CN113876625A - Fucoidin-based long-acting moisturizing and antioxidant eye cream and preparation method thereof - Google Patents
Fucoidin-based long-acting moisturizing and antioxidant eye cream and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of cosmetics, and provides fucoidin-based long-acting moisturizing and antioxidant eye cream and a preparation method thereof. The eye cream disclosed by the invention takes fucoidin, sodium hyaluronate cross-linked polymer, sodium alginate, oat beta-glucan, polyglutamic acid, betaine and tremella polysaccharide as moisturizing components, wherein a layer of water-locking barrier can be formed on the surface of skin by the combination of the fucoidin and the sodium hyaluronate cross-linked polymer, so that the moisturizing duration is effectively prolonged, and the eye cream has excellent long-acting moisturizing effect; fucoidin, salvia miltiorrhiza root extract, peony root extract, angelica root extract, camellia extract, tea polyphenol and ascorbic acid are used as antioxidant ingredients, so that the eye cream has excellent antioxidant activity. The eye cream formula provided by the invention does not contain alcohol, has small irritation, can reduce the problems of skin allergy and tissue inflammation, and is suitable for a wide range of people. In addition, the fucoidin has good antibacterial activity, so that the eye cream has antibacterial and anti-inflammatory effects.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to fucoidin-based long-acting moisturizing and antioxidant eye cream and a preparation method thereof.
Background
The stratum corneum of the skin around the eyes is extremely thin, so that the skin around the eyes is extremely vulnerable. Therefore, the care of eye skin is particularly important. Common ocular problems are: the dry lines caused by water shortage increase the free radicals of the eye skin due to ultraviolet rays and air pollution, so that the eye skin becomes dark and senilism. Therefore, moisturizing and antioxidant properties are particularly important for eye care. Generally, eye creams are thick and heavy, and cannot be completely absorbed by eye skin; moreover, the frequency of use of the eye cream within a day cannot exceed 2 times; therefore, the long-acting moisturizing and antioxidant capacity of the eye cream is very important.
Fucoidin is a water-soluble polysaccharide, is extracted from marine algae, has various biological activities due to unique chemical structure, contains chelated heavy metal ions and has hydrophilic physicochemical properties, so that the fucoidin can be easily added into emulsion and paste preparations, and is particularly applied to the preparation of eye creams. Patent publication No. CN111991267A discloses a moisturizing and wrinkle-resisting eye cream which is prepared from the following raw materials: fucoidin, syn-coll, GATULINEIN-TENSE, glycerin, sorbitol, stearate group, emulsifier, softener, cetostearyl alcohol, thickener, vitamin E acetate, skin feeling regulator, anti-allergy agent, chelating agent, phenoxyethanol, ethylhexyl glycerin, essence and deionized water. However, the above moisturizing anti-wrinkle eye cream has poor long-lasting moisturizing properties.
Disclosure of Invention
In view of the above, the present invention aims to provide a fucoidin-based long-acting moisturizing and antioxidant eye cream and a preparation method thereof. The eye cream provided by the invention has excellent long-acting moisture retention.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides fucoidin-based long-acting moisturizing and antioxidant eye cream which comprises the following components in percentage by mass:
1.0-4.0% of fucoidin, 0.05-5% of sodium hyaluronate cross-linked polymer, 1.0-3.0% of oat beta-glucan, 0.1-2.0% of ascorbic acid, 0.01-0.05% of sodium alginate, 1.0-3.0% of tremella polysaccharide, 0.5-5% of polyglutamic acid, 0.5-3% of betaine, 0.1-0.5% of tea polyphenol, 0.3-1.5% of salvia miltiorrhiza root extract, 0.1-2.0% of peony root extract, 0.1-0.5% of camellia extract, 0.01-0.5% of angelica root extract, 0.05-0.1% of jojoba oil, 0.05-2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0.0.0% of glycerin, 3.0.0% of propylene glycol, 9400.5% of carbopol, 0.7% of triethanolamine, 0. 800.5% of polysorbate, 0.05-15% of water-15% of essence and the balance.
Preferably, the composition comprises the following components in percentage by mass: 1.0% of fucoidan, 0.5% of sodium hyaluronate cross-linked polymer, 1.0% of oat beta-glucan, 0.5% of ascorbic acid, 0.01% of sodium alginate, 1.0% of tremella polysaccharide, 0.5% of polyglutamic acid, 0.5% of betaine, 0.1% of tea polyphenol, 0.3% of salvia miltiorrhiza root extract, 0.5% of peony root extract, 0.1% of camellia extract, 0.05% of angelica root extract, 0.05% of jojoba oil, 2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0% of glycerol, 3.0% of propylene glycol, 9400.5% of carbomethanol, 0.7% of triethanolamine, polysorbate-800.5%, 0.15% of ethylparaben and 0.08% of essence, and the balance of water.
Preferably, the composition comprises the following components in percentage by mass: 2.0% of fucoidin, 1.0% of sodium hyaluronate cross-linked polymer, 1.0% of oat beta-glucan, 0.5% of ascorbic acid, 0.01% of sodium alginate, 1.0% of tremella polysaccharide, 0.5% of polyglutamic acid, 0.5% of betaine, 0.1% of tea polyphenol, 0.3% of salvia miltiorrhiza root extract, 0.5% of peony root extract, 0.1% of camellia extract, 0.05% of angelica root extract, 0.05% of jojoba oil, 2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0% of glycerol, 3.0% of propylene glycol, 9400.5% of carbomer, 0.7% of triethanolamine, polysorbate-800.5%, 0.15% of ethylparaben and 0.07% of essence, and the balance of water.
Preferably, the composition comprises the following components in percentage by mass: 4.0% of fucoidan, 1.5% of sodium hyaluronate cross-linked polymer, 2.0% of oat beta-glucan, 0.5% of ascorbic acid, 0.01% of sodium alginate, 1.0% of tremella polysaccharide, 0.5% of polyglutamic acid, 0.5% of betaine, 0.1% of tea polyphenol, 0.3% of salvia miltiorrhiza root extract, 0.5% of peony root extract, 0.1% of camellia extract, 0.05% of angelica root extract, 0.05% of jojoba oil, 2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0% of glycerol, 3.0% of propylene glycol, 9400.5% of carbomethanol, 0.7% of triethanolamine, polysorbate-800.5%, 0.15% of ethylparaben and 0.08% of essence, and the balance of water.
Preferably, the mass content of L-fucose in the fucoidin is more than or equal to 20%.
Preferably, the preparation method of the fucoidan comprises the following steps:
mixing the kelp powder with an ethanol solution, and performing reflux extraction to obtain reflux kelp powder;
carrying out water leaching on the refluxed kelp powder to obtain a leaching solution;
sequentially carrying out calcium salt precipitation, ethanol fractional precipitation, dialysis and column chromatography separation and purification on the leaching solution to obtain the fucoidin;
the production place of the kelp powder is Fujian.
Preferably, the volume concentration of the ethanol solution is preferably 95%; the feed-liquid ratio of the kelp powder to the ethanol solution is 1 g: 8 mL; the temperature of reflux extraction is 85 ℃, and the time is 3-4 h.
Preferably, the water leaching conditions include: the material-liquid ratio is 1 g: 30mL, 70 ℃ and 4 h.
Preferably, the dialysis has a minimum molecular weight cut-off of 3000.
The invention also provides a preparation method of the fucoidin-based long-acting moisturizing and antioxidant eye cream, which comprises the following steps:
mixing jojoba oil, squalane, isooctyl stearate, isopropyl palmitate, liquid paraffin, white beeswax, glyceryl monostearate and ceramide, and performing first emulsification to obtain a first emulsification system;
mixing fucoidin, sodium hyaluronate cross-linked polymer, oat beta-glucan, ascorbic acid, sodium alginate, tremella polysaccharide, polyglutamic acid, betaine, tea polyphenol, salvia miltiorrhiza root extract, peony root extract, camellia extract, angelica root extract, glycerin, propylene glycol, carbomer 940, triethanolamine, polysorbate-80, ethylparaben and water, and performing second emulsification to obtain a second emulsification system;
and mixing the first emulsifying system and the second emulsifying system, homogenizing and emulsifying, and adding essence to obtain the fucoidin-based long-acting moisturizing and antioxidant eye cream.
The invention provides fucoidin-based long-acting moisturizing and antioxidant eye cream which comprises the following components in percentage by mass: 1.0-4.0% of fucoidin, 0.05-5% of sodium hyaluronate cross-linked polymer, 1.0-3.0% of oat beta-glucan, 0.1-2.0% of ascorbic acid, 0.01-0.05% of sodium alginate, 1.0-3.0% of tremella polysaccharide, 0.5-5% of polyglutamic acid, 0.5-3% of betaine, 0.1-0.5% of tea polyphenol, 0.3-1.5% of salvia miltiorrhiza root extract, 0.1-2.0% of peony root extract, 0.1-0.5% of camellia extract, 0.01-0.5% of angelica root extract, 0.05-0.1% of jojoba oil, 0.05-2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0.0.0% of glycerin, 3.0.0% of propylene glycol, 9400.5% of carbopol, 0.7% of triethanolamine, 0. 800.5% of polysorbate, 0.05-15% of water-15% of essence and the balance. The eye cream takes fucoidin, sodium hyaluronate cross-linked polymer, sodium alginate, oat beta-glucan, polyglutamic acid, betaine and tremella polysaccharide as moisture retention components, wherein the combination of the fucoidin and the sodium hyaluronate cross-linked polymer can form a layer of water-locking barrier on the surface of skin, so that the moisture retention time is effectively prolonged, and the eye cream has excellent long-acting moisture retention; fucoidin, salvia miltiorrhiza root extract, peony root extract, angelica root extract, camellia extract, tea polyphenol and ascorbic acid are used as antioxidant ingredients, so that the eye cream has excellent antioxidant activity. The eye cream provided by the invention is free of alcohol, has small irritation, can reduce the problems of skin allergy and tissue inflammation, and is suitable for a wide range of people. In addition, the fucoidin has good antibacterial activity, can reduce the dosage of the preservative in the eye cream, and enables the eye cream to have antibacterial and anti-inflammatory effects.
Furthermore, the invention takes kelp powder of Fujian as raw material to extract fucoidin, thus further improving the long-acting moisture retention and oxidation resistance of the eye cream.
Drawings
FIG. 1 is a moisture retention curve of a 1% fucoidan solution in an environment with a humidity of 81% within 24 hours;
FIG. 2 is a moisture retention curve of a 1% fucoidan solution in an environment with a humidity of 43% within 24 hours;
FIG. 3 is a graph showing the result of measuring the scavenging ability of fucoidan against DPPH radicals at various concentrations.
Detailed Description
The invention provides fucoidin-based long-acting moisturizing and antioxidant eye cream which comprises the following components in percentage by mass:
1.0-4.0% of fucoidin, 0.05-5% of sodium hyaluronate cross-linked polymer, 1.0-3.0% of oat beta-glucan, 0.1-2.0% of ascorbic acid, 0.01-0.05% of sodium alginate, 1.0-3.0% of tremella polysaccharide, 0.5-5% of polyglutamic acid, 0.5-3% of betaine, 0.1-0.5% of tea polyphenol, 0.3-1.5% of salvia miltiorrhiza root extract, 0.1-2.0% of peony root extract, 0.1-0.5% of camellia extract, 0.01-0.5% of angelica root extract, 0.05-0.1% of jojoba oil, 0.05-2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0.0.0% of glycerin, 3.0.0% of propylene glycol, 9400.5% of carbopol, 0.7% of triethanolamine, 0. 800.5% of polysorbate, 0.05-15% of water-15% of essence and the balance.
In the present invention, all the raw materials of the present invention are preferably commercially available products unless otherwise specified.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 1.0-4.0% of fucoidin by mass, preferably 2.0-4.0%, more preferably 2.0-3.0%, and even more preferably 2.0%. In the invention, the mass content of L-fucose in the fucoidin is preferably more than or equal to 20%. In the present invention, the fucoidan is preferably a commercially available product or a self-made laboratory product well known to those skilled in the art. In the present invention, the preparation method of fucoidan preferably comprises the following steps:
mixing the kelp powder with an ethanol solution, and performing reflux extraction to obtain reflux kelp powder;
carrying out water leaching on the refluxed kelp powder to obtain a leaching solution;
and sequentially carrying out calcium salt precipitation, ethanol fractional precipitation, dialysis and column chromatography separation and purification on the leaching solution to obtain the fucoidin.
The invention mixes kelp powder with ethanol solution, and carries out reflux extraction to obtain the reflux kelp powder.
In the present invention, the production place of the kelp powder is preferably Fujian. In the present invention, the particle diameter of the kelp powder is preferably 0.15mm to 0.85 mm. In the present invention, the kelp powder is preferably prepared by washing, drying and pulverizing dried kelp in this order. In the present invention, the washing reagent preferably includes clean water and distilled water; the number of times of washing is not particularly limited, and the impurities on the surface of the dried kelp can be removed completely. In the present invention, the drying mode is preferably natural airing. The parameters for the pulverization are not particularly limited in the present invention, as long as the kelp powder having a particle size of 0.15mm to 0.85mm can be obtained.
In the present invention, the volume concentration of the ethanol solution is preferably 95%; the feed-liquid ratio of the kelp powder to the ethanol solution is preferably 1 g: 8 mL.
In the invention, the temperature of the reflux extraction is preferably 85 ℃, and the time is preferably 3-4 h.
After the reflux extraction, the invention preferably further comprises the steps of carrying out solid-liquid separation on a reflux extraction system obtained by the reflux extraction, and drying the obtained solid to obtain the reflux kelp powder. In the present invention, the solid-liquid separation is preferably performed by filtration. In the present invention, the temperature of the drying is preferably 45 ℃, and the time of the drying is not particularly limited as long as the drying can be performed to a constant weight.
In the present invention, the reflux extraction can remove most of pigments, lipids, mannitol and inorganic salts.
After the reflux kelp powder is obtained, the reflux kelp powder is subjected to water leaching to obtain a leaching solution.
In the present invention, the water leaching conditions include: the feed-liquid ratio is preferably 1 g: 30mL, the temperature is preferably 70 ℃, and the time is preferably 4 h; the water for water leaching is preferably distilled water.
After the water leaching, the invention preferably further comprises the steps of standing and cooling a water leaching system obtained by the water leaching, and then carrying out solid-liquid separation to obtain the leaching liquor.
After obtaining the leaching liquor, sequentially carrying out calcium salt precipitation, ethanol fractional precipitation, dialysis and column chromatography separation and purification on the leaching liquor to obtain the fucoidin.
In the present invention, the conditions for the calcium salt-based precipitation include: the calcium salt is preferably calcium chloride; the mass concentration of the calcium salt solution is preferably 10 percent; the volume ratio of the calcium salt solution to the leaching liquor is preferably 1: 4; the time for the calcium salt to precipitate is preferably 30 min. After the calcium salt is precipitated, the invention preferably further comprises the step of carrying out solid-liquid separation on a calcium salt precipitation system obtained by the calcium salt precipitation to obtain a precipitate for subsequent operation.
In the present invention, the conditions for the ethanol fractional precipitation include: carrying out first alcohol precipitation on the precipitate obtained by calcium salt precipitation in an ethanol water solution with the volume concentration of 70%, and then carrying out first centrifugation to obtain a first precipitate; carrying out second alcohol precipitation on the first precipitate in an ethanol water solution with the volume concentration of 30%, and then carrying out second centrifugation to obtain a second supernatant; carrying out third alcohol precipitation on the second supernatant in an ethanol water solution with the volume concentration of 70%, and then carrying out third centrifugation to obtain a third precipitate; and mixing the third precipitate with water to obtain an ethanol fractional precipitation solution. In the invention, the rotation speed of the first centrifugation, the second centrifugation and the third centrifugation is preferably 10000r/min, and the time is preferably 5 min.
In the present invention, the minimum cut-off molecular weight of the dialysis is preferably 3000; the dialysis temperature is preferably 4 ℃ and the dialysis time is preferably 72 hours. In the present invention, the dialysis preferably comprises the steps of: pretreating the dialysis bag; and filling the solution obtained by ethanol fractional precipitation into a pretreatment dialysis bag for dialysis. In the present invention, the pretreatment preferably includes: placing the dialysis bag into a beaker filled with distilled water, and boiling for 10 min.
In the invention, the conditions for column chromatography separation and purification comprise: the filler is preferably DEAE-52 cellulose column filler; the chromatographic column is preferably a 30X 600mm atmospheric pressure column; the sampling flow rate is preferably 2 mL/min; the leaching agent is preferably water; the elution reagent is preferably 1.0mol/L sodium chloride aqueous solution; the volume of the elution reagent is preferably 1-10 column volumes.
After the column chromatography separation and purification, the invention preferably further comprises concentrating the obtained eluent, and dialyzing and freeze-drying the obtained concentrated solution in sequence to obtain the fucoidin. In the invention, the cut-off molecular weight of the dialysis is preferably 8-14 kDa; the present invention does not specifically limit the parameters of the lyophilization, as long as the lyophilization is possible.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.05-5% by mass of sodium hyaluronate cross-linked polymer, preferably 0.1-4.0%, more preferably 0.5-2.0%, and more preferably 1.0-1.5%. The sodium hyaluronate cross-linked polymer belongs to a skin conditioner, is an acidic mucopolysaccharide, naturally exists in corneal skin, can absorb 1000 times of water by weight of the corneal skin, so as to achieve the purposes of keeping skin water, preventing water from losing through epidermis, and repairing a barrier when the skin is damaged, so that the skin does not feel dry and glossy after being used, can improve skin nutrition metabolism, enables the skin to be soft and smooth, removes wrinkles, increases elasticity and prevents aging, and is a good transdermal absorption promoter while keeping moisture.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 1.0-3.0% of oat beta-glucan in percentage by mass, preferably 1.5-2.5%, and more preferably 2.0%. In the present invention, the oat β -glucan is preferably extracted from oat seeds of the family Poaceae. In the present invention, oat beta-glucan is present in the cell wall of oat bran and is a polysaccharide composed of cellotriose and cellotetraose-linked sugar monomers. Oat beta glucan extracted from oat seeds of Gramineae contains water-soluble fraction of refined oat glucan, and is free of lipids, fibers and proteins; can keep the moisture of the skin; can promote macrophage to release interleukin-1, accelerate collagen synthesis, resist aging, reduce skin wrinkle, improve skin elasticity, improve skin texture, promote skin absorption, promote wound healing, and repair damaged skin.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.1-2.0% by mass of ascorbic acid, preferably 0.5-1.5%, and more preferably 1.0%.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.01-0.05% of sodium alginate by mass, preferably 0.02-0.04%, and more preferably 0.03%.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 1.0-3.0% of tremella polysaccharide by mass, preferably 1.5-2.5%, and further preferably 2.0%, wherein the tremella polysaccharide is a plant-derived hyaluronic acid substance, the molecular weight of the tremella polysaccharide reaches 100-130 thousands, and the plant-derived high-efficiency humectant is used as a humectant; and can improve the stability of the cosmetic and reduce the interfacial tension.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.5-5% of polyglutamic acid by mass, preferably 1.0-4.0%, and more preferably 2.0-3.0%. In the invention, the polyglutamic acid can more efficiently moisturize and moisturize, and the problem of dry skin is solved; meanwhile, the extensibility of the skin can be improved, so that the skin is moist and soft; moreover, the polyglutamic acid has good promotion effect on the activity of fibroblasts and the like, and has the function of activating skin. In addition, the polyglutamic acid has the effects of whitening and brightening the skin to a certain extent.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.5-3% of betaine in percentage by mass, preferably 1.0-2.5%, and more preferably 1.5-2.0%. In the present invention, betaine has a moisturizing effect like glycerol, but unlike the fixed water molecules of glycerol, betaine is one that allows water molecules to be completely absorbed and utilized by whole living cells. When one water molecule occupies the middle of the betaine zwitterion, the self water molecule can be easily released to the surrounding liquid.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.1-0.5% by mass of tea polyphenol, preferably 0.2-0.4%, and more preferably 0.3%. In the present invention, tea polyphenol is a complex of flavanol compounds and has a strong antioxidant effect, so that it can inhibit peroxidation of substances, and has an anti-aging effect, and it can also scavenge free radicals, and can effectively prevent peroxidation of low-density lipoprotein, and protect endothelial cells.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.3-1.5% of salvia miltiorrhiza root extract by mass, and preferably 0.5-1.0%. In the present invention, the salvia miltiorrhiza root extract has fat-soluble and water-soluble components, and cryptotanshinone in the fat-soluble components has antibacterial activity; the water soluble components including danshensu and protocatechualdehyde have antioxidant, antibacterial and antiinflammatory effects.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.1-2.0% of a peony root extract by mass, and preferably 0.5-1.5%. In the invention, the active ingredient of the paeoniflorin extract is paeoniflorin, which has the inhibiting effect on certain pathogenic bacteria and fungi; the peony root extract has the functions of activating skin and resisting aging, and can be used for anti-aging cosmetics.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.1-0.5% of camellia extract by mass, preferably 0.2-0.4%, and more preferably 0.3%. In the invention, the main antioxidant components in the camellia extract comprise quercetin, isoquercitrin, quercetin and kaempferol. These components can achieve antioxidant effect by scavenging reactive oxygen species ROS in human keratinocytes and enhancing antioxidant enzyme activity. The human body patch test shows that the camellia extract is safe, has no thorns and micro-irritations, and has better DPPH and ABTS free radical scavenging capacity.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.01-0.5% of angelica root extract by mass, and preferably 0.05-0.5%. In the invention, the angelica root extract has good promotion effect on collagen proliferation, so that the metabolism of the dermal layer of the skin can be enhanced, and the angelica root extract can be used in skin-activating anti-wrinkle cosmetics; has oxidation resistance; has effect in promoting hyaluronic acid generation, and can be used as humectant; the composition has no acne treating effect.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.05-0.1% of jojoba oil by mass, preferably 0.06-0.09%, and further preferably 0.07-0.08%.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.05-2.0% of squalane by mass, and preferably 1.0-2.0%.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 2.2% of isooctyl stearate in percentage by mass.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises isopropyl palmitate with the mass percentage of 2.5%.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises liquid paraffin with the mass percentage of 4.2%.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 2.3% of white beeswax in percentage by mass.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 1.5% of glyceryl monostearate in percentage by mass.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.5% by mass of ceramide.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 4.0% of glycerin by mass.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 3.0% of propylene glycol by mass.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.5% of carbomer 940 by mass.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.7% of triethanolamine by mass.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.5% of polysorbate-80 by mass.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.05-0.15% of ethylparaben by mass, preferably 0.06-0.14%, further preferably 0.07-0.13%, and more preferably 0.08-0.12%.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises 0.06-0.08% of essence by mass, and preferably 0.07%. In the present invention, the essence preferably includes one or more of rose essence, lemon essence, and bay essence.
The fucoidin-based long-acting moisturizing and antioxidant eye cream provided by the invention comprises the balance of water, wherein the water is preferably deionized water or purified water.
The invention also provides a preparation method of the fucoidin-based long-acting moisturizing and antioxidant eye cream, which comprises the following steps:
mixing jojoba oil, squalane, isooctyl stearate, isopropyl palmitate, liquid paraffin, white beeswax, glyceryl monostearate and ceramide, and performing first emulsification to obtain a first emulsification system;
mixing fucoidin, sodium hyaluronate cross-linked polymer, oat beta-glucan, ascorbic acid, sodium alginate, tremella polysaccharide, polyglutamic acid, betaine, tea polyphenol, salvia miltiorrhiza root extract, peony root extract, camellia extract, angelica root extract, glycerin, propylene glycol, carbomer 940, triethanolamine, polysorbate-80, ethylparaben and water, and performing second emulsification to obtain a second emulsification system;
and mixing the first emulsifying system and the second emulsifying system, homogenizing and emulsifying, and adding essence to obtain the fucoidin-based long-acting moisturizing and antioxidant eye cream.
The preparation method comprises the steps of mixing jojoba oil, squalane, isooctyl stearate, isopropyl palmitate, liquid paraffin, white beeswax, glyceryl monostearate and ceramide, and carrying out first emulsification to obtain a first emulsification system.
In the invention, the rotation speed of the first emulsification is preferably 80-100 r/min, the temperature is preferably 70-75 ℃, and the time is preferably 5-10 min; after the first emulsification, the invention preferably also comprises sterilizing the first emulsified material liquid obtained by the first emulsification; the time for the sterilization is preferably 25 min.
The preparation method comprises the steps of mixing fucoidin, sodium hyaluronate cross-linked polymer, oat beta-glucan, ascorbic acid, sodium alginate, tremella polysaccharide, polyglutamic acid, betaine, tea polyphenol, salvia miltiorrhiza root extract, peony root extract, camellia extract, angelica root extract, glycerin, propylene glycol, carbomer 940, triethanolamine, polysorbate-80, ethylparaben and water, and carrying out second emulsification to obtain a second emulsification system.
In the invention, the rotation speed of the second emulsification is preferably 500-1000 r/min, the temperature is preferably 75-85 ℃, and the time is preferably 5-10 min; after the second emulsification, the invention preferably also comprises sterilizing the second emulsified feed liquid obtained by the second emulsification; the time for the sterilization is preferably 25 min.
After the first emulsifying system and the second emulsifying system are obtained, the first emulsifying system and the second emulsifying system are mixed, homogenized and emulsified, and then essence is added to obtain the fucoidin-based long-acting moisturizing and antioxidant eye cream.
In the invention, the rotation speed of the homogenizing emulsification is preferably 80-100 r/min, the temperature is preferably 75-85 ℃, and the time is preferably 5-15 min; after homogenizing and emulsifying, the invention cools the homogenized and emulsified material liquid obtained by homogenizing and emulsifying to 55 ℃, and then adds essence.
After the essence is added, the invention preferably further comprises the steps of continuously stirring and sterilizing; the continuous stirring time is preferably 5-15 min; the time for the sterilization is preferably 25 min.
The fucoidan-based moisturizing and antioxidant eye cream and the preparation method thereof according to the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
Cleaning dry kelp (Fujian, the production place) with clear water and distilled water respectively, airing, and crushing for later use to obtain kelp powder with the particle size of 0.425 mm-0.600 mm; mixing kelp powder and 95% ethanol solution according to a material-liquid ratio of 1 g: 8mL of the kelp powder is mixed, the mixture is refluxed for 4 hours at 85 ℃, then is filtered, and filter residue is placed in a drying box at 45 ℃ and is dried to obtain the reflux kelp powder.
Weighing 60g of reflux kelp powder and distilled water according to a material-liquid ratio of 1 g: mixing 30mL of the above components, extracting at 70 ℃ for 4h, standing for 30min, cooling, and filtering with 200-mesh filter cloth to obtain a leaching solution.
Adding calcium salt precipitate into the leaching solution, adding 1/4 v% CaCl2 solution with mass concentration of 10%, precipitating for 30min, and pouring out the supernatant to obtain a flocculent mixture solution with a small amount of supernatant; the solution of the flocculent mixture with a small amount of supernatant was filtered through a filter cloth to obtain a precipitate.
Ethanol fractional precipitation: carrying out first alcohol precipitation on a precipitate obtained by calcium salt precipitation in an ethanol water solution with the volume concentration of 70%, then centrifuging for 5min at 10000r/min, and taking out the first precipitate; carrying out second alcohol precipitation on the first precipitate in an ethanol water solution with the volume concentration of 30%, and then centrifuging at 10000r/min for 5min to obtain a second supernatant; carrying out third alcohol precipitation on the second supernatant in an ethanol solution with the volume concentration of 70%, and then centrifuging for 5min at 10000r/min to obtain a third precipitate; and adding distilled water into the third precipitate to 20mL, and dissolving on a magnetic stirrer to obtain an ethanol fractional precipitation solution.
And (3) dialysis: cutting dialysis bag with lowest cut-off molecular weight of 3000 into proper length, placing dialysis bag into beaker filled with distilled water, boiling for 10min, cooling beaker, taking out dialysis bag; filling the ethanol fractional precipitation solution into dialysis bag, sealing both ends with sealing clamp, checking the tightness of the dialysis bag, and dialyzing in distilled water at 4 deg.C for 72 hr to obtain crude fucoidan.
Detection of crude fucoidan
(1) Determination of moisture
The results of measuring the moisture content by the direct drying method according to the national standard GB 5009.3-2016 moisture measurement in food are shown in Table 1.
(2) Determination of ash content
The ash content was measured according to the national standard GB 5009.4-2016 "measurement of ash in food", and the results are shown in Table 1.
(3) Determination of proteins
The results of protein content determination using the Folin phenol method are shown in Table 1.
(4) Determination of L-fucose
The L-fucose content was determined by the modified Dische method, and the results are shown in Table 1.
(5) Determination of the Total sugar content
The total sugar content was measured by the phenol-sulfuric acid method, and the results are shown in Table 1.
TABLE 1 measurement of the composition of crude fucoidan
Column chromatography separation and purification of fucoidin crude product
(1) DEAE-52 cellulose column packing pretreatment
Weighing 100g of DEAE-52 cellulose column filler, soaking overnight with excessive deionized water, removing small particles suspended on the surface, suction-filtering with a Buchner funnel, adding deionized water for washing for 3 times, soaking for 0.5h with 0.5mol/L NaOH, adding deionized water for repeatedly washing to neutrality, soaking for 0.5h with 0.5mol/L HCl solution, adding deionized water for repeatedly washing to neutrality, soaking the cellulose column filler subjected to acid-base treatment in 0.5In mol/LNaCl overnight to complete the conversion of the filler to Cl-Form, then washed with copious amounts of deionized water. And finally, storing the filler in deionized water for subsequent column filling.
(2) Packing, column packing and balancing
The normal pressure column with the specification of 30 x 600mm is adopted, the chromatographic column is cleaned and dried, and the pretreated filler is subjected to degassing treatment. Filling a small amount of cotton along with deionized water into the bottom of the chromatographic column, opening the valve of the column, slowly adding deionized water along the edge of the column, and compacting the cotton. Closing the valve, firstly adding 1/3 column volumes of deionized water, then draining by virtue of a glass rod, slowly adding the pretreated filler, reducing the generation of bubbles during the filler adding process, adding the mixture until the liquid level is flush with the column port surface, opening the valve to enable the deionized water to flow out, continuing adding the filler solution when the liquid level is reduced to 2/3 column volumes, and repeating the steps until the filler solution is completely added. The packing in the column is agitated from time to time during the process to prevent stratification. And after the filler is settled until the volume of the filler is not changed, obviously layering the filler and the upper layer of deionized water, opening a peristaltic pump, and balancing for 48 hours at the flow rate of 2.0mL/min to compact the chromatographic column.
(3) Sample loading
Preparing 200mg/mL fucoidin crude solution by using deionized water, removing excessive impurities by using a 0.45-micrometer microporous membrane after the fucoidin crude solution is fully dissolved, and adding the fucoidin crude solution along the inner wall of the chromatographic column at the flow rate of 0.5mL/min by using an injector. After the sample loading is finished, leaching with deionized water with the volume being 4-5 times that of the sample, and eluting with a NaCl solution with a certain volume concentration of 2.0mol/L to obtain an eluent; and concentrating the eluent, dialyzing the obtained concentrated solution for 3 days by using a dialysis bag with the molecular weight cutoff of 8-14 kDa, and freeze-drying to obtain the fucoidin.
(1) Determination of Total sugar
The total sugar content was measured by the phenol-sulfuric acid method, and the results are shown in Table 2.
(2) L-fucose assay
The content of L-fucose was measured by the Dische colorimetry, and the results are shown in Table 2.
(3) Determination of sulfate radical content
The content of sulfate groups was measured by the barium sulfate-gelatin method, and the results are shown in Table 2.
TABLE 2 component detection results of pure fucoidan
(4) Moisture retention testing of fucoidan
Preparing fucoidin into a fucoidin solution with the mass fraction of 1% (weighing 0.5g of fucoidin, dissolving in 49.5g of deionized water), respectively weighing three parts of the fucoidin solution in weighing bottles, placing the weighing bottles in driers with the humidity of 81% (saturated ammonium sulfate solution is contained at the bottom of a drying dish) and the humidity of 43% (saturated potassium carbonate solution is contained at the bottom of the drying dish) and the temperature of 20 ℃, and respectively measuring the mass of a sample at 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours and 24 hours. Three experiments were performed in parallel and the average was taken. The water content before standing was recorded as H0And the water content after standing is recorded as HnThe calculation formula of the moisture retention rate is as follows:
(H) moisture retention ratio%n÷H0)×100％
The moisture retention rate graph of fucoidan at a moisture content of 81% within 24 hours is shown in fig. 1.
The moisture retention rate of fucoidan at a moisture content of 43% within 24 hours is shown in fig. 2.
As can be seen from FIGS. 1-2: the moisture-keeping capacity of the fucoidin is still more than 99.5% after 24 hours under higher and lower humidity, which indicates that the fucoidin has long-acting moisture-keeping capacity.
(5) Oxidation resistance test of fucoidan
0.1mmol/L of DPPH ethanol solution is prepared, 1mL of 0.1mmol/L of DPPH ethanol solution is added to 1mL of 0, 3, 5, 7, 9, 11mg/mL fucoidan solution, the mixture is placed in a water bath at 37 ℃ for reaction for 30min, and the absorbance of the solution is measured at a wavelength of 517 nm. Keeping dark in the whole reaction process, and measuring the absorbance value A at 517nm1Absorbance alcohol is used to replace DPPH alcohol solution to measure absorbance value A at 517nm2To do so byAbsorbance alcohol replacing polysaccharide solution for determining absorbance value A0。
Calculating the clearance rate: 1- (A)1-A2)/A0×100％
The clearance of DPPH free radicals by fucoidan with different concentrations is shown in FIG. 3.
As can be seen from fig. 3: when the concentration of the fucoidin solution is 11g/L, the clearance rate of the fucoidin solution is maximum and reaches 90.43%, which indicates that the fucoidin has strong oxidation resistance.
Examples 2 to 5
The formulations of the fucoidan-based long-lasting moisturizing and antioxidant eye creams of examples 2 to 5 are shown in table 3.
TABLE 3 examples 2-5 fucoidan-based long-lasting moisturizing, antioxidant eye cream formulations
The fucoidin in the embodiments 2-4 is obtained by extracting in the embodiment 1; fucoidan in example 5 was purchased from Qingdao Huiyuan biotech development Co.
The preparation method of the fucoidin-based long-acting moisturizing and antioxidant eye cream comprises the following steps:
(1) mixing jojoba oil, squalane, isooctyl stearate, isopropyl palmitate, liquid paraffin, white beeswax, glyceryl monostearate and ceramide, adding into a first emulsifying pot, mixing, heating to 70-75 ℃, stirring to form a homogeneous phase, and sterilizing for 25min by using a sterilizing pot.
(2) Dissolving fucoidin, sodium hyaluronate cross-linked polymer, oat beta-glucan, ascorbic acid, sodium alginate, tremella polysaccharide, polyglutamic acid, betaine, tea polyphenol, salvia miltiorrhiza root extract, peony root extract, camellia extract, angelica root extract, glycerin, propylene glycol, carbomer 940, triethanolamine, polysorbate-80 and ethylparaben in deionized water, adding into a second emulsifying pot, heating to 75-85 ℃, stirring to be homogeneous, and sterilizing for 25min by using a sterilizing pot.
(3) And (3) mixing the materials obtained in the steps (1) and (2), homogenizing and emulsifying, homogenizing at 75-85 ℃ for 15min, cooling to 45 ℃, adding essence, continuously stirring for 15min, cooling to room temperature, and sterilizing to obtain the fucoidin-based long-acting moisturizing and antioxidant eye cream.
The eye creams obtained in examples 2 to 5 were tested for moisture retention at a temperature of 20 deg.c and a humidity of 43% and 81% for 24 hours according to the moisture retention test method of fucoidan in example 1, and the results are shown in table 4.
TABLE 4 results of moisturizing effect of eye creams obtained in examples 2 to 5
Example 6 method of use of eye cream
After cleaning the eye skin, a proper amount of eye cream is uniformly smeared on the skin around the eyes and is gently massaged until the eye cream is completely absorbed.
Example 7 use population testing
The test experiment is carried out on 200 persons, the age is 15-50 years old, after the eye mask is continuously used for a period of time, more than 96% of the persons react with the skin around the eyes to quickly replenish water, the skin around the eyes is strengthened, wrinkles are quickly faded, the black eye circles of more than 97% of the persons are obviously improved, more than 98% of the persons react with the skin around the eyes to be tightened, and under-eye bags are reduced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The fucoidin-based long-acting moisturizing and antioxidant eye cream is characterized by comprising the following components in percentage by mass:
1.0-4.0% of fucoidin, 0.05-5% of sodium hyaluronate cross-linked polymer, 1.0-3.0% of oat beta-glucan, 0.1-2.0% of ascorbic acid, 0.01-0.05% of sodium alginate, 1.0-3.0% of tremella polysaccharide, 0.5-5% of polyglutamic acid, 0.5-3% of betaine, 0.1-0.5% of tea polyphenol, 0.3-1.5% of salvia miltiorrhiza root extract, 0.1-2.0% of peony root extract, 0.1-0.5% of camellia extract, 0.01-0.5% of angelica root extract, 0.05-0.1% of jojoba oil, 0.05-2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0.0.0% of glycerin, 3.0.0% of propylene glycol, 9400.5% of carbopol, 0.7% of triethanolamine, 0. 800.5% of polysorbate, 0.05-15% of water-15% of essence and the balance.
2. The fucoidin-based long-acting moisturizing and antioxidant eye cream as claimed in claim 1, which is characterized by comprising the following components in percentage by mass: 1.0% of fucoidan, 0.5% of sodium hyaluronate cross-linked polymer, 1.0% of oat beta-glucan, 0.5% of ascorbic acid, 0.01% of sodium alginate, 1.0% of tremella polysaccharide, 0.5% of polyglutamic acid, 0.5% of betaine, 0.1% of tea polyphenol, 0.3% of salvia miltiorrhiza root extract, 0.5% of peony root extract, 0.1% of camellia extract, 0.05% of angelica root extract, 0.05% of jojoba oil, 2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0% of glycerol, 3.0% of propylene glycol, 9400.5% of carbomethanol, 0.7% of triethanolamine, polysorbate-800.5%, 0.15% of ethylparaben and 0.08% of essence, and the balance of water.
3. The fucoidin-based long-acting moisturizing and antioxidant eye cream as claimed in claim 1, which is characterized by comprising the following components in percentage by mass: 2.0% of fucoidin, 1.0% of sodium hyaluronate cross-linked polymer, 1.0% of oat beta-glucan, 0.5% of ascorbic acid, 0.01% of sodium alginate, 1.0% of tremella polysaccharide, 0.5% of polyglutamic acid, 0.5% of betaine, 0.1% of tea polyphenol, 0.3% of salvia miltiorrhiza root extract, 0.5% of peony root extract, 0.1% of camellia extract, 0.05% of angelica root extract, 0.05% of jojoba oil, 2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0% of glycerol, 3.0% of propylene glycol, 9400.5% of carbomer, 0.7% of triethanolamine, polysorbate-800.5%, 0.15% of ethylparaben and 0.07% of essence, and the balance of water.
4. The fucoidin-based long-acting moisturizing and antioxidant eye cream as claimed in claim 1, which is characterized by comprising the following components in percentage by mass: 4.0% of fucoidan, 1.5% of sodium hyaluronate cross-linked polymer, 2.0% of oat beta-glucan, 0.5% of ascorbic acid, 0.01% of sodium alginate, 1.0% of tremella polysaccharide, 0.5% of polyglutamic acid, 0.5% of betaine, 0.1% of tea polyphenol, 0.3% of salvia miltiorrhiza root extract, 0.5% of peony root extract, 0.1% of camellia extract, 0.05% of angelica root extract, 0.05% of jojoba oil, 2.0% of squalane, 2.2% of isooctyl stearate, 2.5% of isopropyl palmitate, 4.2% of liquid paraffin, 2.3% of white beeswax, 1.5% of glyceryl monostearate, 0.5% of ceramide, 4.0% of glycerol, 3.0% of propylene glycol, 9400.5% of carbomethanol, 0.7% of triethanolamine, polysorbate-800.5%, 0.15% of ethylparaben and 0.08% of essence, and the balance of water.
5. The fucoidin-based long-acting moisturizing and antioxidant eye cream as claimed in any one of claims 1 to 4, wherein the L-fucose content in the fucoidin is not less than 20% by mass.
6. The fucoidan-based long-acting moisturizing and antioxidant eye cream of claim 5, wherein the fucoidan is prepared by a method comprising the steps of:
mixing the kelp powder with an ethanol solution, and performing reflux extraction to obtain reflux kelp powder;
carrying out water leaching on the refluxed kelp powder to obtain a leaching solution;
sequentially carrying out calcium salt precipitation, ethanol fractional precipitation, dialysis and column chromatography separation and purification on the leaching solution to obtain the fucoidin;
the production place of the kelp powder is Fujian.
7. The fucoidan-based long-lasting moisturizing and antioxidant eye cream of claim 6, wherein the ethanol solution has a volume concentration of preferably 95%; the feed-liquid ratio of the kelp powder to the ethanol solution is 1 g: 8 mL; the temperature of reflux extraction is 85 ℃, and the time is 3-4 h.
8. The fucoidan-based long-lasting moisturizing and antioxidant eye cream of claim 6, wherein the water leaching conditions comprise: the material-liquid ratio is 1 g: 30mL, 70 ℃ and 4 h.
9. The fucoidan-based long-acting moisturizing and antioxidant eye cream of claim 6, wherein the dialysis has a minimum molecular weight cutoff of 3000.
10. The method for preparing fucoidan-based long-acting moisturizing and antioxidant eye cream according to any one of claims 1 to 9, comprising the steps of:
mixing jojoba oil, squalane, isooctyl stearate, isopropyl palmitate, liquid paraffin, white beeswax, glyceryl monostearate and ceramide, and performing first emulsification to obtain a first emulsification system;
mixing fucoidin, sodium hyaluronate cross-linked polymer, oat beta-glucan, ascorbic acid, sodium alginate, tremella polysaccharide, polyglutamic acid, betaine, tea polyphenol, salvia miltiorrhiza root extract, peony root extract, camellia extract, angelica root extract, glycerin, propylene glycol, carbomer 940, triethanolamine, polysorbate-80, ethylparaben and water, and performing second emulsification to obtain a second emulsification system;
and mixing the first emulsifying system and the second emulsifying system, homogenizing and emulsifying, and adding essence to obtain the fucoidin-based long-acting moisturizing and antioxidant eye cream.
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| CN115068371A (en) * | 2022-05-26 | 2022-09-20 | 广州市盛美化妆品有限公司 | Moisturizing cream with repairing effect and preparation method thereof |
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| CN114748385A (en) * | 2022-04-08 | 2022-07-15 | 广州优理氏生物科技有限公司 | Composition and eye cream with effects of resisting wrinkles, removing dark eye circles and improving eye bags |
| CN114748385B (en) * | 2022-04-08 | 2022-12-09 | 广州优理氏生物科技有限公司 | Composition and eye cream with effects of resisting wrinkles, removing dark eye circles and improving eye bags |
| CN115068371A (en) * | 2022-05-26 | 2022-09-20 | 广州市盛美化妆品有限公司 | Moisturizing cream with repairing effect and preparation method thereof |
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