus crispus and sodium hyaluronate into glycerol, mixing, adding into water, and heating to 70-90 deg.C to obtain a first solution; 2) adding L-serine into the first solution obtained in the step 1), adding a pH regulator, and regulating the pH to 4.5-5.5 to obtain a second solution; 3) adding betaine and sodium pyrrolidone carboxylate into the second solution obtained in the step 2).
5. Use of the moisturizing composition of any of claims 1 to 3 in the preparation of a skin care product.
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