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CN118203517B - Composition with slow release repairing function from natural sources and preparation method and application thereof - Google Patents

Composition with slow release repairing function from natural sources and preparation method and application thereof Download PDF

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Publication number
CN118203517B
CN118203517B CN202410290654.6A CN202410290654A CN118203517B CN 118203517 B CN118203517 B CN 118203517B CN 202410290654 A CN202410290654 A CN 202410290654A CN 118203517 B CN118203517 B CN 118203517B
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gel
homogenizing
pyrrolidone
composition
speed
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CN118203517A (en
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舒俊超
吴晚明
刘清连
谢格格
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Kelemei Guangzhou Biotechnology Co ltd
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Kelemei Guangzhou Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0216Solid or semisolid forms
    • A61K8/022Powders; Compacted Powders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/042Gels
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24Phosphorous; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4906Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
    • A61K8/4913Cosmetics 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
    • A61K8/498Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/673Vitamin B group
    • A61K8/675Vitamin B3 or vitamin B3 active, e.g. nicotinamide, nicotinic acid, nicotinyl aldehyde
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/676Ascorbic acid, i.e. vitamin C
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/68Sphingolipids, e.g. ceramides, cerebrosides, gangliosides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/733Alginic acid; Salts thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/48Thickener, Thickening system
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    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/522Antioxidants; Radical scavengers
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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Abstract

The invention belongs to the technical field of skin care products and preparation thereof, and discloses a composition with a slow release repairing function from natural sources, a preparation method and application thereof. The composition is prepared from the following raw materials in parts by weight: 50-60 parts of carrageenan gel, 20-30 parts of rhizobia gel and 10-30 parts of hydrolyzed algin gel; the carrageenan gel is prepared by crosslinking carrageenan extract, sodium pyrrolidone carboxylate and water; the rhizobia gel is prepared by crosslinking rhizobia gel, pyrrolidone magnesium carboxylate and water; the hydrolyzed algin gel is prepared by crosslinking hydrolyzed algin tetrasodium pyrophosphate, pyrrolidone calcium carboxylate and water. The preparation method adopts specific preparation process steps and addition sequence to obtain the multi-crosslinked composition gel, and then the powder mixture is prepared by low-temperature vacuum drying. The powder mixture has slow release active substances, self-repairing effect, and can be used for thickening and suspending.

Description

Composition with slow release repairing function from natural sources and preparation method and application thereof
Technical Field
The invention belongs to the technical field of skin care products and preparation thereof, and particularly relates to a composition with a slow release repairing function from natural sources, a preparation method and application thereof.
Background
The functional substances generally have the characteristics of strong effect, quick action, high osmotic concentration and the like, and have the advantages of instant effect, quick and effective effect, and the defects of overlarge local concentration, strong irritation and non-lasting effect. Slow release of functional targets is therefore becoming an important issue. At present, the slow release technology is widely and ripely applied in the medicine and food industries. The existing sustained release technology without changing chemical properties is mainly divided into the following categories: 1. solid dispersion sustained release, such as tablets; 2. coating sustained release, such as capsule, coating, and film forming; 3. liquid suspensions, such as suspensions; 4. changing particle size, such as nanocrystallization; 5. semisolid, such as jelly gel. The food and the medicine mainly take effect orally, are applied to less products related to skin, and many slow release technologies are not applicable to skin care product production, so that the use situations are quite different.
The prior slow release technology has the following defects aiming at the production of skin care products:
A. the application method is not suitable, if solid slow release is not suitable for skin;
B. the material is not well-suited to the skin, such as coatings, semi-solids, etc.;
C. if the suspension is not a stable system, the suspension is not suitable for skin care products;
D. Nanocrystallized additives are unhealthy, and if synthetic emulsifiers are not allowed to be added to skin care products.
Disclosure of Invention
In order to overcome the drawbacks and disadvantages of the prior art, a primary object of the present invention is to provide a composition with sustained release repair function from natural sources; the composition selects natural green healthy raw materials, the product is easy to dissolve in water to form liquid with certain consistency after being prepared into powder, the composition has the function of repairing skin, has good affinity with skin, is convenient to use, is easy to apply and has no rubbing, and the stability is particularly good when in application.
The invention also aims to provide a preparation method of the composition with the sustained-release restoration function.
Still another object of the present invention is to provide an application of the composition with sustained release repairing function from the above natural source.
The aim of the invention is achieved by the following technical scheme:
The composition with the sustained-release repairing function is prepared from the following raw materials in parts by weight: 50-60 parts of carrageenan gel, 20-30 parts of rhizobia gel and 10-30 parts of hydrolyzed algin gel;
The carrageenan gel is prepared by crosslinking carrageenan extract, sodium pyrrolidone carboxylate and water;
the rhizobia gel is prepared by crosslinking rhizobia gel, pyrrolidone magnesium carboxylate and water;
the hydrolyzed algin gel is prepared by crosslinking hydrolyzed algin tetrasodium pyrophosphate, pyrrolidone calcium carboxylate and water.
The preparation method of the composition with the sustained-release restoration function from the natural source comprises the following operation steps:
(1) Respectively preparing carrageenan gel, rhizobia gel and hydrolyzed algin gel;
(2) Weighing 50-60 parts by weight of carrageenan gel, 20-30 parts by weight of rhizobia gel and 10-30 parts by weight of hydrolyzed algin gel; putting half weight of carrageenan gel into stirring homogenizing equipment, starting homogenizing at 5000-8000r/min at medium speed, putting half weight of rhizobia gel while homogenizing, stirring for 10-15min, continuing to start homogenizing at 5000-8000r/min at medium speed, putting 5-15g half weight of hydrolyzed algin gel while homogenizing, and stirring for 10-15min to obtain preliminarily crosslinked gel;
(3) Continuously starting 5000-8000r/min medium-speed homogenizing in the preliminarily crosslinked gel, adding the rest half weight of carrageenan gel while homogenizing, starting 5000-8000r/min medium-speed homogenizing after stirring for 10-15min, adding the rest half weight of rhizobia gel while homogenizing, continuously starting 5000-8000r/min medium-speed homogenizing after stirring for 10-15min, adding the rest half weight of hydrolyzed algin gel while homogenizing, and stirring for 10-15min to obtain multiple crosslinked composition gel;
(4) And (3) performing vacuum low-temperature drying on the multi-crosslinked composition gel obtained in the step (3) for 1-3h at the vacuum degree of 0.06-0.1 MPa and the temperature of 55-70 ℃, crushing the dried composition, and sieving the crushed composition with a 800-100-mesh screen to obtain the composition with the slow-release repairing function from natural sources.
The carrageenan gel of step (1) is prepared according to the following steps: sprinkling the carrageenan extract into 80-90 ℃ hot water which is subjected to low-speed homogenization at a speed of 3000-5000r/min, then starting 30-50r/min, uniformly stirring, adding pyrrolidone sodium carboxylate (PCA sodium) solution, carrying out low-speed homogenization at a speed of 2000-3000r/min for 3-5min, and then stirring and cooling to 40-45 ℃ to obtain carrageenan gel; the pyrrolidone sodium carboxylate solution is obtained by dissolving pyrrolidone sodium carboxylate (PCA sodium) with water of which the mass is 5 times that of the pyrrolidone sodium carboxylate; the use amounts of the carrageenan extract, 80-90 ℃ hot water and sodium pyrrolidone carboxylate are as follows by mass percent: 96.50-97.90%, 2.00-3.25% and 0.10-0.25%;
The rhizobium gel is prepared according to the following steps: sprinkling rhizobia gel into 80-90 ℃ hot water which is homogenized at a low speed of 3000-5000r/min, stirring uniformly at a speed of 30-50r/min, adding pyrrolidone magnesium carboxylate (PCA magnesium) solution, homogenizing at a low speed of 2000-3000r/min for 3-5min, and stirring and cooling to 40-45 ℃ to obtain rhizobia gel; the pyrrolidone carboxylic acid magnesium solution is obtained by dissolving pyrrolidone carboxylic acid magnesium (PCA magnesium) with water of which the mass is 5 times that of the pyrrolidone carboxylic acid magnesium; the rhizobia gum, 80-90 ℃ hot water and pyrrolidone magnesium carboxylate are used in the following mass percent: 96.40-97.70%, 2.00-3.25% and 0.30-0.60%;
The hydrolyzed algae gel is prepared according to the following steps: sprinkling the hydrolyzed algin into 80-90 ℃ hot water which is started to be homogenized at a low speed of 3000-5000r/min, starting to be stirred uniformly at a speed of 30-50r/min, adding tetrasodium pyrophosphate solution, homogenizing at a low speed of 2000-3000r/min for 3-5min, adding pyrrolidone calcium carboxylate (PCA calcium) solution, homogenizing at a low speed of 2000-3000r/min for 3-5min, and stirring and cooling to 40-45 ℃ to obtain hydrolyzed algin; the tetrasodium pyrophosphate solution is obtained by dissolving 0.3-0.5% of tetrasodium pyrophosphate with 5 times of water, and the pyrrolidone calcium carboxylate solution is obtained by dissolving 0.2-0.3% of pyrrolidone calcium carboxylate (PCA calcium) with 5 times of water; the use amounts of the hydrolyzed algin, the hot water at 80-90 ℃ and the tetrasodium pyrophosphate and the pyrrolidone calcium carboxylate are calculated according to the following mass percentages: 96.00-97.50%, 2.00-3.25%, 0.30-0.60% and 0.20-0.325%.
The composition with the slow release repairing function from the natural source is applied to the preparation of skin care products.
The skin care product can also contain functional substances.
The functional substances are ascorbyl tetraisopalmitate (with whitening and antioxidant functions), nicotinamide, ceramide, glabridin, etc.
The composition of the invention selects biological source sugar gum rhizobium gum, aquatic plant sugar gum carrageenan and hydrolyzed algin as main raw materials, the raw materials have the advantages of network structure, cross-linking formation of space structure, good suspension capacity, better thickening capacity and good moisture absorption and water retention effects, firstly, the raw materials and different metal ions form hydrogel at different temperatures, multiple cross-linked composition gel is obtained by adopting specific preparation process steps and adding sequence, and then the powder mixture is prepared by low-temperature vacuum drying. The powder mixture has slow release active substances and self-repairing effect, can be applied to thickening and suspending, and can be widely applied to cosmetic water, essence, emulsion, cream and the like.
Compared with the prior art, the invention has the following advantages and effects:
(1) The invention adopts natural materials, is green and safe, and is suitable for skin;
(2) The invention prepares the product with better slow release function by compounding and multiple crosslinking of the raw materials;
(3) The product has a repairing function, and no additional repairing functional component is added;
(4) The product of the invention has a repairing function and an excellent slow-release function, so that the product can be obviously synergistic when being matched with other functional components for use.
Drawings
FIG. 1 is a comparison of cell morphologies.
Fig. 2 is a scratch image display diagram.
FIG. 3 is a graph of cell scratch mobility results.
FIG. 4 is a graph showing the results of melanin synthesis-inhibiting rates.
FIG. 5 is a graph of the results of an inhibition capability test of ROS.
Detailed Description
The present invention is further illustrated below in conjunction with specific examples, but should not be construed as limiting the invention.
The compositions with slow release repair function of natural sources described in examples 1-4 below were prepared according to the following procedures:
(1) Sprinkling the carrageenan extract into 80-90deg.C water which is homogenized at a low speed of 3000-5000r/min to obtain phase A; then stirring uniformly by opening 30-50r/min, adding aqueous solution of sodium pyrrolidone carboxylate (namely A1 phase), homogenizing at a low speed of 2000-3000r/min for 3-5min, and stirring and cooling to 40-45 ℃ to obtain carrageenan gel;
(2) Sprinkling rhizobia gel into 80-90 ℃ water which is homogenized at a low speed of 3000-5000r/min to obtain phase B; stirring uniformly at 30-50r/min, adding aqueous solution of pyrrolidone magnesium carboxylate (namely B1 phase), homogenizing at low speed of 2000-3000r/min for 3-5min, and stirring and cooling to 40-45deg.C to obtain rhizobia gel;
(3) Sprinkling the hydrolyzed algin into 80-90deg.C water which is homogenized at a low speed of 3000-5000r/min to obtain phase C; stirring uniformly at a speed of 30-50r/min, adding an aqueous solution of tetrasodium pyrophosphate (namely C1 phase), homogenizing at a low speed of 2000-3000r/min for 3-5min, adding an aqueous solution of calcium pyrrolidone carboxylate (namely C2 phase), homogenizing at a low speed of 2000-3000r/min for 3-5min, and stirring and cooling to 40-45 ℃ to obtain hydrolyzed algae gel;
(4) Putting half of the carrageenan gel obtained in the step (1) into stirring homogenizing equipment, starting to homogenize at a medium speed of 5000-8000r/min, putting half of the rhizobia gel obtained in the step (2) while homogenizing, continuing to start to homogenize at a medium speed of 5000-8000r/min after stirring for 10min, putting half of the hydrolyzed algin gel obtained in the step (3) while homogenizing, and stirring for 10min to obtain preliminarily crosslinked gel;
(5) Continuously starting 5000-8000r/min medium-speed homogenization into the primarily crosslinked gel, adding the rest half weight of carrageenan gel while homogenizing, stirring for 10min, starting 5000-8000r/min medium-speed homogenization, adding the rest half weight of rhizobia gel while homogenizing, stirring for 10min, continuously starting 5000-8000r/min medium-speed homogenization, adding the rest half weight of hydrolyzed algin gel while homogenizing, and stirring for 10min to obtain multiple crosslinked composition gel;
(6) And (3) carrying out vacuum low-temperature drying on the multi-crosslinked composition gel obtained in the step (5) for 1-3h at the vacuum degree of 0.06-0.1 MPa and the temperature of 55-70 ℃, crushing the dried composition, and sieving the crushed composition with a 800-100-mesh screen to obtain the composition with the slow-release repairing function from natural sources.
Example 1
The composition with the sustained-release repairing function is prepared from the following raw materials in percentage by weight:
Example 2
The composition with the sustained-release repairing function is prepared from the following raw materials in percentage by weight:
Example 3
The composition with the sustained-release repairing function is prepared from the following raw materials in percentage by weight:
Example 4
The composition with the sustained-release repairing function is prepared from the following raw materials in percentage by weight:
Comparative example 1: the composition is prepared without metal ion crosslinking, and is prepared from the following raw materials in percentage by weight:
steps (4) to (6) of this comparative example are identical to examples 1 to 4 described above, except that no metal ion is added for crosslinking in steps (1) to (3), specifically according to the following steps:
(1) Sprinkling the carrageenan extract into 80-90deg.C water which is homogenized at a low speed of 3000-5000r/min to obtain phase A; then stirring and cooling to 40-45 ℃ to obtain carrageenan gel;
(2) Sprinkling rhizobia gel into 80-90 ℃ water which is homogenized at a low speed of 3000-5000r/min to obtain phase B; then stirring and cooling to 40-45 ℃ to obtain rhizobium gel;
(3) Sprinkling the hydrolyzed algin into 80-90deg.C water which is homogenized at a low speed of 3000-5000r/min to obtain phase C; then stirring and cooling to 40-45 ℃ to obtain the hydrolyzed algae gelling gum.
Comparative example 2: removing hydrolyzed algin to prepare a composition, wherein the composition is prepared from the following raw materials in percentage by weight:
steps (1), (2) and (6) of this comparative example are identical to examples 1 to 4 described above, except that hydrolyzed phycocolloids are not used, i.e., step (3) is removed, and steps (4) and (5) are removed and hydrolyzed phycocolloids gel is added.
Comparative example 3: removing rhizobia gum to prepare a composition, wherein the composition is prepared from the following raw materials in percentage by weight:
Steps (1), (3) and (6) of this comparative example are identical to examples 1 to 4 described above, except that hydrolyzed algin is not used, i.e., the step of removing step (2) and the step of adding rhizobia gel in steps (4) and (5) are removed.
Comparative example 4: removing carrageenan to prepare a composition which is prepared from the following raw materials in percentage by weight:
Steps (2), (3) and (6) of this comparative example are identical to examples 1 to 4 described above, except that no hydrolyzed algin is used, i.e., the step of adding carrageenan gel in step (1) and steps (4) and (5) are removed.
Comparative example 5: the hydrolyzed algin is replaced by sodium alginate, and the prepared composition is prepared from the following raw materials in percentage by weight:
Steps (1), (2) and (6) of this comparative example are identical to examples 1 to 4 described above, except that the hydrolyzed algin in step (3) is replaced with sodium alginate to prepare sodium alginate gel, and the hydrolyzed algin added in steps (4) and (5) is replaced with sodium alginate gel obtained in step (3).
Comparative example 6: the rhizobia gum is replaced by xanthan gum, and the prepared composition is prepared from the following raw materials in percentage by weight:
Steps (1), (3) and (6) of this comparative example are identical to examples 1 to 4 described above, except that the rhizobia gum in step (4) is replaced with xanthan gum to prepare xanthan gum gel, and the rhizobia gel added in steps (4) and (5) is replaced with xanthan gum gel obtained in step (3).
Comparative example 7: the carrageenan is replaced by the polysaccharide of Euglena parvula (EUGLENA GRACILIS), and the prepared composition is prepared from the following raw materials in percentage by weight:
steps (2), (3) and (6) of this comparative example are identical to examples 1 to 4 described above, except that the extract of Chondrus crispus in step (1) is replaced with the fine Euglena polysaccharide to prepare fine Euglena polysaccharide gel, and the carrageenan gel added in steps (4) and (5) is replaced with the fine Euglena polysaccharide gel obtained in step (3).
Effect example 1: repair function contrast
1) HaCat cells were selected for the cell scratch test. The concentration of the test substance suitable for the scratch test is firstly screened, namely the cytotoxicity concentration of the test substance is detected.
The MTT method is adopted to detect the activity of the cells, and the maximum safe concentration of the cell sample is screened. The experiments were run with a blank (medium) and zeroed wells (PBS), sample concentration settings are shown in table 1, with 6 replicate wells per concentration setting. The specific operation steps are as follows:
(1) Inoculating: taking cells in logarithmic growth phase, inoculating the cells to a 96-well culture plate, and placing the culture plate in a 5% CO2 incubator at 37 ℃ for incubation for 18-24 hours.
(2) Test substances of different concentrations were prepared with the complete medium at the concentration settings in table 1.
TABLE 1 sample cytotoxicity concentration setting
(3) Sample feeding: after 18-24h of cell growth, the supernatant was discarded, medium containing different concentrations of the test substance was added, and the plates were placed in a 5% CO2 incubator at 37℃for incubation for 18-24h.
(4) And (3) detection: after 18-24h of cell culture, the supernatant was discarded, and the formulated and filtered MTT (0.5 mg/mL) was added, gently mixed, and incubated at 37℃for 4h in the absence of light. After the incubation, the supernatant was discarded, 100. Mu.L of DMSO was added to each well, and the wells were shaken for 10min, and the OD 490 nm was read with an ELISA reader.
(5) Relative cell viability calculation formula:
(6) Morphology judgment picture shows that as shown in fig. 1, cell scratch test was performed by screening out 0.16% concentration, which is not cytotoxic.
2) Scratch test detection based on HaCaT cells.
(1) Inoculating: cells were first inoculated into 24-well plates with a sign pen from a ruler against two vertical lines, 37 ℃ and incubated overnight in a 5% co2 incubator.
(2) Scoring: after cells were plated in 24-well plates for 18-24h, each well was scored with a 1mL gun head against a ruler, perpendicular to the back transverse line, two wells were scored, the supernatant discarded, and washed three times with PBS to remove scored cells.
(3) Preparing liquid: test and positive controls were formulated according to table 2.
Table 2 test grouping and concentration settings
Note that: the sample set contained the compositions obtained in examples 1-4 and comparative examples 1-7.
(4) Dosing and photographing: the prepared samples were added to the corresponding positions of the 24-well plates for administration, and photographed under a 4X mirror for 0h (immediately). The plates were incubated at 37℃under 5% CO2 for 18-24h.
(5) Photographing and image analysis: after cell culture for 24h, the cells were photographed again under a 4X mirror at the same position as at 0h, after which migration area analysis was performed with image J.
(6) Cell mobility calculation: calculated from the cell mobility formula, the calculation formula is as follows:
wherein A 0 refers to the blank area when photographing for 0h, and A 24 refers to the blank area of the photographed picture when photographing for 24 h.
(7) And (3) data processing: various data obtained in the test were processed and plotted by Excel software. Statistical analysis was performed with SPSS17.0, and group comparisons were performed using one-way analysis of variance (ANOVA), with significant differences being judged when P <0.05, and with very significant differences being judged when P < 0.01.
(8) Scratch images were displayed as shown in fig. 2, and cell scratch mobilities were shown in table 3 and fig. 3:
TABLE 3 cell scratch mobility
As can be seen from table 3 and fig. 3: the composition with the slow-release repairing function has remarkable repairing effect, and mainly depends on raw material collocation, crosslinking and functional enhancement after multiple crosslinking.
Effect example 2: contrast of sustained release function
Application and efficacy addition: 2g of the composition powder obtained in examples 1-4 and comparative examples 1-7 are weighed respectively, slowly spread into a hot water container which is opened for 3000-5000r/min and is homogenized at a low speed, 95g of the composition powder is heated to 80-90 ℃, 0.5g of p-hydroxyacetophenone is added, the mixture is homogenized and cooled to 40-45 ℃, and 2g of tetraisopalmitate of ascorbic acid and 0.5g of 1, 2-hexanediol are added to obtain the slow-release brightening essence.
1) Function synergy: b16 cell melanin synthesis inhibition experiments were tested in vitro using TSHRH 027-2019, with each 100g of medium containing 8g of the subject slow-release lightening essence. The positive control selected 0.35% of alpha-arbutin.
TABLE 4 melanin synthesis inhibition rate
The results are shown in table 4 and fig. 4, and it can be seen from the experimental results that the composition with slow release repairing function of the present invention has excellent function in terms of function synergy, and compared with comparative examples 1-7, the compositions obtained in examples 1-4 of the present invention have more remarkable effects of enhancing melanin synthesis inhibition.
2) And (3) slow release effect test: skin irritation
The tests were carried out according to 5.3 skin irritation test methods of GB 7919-87 cosmetic safety evaluation procedure and method. 10 guinea pigs per sample were selected and the above-described essence was applied once.
The evaluation mode is according to the following standard:
skin irritation response score:
erythema formation: no erythema was 0 score, barely visible as 1 score, apparent erythema was 2 score, medium-severe erythema was 3 score, purplish red erythema and eschar formation was 4 score.
Edema formation: no edema was 0 minutes, barely visible as1 minute, skin doming profile clearly was 2 minutes, edema doming was about 1mm to 3 minutes, edema doming exceeded 1mm and the range was enlarged to 4 minutes.
Skin irritation intensity score:
The non-irritation is 0-0.4 point, the light irritation is 0.5-1.9 point, the medium irritation is 2.0-5.9 point, and the strong irritation is 6.0-8.0 point.
TABLE 5 skin irritation intensity scoring results
As can be seen from Table 5 above, the compositions obtained in examples 1-4 were all non-irritating and the compositions obtained in comparative examples 1-7 were all slightly irritating. Analysis: because the local and instantaneous active matter concentration is too high, the product has strong skin irritation, and the more uniform the release, the slower the release, the lower the irritation and the longer the effect are, thus proving that the composition with the slow release repairing effect has good repairing and slow release effects.
3) The antioxidant function persistence and effect were tested by selecting the inhibition ability of ROS in 5.2 photoaging-induced cells in the evaluation cell evaluation method for antioxidant activity of T/GDCA 012-2021 cosmetic. Each 100g of culture medium contains 8g of slow-release brightening essence of a tested object, and the effective duration and the slow-release degree are judged by controlling the UVB irradiation duration to obtain different inhibition rates.
TABLE 6ROS inhibition test results
From the data in Table 6 and FIG. 5 above, it is shown that the compositions of examples 1-4 and comparative examples 1-7 provide a ROS inhibiting effect comparable, but the compositions of examples 1-4 provide a long lasting effect on ROS inhibition, demonstrating that the antioxidant activity, ascorbyl tetraisopalmitate, is a good aid in the release of the active after treatment with the compositions of the present invention having a sustained release healing effect.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (4)

1. A composition of natural origin having a sustained release repair function, characterized in that: the composition is prepared from the following raw materials in parts by weight: 50-60 parts of carrageenan gel, 20-30 parts of rhizobia gel and 10-30 parts of hydrolyzed algin gel;
The composition with the slow release repair function from the natural source is prepared according to the following operation steps:
(1) Respectively preparing carrageenan gel, rhizobia gel and hydrolyzed algin gel;
(2) Weighing 50-60 parts by weight of carrageenan gel, 20-30 parts by weight of rhizobia gel and 10-30 parts by weight of hydrolyzed algin gel; putting half weight of carrageenan gel into stirring homogenizing equipment, starting homogenizing at 5000-8000r/min at medium speed, putting half weight of rhizobia gel while homogenizing, stirring for 10-15min, continuing to start homogenizing at 5000-8000r/min at medium speed, putting half weight of hydrolyzed algin gel while homogenizing, and stirring for 10-15min to obtain primary crosslinked gel;
(3) Continuously starting 5000-8000r/min medium-speed homogenizing in the preliminarily crosslinked gel, adding the rest half weight of carrageenan gel while homogenizing, starting 5000-8000r/min medium-speed homogenizing after stirring for 10-15min, adding the rest half weight of rhizobia gel while homogenizing, continuously starting 5000-8000r/min medium-speed homogenizing after stirring for 10-15min, adding the rest half weight of hydrolyzed algin gel while homogenizing, and stirring for 10-15min to obtain multiple crosslinked composition gel;
(4) The multi-crosslinked composition gel obtained in the step (3) is dried for 1 to 3 hours under vacuum at a vacuum degree of between 0.06 and 0.1MPa and a temperature of between 55 and 70 ℃, and the dried composition is crushed and then passes through a screen with 800 to 100 meshes to obtain the composition with the slow release repairing function from natural sources;
The carrageenan gel of step (1) is prepared according to the following steps: sprinkling the carrageenan extract into 80-90 ℃ hot water which is subjected to low-speed homogenization at a speed of 3000-5000r/min, then starting 30-50r/min, uniformly stirring, adding pyrrolidone sodium carboxylate solution, homogenizing at a speed of 2000-3000r/min for 3-5min, and then stirring and cooling to 40-45 ℃ to obtain carrageenan gel; the pyrrolidone sodium carboxylate solution is obtained by dissolving pyrrolidone sodium carboxylate with water of which the mass is 5 times that of the pyrrolidone sodium carboxylate; the use amounts of the carrageenan extract, 80-90 ℃ hot water and sodium pyrrolidone carboxylate are as follows by mass percent: 96.50-97.90%, 2.00-3.25% and 0.10-0.25%;
The rhizobia gel in the step (1) is prepared according to the following steps: sprinkling rhizobia gel into 80-90 ℃ hot water which is subjected to low-speed homogenization at a speed of 3000-5000r/min, stirring uniformly at a speed of 30-50r/min, adding pyrrolidone magnesium carboxylate solution, homogenizing at a speed of 2000-3000r/min for 3-5min, and then stirring and cooling to 40-45 ℃ to obtain rhizobia gel; the pyrrolidone magnesium carboxylate solution is obtained by dissolving pyrrolidone magnesium carboxylate with water of which the mass is 5 times that of the pyrrolidone magnesium carboxylate; the rhizobia gum, 80-90 ℃ hot water and pyrrolidone magnesium carboxylate are used in the following mass percent: 96.40-97.70%, 2.00-3.25% and 0.30-0.60%;
The hydrolyzed algae gelling gum in the step (1) is prepared according to the following steps: sprinkling the hydrolyzed algin into 80-90 ℃ hot water which is started to be homogenized at a low speed of 3000-5000r/min, starting to be stirred uniformly at a speed of 30-50r/min, adding tetrasodium pyrophosphate solution, homogenizing at a low speed of 2000-3000r/min for 3-5min, adding pyrrolidone calcium carboxylate solution, homogenizing at a low speed of 2000-3000r/min for 3-5min, and stirring and cooling to 40-45 ℃ to obtain hydrolyzed algin; the tetrasodium pyrophosphate solution is obtained by dissolving 0.3-0.5% of tetrasodium pyrophosphate with 5 times of water, and the pyrrolidone calcium carboxylate solution is obtained by dissolving 0.2-0.3% of pyrrolidone calcium carboxylate with 5 times of water; the use amounts of the hydrolyzed algin, the hot water at 80-90 ℃ and the tetrasodium pyrophosphate and the pyrrolidone calcium carboxylate are calculated according to the following mass percentages: 96.00-97.50%, 2.00-3.25%, 0.30-0.60% and 0.20-0.325%.
2. The use of a composition of natural origin having a sustained release repair function according to claim 1 for the preparation of skin care products.
3. The use according to claim 2, characterized in that: the skin care product also comprises functional substances.
4. A use according to claim 3, characterized in that: the functional substance is ascorbyl tetraisopalmitate, nicotinamide, ceramide or glabridin.
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CN109276513A (en) * 2018-10-12 2019-01-29 诺斯贝尔化妆品股份有限公司 A kind of composite plant oil-control bilayer surfactant at Han You le bamboo powder end
CN112294682A (en) * 2019-07-31 2021-02-02 太和康美(北京)中医研究院有限公司 Composition and preparation method and application thereof

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KR101296754B1 (en) * 2010-08-13 2013-08-20 신현우 A Hydrogel Composition For Transdermal Administration of Drug
CN113244224B (en) * 2021-05-27 2022-06-03 中南林业科技大学 Ellagic acid sustained-release gel and preparation method and application thereof
CN114796050B (en) * 2022-04-27 2024-07-09 蓓悠清(广东)健康科技有限公司 Gel mask with high-efficiency moisturizing and relieving functions and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN109276513A (en) * 2018-10-12 2019-01-29 诺斯贝尔化妆品股份有限公司 A kind of composite plant oil-control bilayer surfactant at Han You le bamboo powder end
CN112294682A (en) * 2019-07-31 2021-02-02 太和康美(北京)中医研究院有限公司 Composition and preparation method and application thereof

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