CN113332208A - Preparation method of corn germ extracting solution and anti-inflammatory repair emulsion - Google Patents
Preparation method of corn germ extracting solution and anti-inflammatory repair emulsion Download PDFInfo
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Abstract
A preparation method of corn germ extracting solution comprises the following steps: a) mashing corn germ, uniformly mixing the corn germ, ethanol, butanediol and water according to a proportion, and adding compound protease with the quality of the corn germ for enzymolysis to obtain an enzymolysis liquid; b) b, performing ultrasonic extraction on the enzymatic hydrolysate obtained in the step a, and performing suction filtration to obtain filtrate; c) adding sodium citrate and potassium chloride into the filtrate; d) and (3) taking a cathode electrode and an anode electrode which are both platinum electrodes, taking the filtrate obtained in the step b) as catholyte, taking the aqueous solution of sodium citrate and sodium citrate as anolyte, separating the cathode and the anode by using an anion exchange membrane, and electrifying and activating to obtain the corn germ extracting solution. The invention also provides an anti-inflammatory repair emulsion containing the millettia extract and the corn germ extract. According to the invention, through scientific compatibility of the components, the synergistic interaction among the components is realized, the long-acting anti-inflammatory repair effect can be achieved, and the anti-inflammatory repair liquid can keep fresh and cool, and is moist but not greasy.
Description
Technical Field
The invention belongs to the field of skin care products, and particularly relates to a preparation method of a corn germ extracting solution and an anti-inflammatory repair emulsion.
Background
The skin is the outermost layer structure of the human body, is the largest organ of the human body, is a sensor of a nervous system and an effector, can reflectively cause the change of the skin to external stimulation, and can be quickly lost along with the continuous fading of the physiological mechanism of the human body under the influence of adverse factors such as pollution, pressure, ultraviolet rays and the like, so that the skin is frequently damaged, the skin aging is accelerated, signs such as wrinkles, color spots, skin looseness, chin contour change and the like appear in advance, the skin is continuously deteriorated, even inflammation of different degrees occurs, and if the damaged skin is not repaired in time, more serious skin problems can be caused. And with the continuous degeneration of physiological functions, the collagen generating capacity is greatly reduced, the internal structure of the skin is collapsed, the skin becomes loose, and if free radicals cannot be removed, the damaged skin barrier cannot be effectively repaired, so that the self-renewal and repair capacity in the skin is reduced, and the skin aging speed is accelerated. In order to promote collagen hyperplasia and reduce wrinkle visibility, the collagen-containing skin cream can help repair skin matrixes and promote self repair and renewal of the skin matrixes aiming at skin structures, and is rich in anti-oxidation ingredients, so that the collagen-containing skin cream can help skin resist environmental pressure, slow down aging, and is full, compact and permanently moist. Therefore, repairing skin by external force such as skin care products to supplement nutrients required by skin is the best way to maintain skin health.
The corn germ has high nutritive value, and it contains 18-25% of protein, 75-90% of mineral matter and 80-88% of oil in corn. In the oil, the linoleic acid content is more than 60%, and the linoleic acid and the microorganism E have synergistic effect, and have multiple effects of diminishing inflammation, resisting oxidation, resisting aging and the like. Meanwhile, active protein and other components in the maize germ also have high utilization value.
The existing process for extracting the maize germ lacks an activity activation step, so that the utilization rate of the effective components of the maize germ is reduced.
Artocarpus heterophyllus is also called as the south African phoenix grass and called as the 'regenerated grass', grows in the remote ancient mysterious south African plateau and is the only woody plant capable of reviving in the world. The Artocarpus heterophyllus extract can assist skin in maintaining moisture and supplementing water, reduce ultraviolet light damage, rapidly adapt to skin and weather change, and repair damaged skin. The skin care products of the skin-friendly series products with the millettia speciosa component can repair damaged body cells, adjust the water-oil balance of the skin and generate a high-quality skin barrier.
Patent CN112386532A discloses a preparation method of a millettia extract and application thereof, but the preparation method of the patent mainly only extracts flavones in the millettia, and the extraction of each component of the millettia is not complete, which causes resource waste, cannot realize reasonable utilization of the millettia components, and has high cost.
Disclosure of Invention
Based on the defects and shortcomings in the prior art, the invention aims to provide the anti-inflammatory repair emulsion containing the millettia extract and the corn germ extract, which can realize good anti-inflammatory repair effect by fully extracting the millettia and activating the millettia extract and the corn germ extract and scientifically matching other components.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of corn germ extracting solution comprises the following steps:
a) mashing corn germs, uniformly mixing the corn germs, ethanol, butanediol and water according to the mass ratio of 8:1-4:0.5-1:20-30, and adding 0.5-3% of compound protease of the corn germs for enzymolysis to obtain an enzymolysis liquid;
b) b, performing ultrasonic extraction on the enzymatic hydrolysate obtained in the step a, and performing suction filtration to obtain filtrate;
c) adding 5-8% of sodium citrate and 1-3% of potassium chloride into the filtrate;
d) and (b) taking a cathode electrode and an anode electrode which are both platinum electrodes, taking the filtrate obtained in the step b) as catholyte, taking an aqueous solution of sodium citrate with the mass concentration of 5% -8% and potassium chloride with the mass concentration of 1% -3% as anolyte, separating the cathode and the anode by using an anion exchange membrane, and electrifying and activating to obtain the corn germ extracting solution.
Preferably, the compound protease is papain, trypsin, carboxypeptidase and neutral protease in a ratio of 1:1:3:2, the enzymolysis time is 40-80min, and the enzymolysis temperature is 34-39 ℃.
Preferably, the current density of the electrification activation is 1-20A/m2, and the temperature is 20-50 ℃.
Preferably, the ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-500W.
The invention also provides an anti-inflammatory repair emulsion containing the corn germ extracting solution, which comprises the following components in percentage by mass: 0.2% -2.6% of millettia extract, 0.8% -1.7% of corn germ extract, 0.15% -2.2% of magnesium ascorbyl phosphate, 0.1% -5% of hyaluronic acid, 0.1% -0.5% of succinic acid, 0.1% -0.8% of distearyl dimonium hectorite, 0.2% -0.9% of methylparaben, 2% -4% of glyceryl stearate PEG-75, 0.1% -2.3% of polysorbate-80, 0.1% -0.6% of stearyl alcohol, 0.1% -3% of butanediol, 3% -10% of glycerol and the balance of water;
the corn germ extracting solution is prepared by the preparation method.
Preferably, the preparation method of the extract of Artocarpus heterophyllus comprises the following steps:
1) putting the Artocarpus heterophyllus in a mortar, and mixing according to the mass ratio of Artocarpus heterophyllus to ethanol of 2.5-3.5: adding ethanol according to the proportion of 1, grinding and crushing to obtain Artocarpus millefolius powder A;
2) putting the Artocarpus mollis into a sealed inert gas atmosphere environment, carrying out treatment heat treatment at 130-200 ℃ for 8-13 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 1.5-2.8:1, grinding and crushing, and dropwise adding hyaluronic acid of which the mass is 12-17% of that of the millettia speciosa in the grinding process; obtaining Artocarpus heterophyllus powder B;
the tissues of the Artocarpus heterophyllus can be tenderized and softened by heat treatment in an inert gas atmosphere environment, so that the components of the Artocarpus heterophyllus can be fully extracted in the subsequent extraction process. During the grinding and extraction process, hyaluronic acid is added dropwise to promote the extraction of various components of Artocarpus heterophyllus. Meanwhile, the activity of the hyaluronic acid and the millettia speciosa can be crosslinked to a certain extent under the condition of slight heat in the grinding process, so that the repairing effect of the millettia speciosa is enhanced.
3) Mixing Artocarpus heterophyllus powder A, Artocarpus heterophyllus powder B, water and ethanol at a ratio of 10: 0.9-1.4: uniformly mixing the components in a ratio of 40-50:12-16, and performing ultrasonic extraction; respectively obtaining a first filtrate and a first filter residue after suction filtration;
4) placing the first filter residue after suction filtration in a sealed oxygen atmosphere environment, performing thermal oxidation treatment at 310-340 ℃ for 15-18 minutes, and then cooling to room temperature; uniformly mixing the millettia subjected to thermal oxidation treatment according to the mass ratio of 2.4-3.4:0.7-1.2:0.1-0.3:0.05-0.1 of the millettia, ethanol, ascorbic acid and EDTA, and grinding and crushing to obtain millettia powder C;
5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate in an amount which is 12-25% of the mass of the Artocarpus heterophyllus powder A in the step 3, uniformly mixing, performing secondary ultrasonic extraction, and performing suction filtration to obtain a second filtrate and a second filter residue respectively, wherein the second filtrate is Artocarpus heterophyllus extract.
A part of trace metal elements in the Artocarpus heterophyllus are still left in the first filter residue and are not extracted. In a closed oxygen atmosphere environment at the temperature of 300-360 ℃, trace metal elements in the oxygen atmosphere can be embodied in the form of oxides and retained; after cooling, grinding and extracting by ethanol, ascorbic acid and EDTA according to a proper proportion, and adding the mixture into the first filtrate again for secondary ultrasonic extraction to fully utilize each component in the Artocarpus heterophyllus.
Preferably, the filtrate in the step 3 is added with dipotassium glycyrrhizinate accounting for 2.1-4.3% of the mass of the extract of the millettia speciosa.
Preferably, the mortar is agate mortar.
Preferably, the paint consists of the following components in percentage by mass: 0.84% of millettia extract, 1.3% of corn germ extract, 0.76% of magnesium ascorbyl phosphate, 0.23% of hyaluronic acid, 0.34% of succinic acid, 0.66% of disteardimonium hectorite, 0.68% of methylparaben, 2.46% of glyceryl stearate PEG-75, 0.44% of polysorbate-80, 0.54% of stearyl alcohol, 1.48% of butanediol, 8% of glycerin, and the balance of water.
Preferably, the ethanol is absolute ethanol or 95% ethanol.
The invention has the beneficial effects that:
1. according to the preparation method of the corn germ extracting solution, the cathode is electrified and activated, so that the partially oxidized corn germ active substances in the extracting process can be reduced, and meanwhile, the partial corn culture active substances can be subjected to electrocatalytic hydrogenation and activation, so that the antioxidant effect of the corn germ extracting solution is improved.
2. The preparation method of the extract of the Artocarpus heterophyllus is used for fully extracting various components of the Artocarpus heterophyllus through the treatment processes of grinding, heat treatment and grinding, ultrasonic extraction, thermal oxidation treatment of filter residue, secondary ultrasonic extraction and the like, so that the components of the Artocarpus heterophyllus are fully and reasonably utilized.
3. The millettia extract used in the invention and the preparation method adopted by the millettia extract can mutually promote the absorption of the skin on the dipotassium glycyrrhizinate and the millettia components by adding the dipotassium glycyrrhizinate in the preparation process, thereby achieving the synergistic effect and enhancing the repairing and moisturizing effects.
4. The millettia extract used in the invention is matched with the millettia extracted by different extraction methods, and because the contents of all components of the millettia extracted by different extraction methods have certain difference, for example, the heat treatment can extract the components which can supplement hyaluronic acid, the thermal oxidation treatment can extract trace metal elements in residues, and the full absorption of skin to all the components can be improved by reasonable proportioning.
5. According to the invention, through scientific compatibility of the components, the synergistic interaction effect among the components is realized, the long-acting anti-inflammatory repair effect can be achieved, and the anti-inflammatory repair liquid can keep fresh, moist and not greasy.
Detailed Description
In order to more clearly illustrate the examples of the present invention, the following will describe embodiments of the present invention with reference thereto. It is to be understood that the following description is of only some embodiments of the invention and that other embodiments may be devised by those skilled in the art without the use of inventive faculty.
Example 1:
a preparation method of corn germ extracting solution comprises the following steps:
a) mashing corn germ, uniformly mixing the corn germ, ethanol, butanediol and water according to the mass ratio of 8:3.8:0.7:28, and adding compound protease accounting for 1.88% of the mass of the corn germ for enzymolysis to obtain an enzymolysis solution;
the compound protease is composed of papain, trypsin, carboxypeptidase and neutral protease according to the proportion of 1:1:3:2, the enzymolysis time is 45min, and the enzymolysis temperature is 37 ℃.
b) B, performing ultrasonic extraction on the enzymatic hydrolysate obtained in the step a, and performing suction filtration to obtain filtrate;
c) adding 5% of sodium citrate and 2% of potassium chloride into the filtrate;
d) and (3) taking a cathode electrode and an anode electrode which are both platinum electrodes, taking the filtrate obtained in the step b) as catholyte, taking an aqueous solution of sodium citrate with the mass concentration of 5% and potassium chloride with the mass concentration of 2% as anolyte, separating the cathode and the anode by using an anion exchange membrane, and electrifying and activating to obtain the corn germ extracting solution. The current density of the electrified activation is 1A/m2The temperature was 45 ℃.
The ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.
Example 2:
a preparation method of corn germ extracting solution comprises the following specific steps:
a) mashing corn germ, uniformly mixing the corn germ, ethanol, butanediol and water according to the mass ratio of 8:2:0.8:20, and adding 0.5% of compound protease of the corn germ for enzymolysis to obtain enzymolysis liquid;
the compound protease is composed of papain, trypsin, carboxypeptidase and neutral protease according to the proportion of 1:1:3:2, the enzymolysis time is 40min, and the enzymolysis temperature is 35 ℃.
b) B, performing ultrasonic extraction on the enzymatic hydrolysate obtained in the step a, and performing suction filtration to obtain filtrate;
c) adding 6% of sodium citrate and 3% of potassium chloride into the filtrate;
d) and (3) taking a cathode electrode and an anode electrode which are both platinum electrodes, taking the filtrate obtained in the step b) as catholyte, taking an aqueous solution of sodium citrate with the mass concentration of 6% and potassium chloride with the mass concentration of 3% as anolyte, separating the cathode and the anode by using an anion exchange membrane, and electrifying and activating to obtain the corn germ extracting solution. The current density of the electrified activation is 20A/m2The temperature was 35 ℃.
The ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.
Example 3:
a preparation method of corn germ extracting solution comprises the following steps:
a) mashing corn germ, uniformly mixing the corn germ, ethanol, butanediol and water according to the mass ratio of 8:2:0.8:20, and adding compound protease accounting for 1% of the mass of the corn germ for enzymolysis to obtain enzymolysis liquid;
the compound protease is composed of papain, trypsin, carboxypeptidase and neutral protease according to the proportion of 1:1:3:2, the enzymolysis time is 70min, and the enzymolysis temperature is 34 ℃.
b) B, performing ultrasonic extraction on the enzymatic hydrolysate obtained in the step a, and performing suction filtration to obtain filtrate;
c) adding 7% of sodium citrate and 1% of potassium chloride into the filtrate;
d) and (b) taking a cathode electrode and an anode electrode which are both platinum electrodes, taking the filtrate obtained in the step b) as catholyte, taking an aqueous solution of sodium citrate with the mass concentration of 7% and potassium chloride with the mass concentration of 1% as anolyte, separating the cathode and the anode by using an anion exchange membrane, and electrifying and activating to obtain the corn germ extracting solution. The current density of the electrified activation is 10A/m2The temperature was 20 ℃.
Example 4:
a preparation method of corn germ extracting solution comprises the following steps:
a) mashing corn germ, uniformly mixing the corn germ, ethanol, butanediol and water according to the mass ratio of 8:2:0.8:20, and adding compound protease accounting for 2.9% of the mass of the corn germ for enzymolysis to obtain enzymolysis liquid;
the compound protease is composed of papain, trypsin, carboxypeptidase and neutral protease according to the proportion of 1:1:3:2, the enzymolysis time is 50min, and the enzymolysis temperature is 39 ℃.
b) B, performing ultrasonic extraction on the enzymatic hydrolysate obtained in the step a, and performing suction filtration to obtain filtrate;
c) adding 8% of sodium citrate and 2.5% of potassium chloride into the filtrate;
d) and (b) taking a cathode electrode and an anode electrode which are both platinum electrodes, taking the filtrate obtained in the step b) as catholyte, taking an aqueous solution of sodium citrate with the mass concentration of 8% and potassium chloride with the mass concentration of 2.5% as anolyte, separating the cathode and the anode by using an anion exchange membrane, and electrifying and activating to obtain the corn germ extracting solution. The current density of the electrified activation is 15A/m2The temperature was 28 ℃.
The ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.
Example 5:
an anti-inflammatory repair emulsion containing corn germ extracting solution comprises the following components in percentage by mass: 1.8% of millettia extract, 0.86% of corn germ extract, 0.6% of magnesium ascorbyl phosphate, 2.3% of hyaluronic acid, 0.4% of succinic acid, 0.7% of disteardimonium hectorite, 0.7% of methylparaben, 2% of glyceryl stearate PEG-75, 0.64% of polysorbate-80, 0.5% of stearyl alcohol, 2.8% of butylene glycol, 10% of glycerin, the balance being water;
the corn germ extract was prepared by the method of example 1.
The preparation method of the millettia extract comprises the following steps:
1) putting the Artocarpus heterophyllus in an agate mortar, and mixing the Artocarpus heterophyllus and ethanol according to the mass ratio of 2.5: adding ethanol according to the proportion of 1, grinding and crushing to obtain Artocarpus millefolius powder A;
2) putting the Artocarpus mandshurica in a sealed inert gas atmosphere environment, carrying out treatment heat treatment at 134 ℃ for 13 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 2.7:1, grinding and crushing, and dropwise adding hyaluronic acid accounting for 15% of the mass of the millettia speciosa in the grinding process; obtaining Artocarpus heterophyllus powder B;
the tissues of the Artocarpus heterophyllus can be tenderized and softened by heat treatment in an inert gas atmosphere environment, so that the components of the Artocarpus heterophyllus can be fully extracted in the subsequent extraction process. During the grinding and extraction process, hyaluronic acid is added dropwise to promote the extraction of various components of Artocarpus heterophyllus. Meanwhile, the activity of the hyaluronic acid and the millettia speciosa can be crosslinked to a certain extent under the condition of slight heat in the grinding process, so that the moisturizing and repairing effects of the millettia speciosa are enhanced.
3) Mixing the Artocarpus heterophyllus powder A, Artocarpus heterophyllus powder B, water and ethanol at a ratio of 10:1.01:48:13, adding dipotassium glycyrrhizinate 4.0 wt% of Artocarpus heterophyllus extractive solution, and ultrasonic extracting; respectively obtaining a first filtrate and a first filter residue after suction filtration;
4) placing the first filter residue after suction filtration in a closed oxygen atmosphere environment, carrying out thermal oxidation treatment at 316 ℃ for 16 minutes, and then cooling to room temperature; uniformly mixing the millettia subjected to thermal oxidation treatment according to the mass ratio of the millettia to the ethanol to the ascorbic acid to the EDTA of 2.5:1:0.15:0.06, and grinding and crushing to obtain millettia powder C;
5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate by 13% of the mass of the Artocarpus heterophyllus powder A in the step 3, uniformly mixing, performing secondary ultrasonic extraction, and performing suction filtration to obtain a second filtrate and a second filter residue respectively, wherein the second filtrate is Artocarpus heterophyllus extract.
Part of trace metal elements still in the Artocarpus heterophyllus in the first filter residue can be reflected in the form of oxides and retained at 316 ℃ in a sealed oxygen atmosphere environment; cooling, grinding and extracting with proper proportion of ethanol, ascorbic acid and EDTA, adding into the first filtrate again, and performing secondary ultrasonic extraction to make full use of each component in Artocarpus heterophyllus.
The ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.
Example 6:
an anti-inflammatory repair emulsion containing corn germ extracting solution comprises the following components in percentage by mass: 0.46% of millettia extract, 1.6% of corn germ extract, 1.43% of magnesium ascorbyl phosphate, 4.8% of transparent acid, 0.1% of succinic acid, 0.5% of disteardimonium hectorite, 0.9% of methylparaben, 2.8% of glyceryl stearate PEG-75, 1.4% of polysorbate-80, 0.2% of stearyl alcohol, 0.5% of butylene glycol, 9% of glycerin, and the balance of water; is prepared by a conventional mixing and emulsifying method.
The corn germ extract was prepared by the preparation method of example 2.
The preparation method of the millettia extract comprises the following steps:
1) putting the Artocarpus heterophyllus in an agate mortar, and mixing the Artocarpus heterophyllus and ethanol according to the mass ratio of 2.7: adding ethanol according to the proportion of 1, grinding and crushing to obtain Artocarpus millefolius powder A;
2) putting the Artocarpus heterophyllus in a sealed inert gas atmosphere environment, carrying out treatment heat treatment at 200 ℃ for 12 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 1.6:1, grinding and crushing, and dropwise adding hyaluronic acid of which the mass is 13% of that of the millettia speciosa in the grinding process; obtaining Artocarpus heterophyllus powder B;
3) mixing the millettia speciosa powder A, the millettia speciosa powder B, water and ethanol uniformly according to the proportion of 10:1.2:42:15, adding dipotassium glycyrrhizinate accounting for 2.5% of the mass of the millettia speciosa extract, and performing ultrasonic extraction; respectively obtaining a first filtrate and a first filter residue after suction filtration;
4) placing the first filter residue after suction filtration in a closed oxygen atmosphere environment, carrying out thermal oxidation treatment at 360 ℃ for 15 minutes, and then cooling to room temperature; uniformly mixing the millettia subjected to thermal oxidation treatment according to the mass ratio of the millettia to the ethanol to the ascorbic acid to the EDTA of 3.0:0.9:0.21:0.08, and grinding and crushing to obtain millettia powder C;
5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate by 22% of the mass of the Artocarpus heterophyllus powder A in the step 3, uniformly mixing, performing secondary ultrasonic extraction, and performing suction filtration to obtain a second filtrate and a second filter residue respectively, wherein the second filtrate is Artocarpus heterophyllus extract.
The ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.
Example 7:
an anti-inflammatory repair emulsion containing corn germ extracting solution comprises the following components in percentage by mass: 0.46% of millettia extract, 2.5% of corn germ extract, 2.15% of magnesium ascorbyl phosphate, 2.6% of transparent acid, 0.38% of succinic acid, 0.18% of disteardimonium hectorite, 0.3% of methylparaben, 3.7% of glyceryl stearate PEG-75, 2.3% of polysorbate-80, 0.46% of stearyl alcohol, 1.98% of butanediol, 4% of glycerin, and the balance of water;
the corn germ extract was prepared by the preparation method of example 3.
The preparation method of the millettia extract comprises the following steps:
1) putting the Artocarpus heterophyllus in an agate mortar, and mixing the Artocarpus heterophyllus and ethanol according to the mass ratio of 3.3: adding ethanol according to the proportion of 1, grinding and crushing to obtain Artocarpus millefolius powder A;
2) putting the Artocarpus heterophyllus in a sealed inert gas atmosphere environment, carrying out treatment heat treatment at 180 ℃ for 8 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 1.5:1, grinding and crushing, and dropwise adding hyaluronic acid with the mass of 14% of the millettia speciosa in the grinding process; obtaining Artocarpus heterophyllus powder B;
3) mixing the Artocarpus heterophyllus powder A, Artocarpus heterophyllus powder B, water and ethanol at a ratio of 10:1.4:44:12, adding dipotassium glycyrrhizinate 3.8% of the extract, and ultrasonic extracting; respectively obtaining a first filtrate and a first filter residue after suction filtration;
4) placing the first filter residue after suction filtration in a closed oxygen atmosphere environment, carrying out thermal oxidation treatment at 336 ℃ for 15 minutes, and then cooling to room temperature; uniformly mixing the millettia subjected to thermal oxidation treatment according to the mass ratio of the millettia to the ethanol to the ascorbic acid to the EDTA of 2.85:0.9:0.17:0.076, and grinding and crushing to obtain millettia powder C;
5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate by 20% of the mass of the Artocarpus heterophyllus powder A in the step 3, uniformly mixing, performing secondary ultrasonic extraction, and performing suction filtration to obtain a second filtrate and a second filter residue respectively, wherein the second filtrate is Artocarpus heterophyllus extract. .
The ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.
Example 8:
an anti-inflammatory repair emulsion containing corn germ extracting solution comprises the following components in percentage by mass: 0.84% of millettia extract, 1.3% of corn germ extract, 0.76% of magnesium ascorbyl phosphate, 0.23% of transparent acid, 0.34% of succinic acid, 0.66% of disteardimonium hectorite, 0.68% of methylparaben, 2.46% of glyceryl stearate PEG-75, 0.44% of polysorbate-80, 0.54% of stearyl alcohol, 1.48% of butylene glycol, 8% of glycerin, and the balance of water;
the corn germ extract was prepared by the preparation method of example 4.
The preparation method of the millettia extract comprises the following steps:
1) putting the Artocarpus heterophyllus in an agate mortar, and mixing the Artocarpus heterophyllus and ethanol according to the mass ratio of 2.6: adding ethanol according to the proportion of 1, grinding and crushing to obtain Artocarpus millefolius powder A;
2) putting the Artocarpus heterophyllus in a sealed inert gas atmosphere environment, carrying out treatment heat treatment at 200 ℃ for 11 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 2.45:1, grinding and crushing, and dropwise adding hyaluronic acid with the mass of 14% of the millettia speciosa in the grinding process; obtaining Artocarpus heterophyllus powder B;
3) mixing the Artocarpus heterophyllus powder A, Artocarpus heterophyllus powder B, water and ethanol at a ratio of 10:1.28:49:13, adding dipotassium glycyrrhizinate 2.6% of the extract, and ultrasonic extracting; respectively obtaining a first filtrate and a first filter residue after suction filtration;
4) placing the first filter residue after suction filtration in a sealed oxygen atmosphere environment, carrying out thermal oxidation treatment at 324 ℃ for 16.5 minutes, and then cooling to room temperature; uniformly mixing the millettia subjected to thermal oxidation treatment according to the mass ratio of the millettia to the ethanol to the ascorbic acid to the EDTA of 2.8:0.92:0.27:0.06, and grinding and crushing to obtain millettia powder C;
5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate by 18% of the mass of the Artocarpus heterophyllus powder A in the step 3, uniformly mixing, performing secondary ultrasonic extraction, and performing suction filtration to obtain a second filtrate and a second filter residue respectively, wherein the second filtrate is Artocarpus heterophyllus extract.
The ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.
Comparative example 1:
an anti-inflammatory repair emulsion containing corn germ extract is different from example 8 in that the preparation steps of the millettia extract only comprise step 1 and step 3, the weight ratio of the millettia powder B in the step 3 is 0, and the obtained first filtrate is the millettia extract.
Comparative example 2:
an anti-inflammatory and repairing emulsion containing corn germ extract is different from example 8 in that the preparation of the millettia extract only comprises steps 1-3, and the first filtrate is millettia extract.
Comparative example 3:
an anti-inflammatory and repairing emulsion containing corn germ extract, which is different from example 8 in that the extract of Artocarpus heterophyllus is prepared without heat treatment in step 2.
Comparative example 4:
an anti-inflammatory and repairing emulsion containing corn germ extract is different from example 8 in that the millettia extract is prepared without thermal oxidation treatment in step 5.
Comparative example 5:
an anti-inflammatory repair emulsion containing corn germ extract is different from example 8 in that hyaluronic acid with the mass of 14% of millettia added in step 2 of the preparation step of the millettia extract is added after suction filtration in step 5.
Comparative example 6:
an anti-inflammatory and repairing emulsion containing corn germ extract is different from that of example 8 in that dipotassium glycyrrhizinate is not added in step 3 of the preparation step of the millettia extract.
Comparative example 7:
an anti-inflammatory and repair emulsion comprising corn germ extract, which is different from example 8 in that corn germ extract is not added.
Comparative example 8:
an anti-inflammatory repair emulsion containing corn germ extract is different from example 8 in that the corn germ extract is prepared without electrifying and activating, namely step d, and the filtrate obtained at the end of step c is the corn germ extract of the comparative example.
Comparative example 9:
an anti-inflammatory and repairing emulsion containing corn germ extract, which is different from the emulsion of example 8 in that the extract of Cryptocarya japonica is not added
Performance test
260 female volunteers with certain pox inflammation on the face are selected and tested (the age is 25-55 years, and the test meets the volunteer selection standard of the test subject), and the test is divided into eight groups. After each group of volunteers cleaned their face every morning and evening, the anti-inflammatory repair lotions according to examples 1 to 4 and comparative examples 1 to 8 were applied to the facial skin at 3 to 5 drops each time, and the following tests were performed.
1. Sensory evaluation
Volunteers performed sensory evaluation of the anti-inflammatory repair emulsions of examples 5 to 8 and comparative examples 1 to 9 according to feeling of use, and evaluated in terms of freshness, water-wettability, and comfort. The above effects were evaluated using 100 ratings, each group averaging the evaluation values, shown in table 1:
TABLE 1 results of sensory evaluation of the anti-inflammatory repair emulsions of examples 5 to 8 and comparative examples 1 to 9
Degree of relief | Degree of freshness | Lightness and thinness | Degree of mildness | Overall evaluation | |
Example 1 | 86.5 | 90.1 | 92.8 | 88.6 | 89.5 |
Example 2 | 85.8 | 88.7 | 92.4 | 91.9 | 89.7 |
Example 3 | 91.1 | 87.2 | 91.6 | 93.8 | 90.9 |
Example 4 | 93.6 | 92.0 | 95.1 | 94.3 | 93.8 |
Comparative example 1 | 60.9 | 68.7 | 64.1 | 79.3 | 68.3 |
Comparative example 2 | 77.6 | 78.1 | 84.9 | 82.6 | 80.8 |
Comparative example 3 | 73.5 | 76.8 | 86.2 | 83.1 | 79.9 |
Comparative example 4 | 79.2 | 78.3 | 85.7 | 83.6 | 81.7 |
Comparative example 5 | 73.6 | 74.8 | 84.3 | 82.9 | 78.9 |
Comparative example 6 | 71.3 | 77.2 | 85.0 | 80.8 | 78.6 |
Comparative example 7 | 64.8 | 71.6 | 70.0 | 76.0 | 70.6 |
Comparative example 8 | 72.6 | 78.0 | 84.7 | 82.3 | 79.4 |
Comparative example 9 | 61.2 | 72.3 | 71.8 | 80.4 | 71.4 |
Comparing examples 5-8 with comparative examples 1-2, it can be seen that the millettia extract of the invention improves the absorption of skin to each component and improves the use experience by reasonably matching the millettia extract with different extraction methods.
Comparing examples 5-8 with comparative example 3, it can be seen that the heat treatment in step 2 can promote the extraction of the active components of the Artocarpus heterophyllus during the extraction process, so as to improve the freshness and water-wettability and improve the use experience.
Comparing examples 5-8 with comparative example 4, it can be seen that in the extraction of the millettia extract of the present invention, the thermal oxidation treatment in step 4 can further extract trace metal elements in the millettia, and the use experience of the user can be improved by proper proportion. Meanwhile, as can be seen from comparison of comparative example 2 and comparative example 4, the effect and use experience of the millettia extract prepared by omitting steps 4 to 5 are close to those of the millettia extract prepared by omitting the thermal oxidation treatment only in step 4.
Comparing examples 5 to 8 with comparative example 5, it can be seen that the addition of hyaluronic acid with appropriate quality in step 2 of the present invention can improve the comfort, freshness, etc. of the user during use, thereby improving the use experience.
Comparing examples 5-8 with comparative example 6, it can be seen that the dipotassium glycyrrhizate added during the extraction of the extract of Artocarpus heterophyllus can be compatible with Artocarpus heterophyllus and synergically enhance the use experience.
Comparing examples 5-8 with comparative example 7, it can be seen that the addition of the corn germ extract solution of the present invention can improve the comfort and mildness of the user during use, and improve the use experience.
Comparing examples 5-8 with comparative example 8, it can be seen that the corn germ extract solution prepared by the energization activation method of the present invention can improve the comfort, freshness, etc. of the user, and improve the user experience.
Comparing examples 5-8 with comparative example 9, it can be seen that the addition of the extract of Artocarpus heterophyllus of the present invention can improve the comfort and mildness of the user during use and improve the use experience.
Comparing examples 5-8 with comparative examples 7 and 9, it can be seen that the addition of the millettia extract and the corn germ extract can greatly improve the comfort, freshness, lightness, thinness and mildness of the composition, and can comprehensively improve the use experience.
2. Skin barrier function repair test: the TEWL values were measured on the cheek area using a Tewameter TM300 after 2 and 4 weeks of continuous use, with the reference TEWL being measured in a dry, non-sweaty skin condition, at an ambient temperature of 25 ℃ and an ambient humidity of 45%. The integrity of skin barrier function is well reflected by the TEWL, an increase in TEWL values, meaning increased skin moisture emission, and conversely a decrease in TEWL values, indicating that the barrier has been repaired. The test results are shown in table 3.
TABLE 2 results of skin Barrier function repair test in examples 5-8 and comparative examples 1-9
Comparative examples 5 to 8 show that example 8 has the best repairing effect.
Comparing examples 5-8 with comparative examples 1-2, it can be seen that the millettia extract of the invention, which is extracted by different extraction methods, is reasonably matched, so that the absorption of the skin to each component is improved, and the repair effect of the anti-inflammatory repair emulsion to the skin barrier is improved.
Comparing examples 5-8 with comparative example 3, it can be seen that, in the extraction of the millettia extract of the present invention, the heat treatment in step 2 can promote the extraction of the active components of the millettia extract, and the repair effect of the anti-inflammatory repair emulsion can be improved by reasonable proportioning.
Comparing examples 5-8 with comparative example 4, it can be seen that in the extraction of the extract of melaleuca mollissima of the present invention, the thermal oxidation treatment in step 4 can further extract trace metal elements in melaleuca mollissima, and the repair effect of the anti-inflammatory repair emulsion is improved by proper proportioning.
Comparing examples 5-8 with comparative example 5, it can be seen that the addition of hyaluronic acid with appropriate quality in the extraction process of step 2 can promote the extraction of the active components of Artocarpus heterophyllus and improve the repair effect of the anti-inflammatory repair emulsion.
Comparing examples 5-8 with comparative example 6, it can be seen that the dipotassium glycyrrhizate added during the extraction of the extract of Artocarpus heterophyllus of the present invention can be compatible with Artocarpus heterophyllus and synergistically enhance the repair effect of the anti-inflammatory repair emulsion.
Comparing examples 5-8 with comparative example 7, it can be seen that the addition of the corn germ extract of the present invention can enhance the repair effect of the anti-inflammatory repair emulsion.
Comparing examples 5-8 with comparative example 8, it can be seen that the corn germ extract solution prepared by the electrifying activation method of the present invention can improve the repair effect of the anti-inflammatory repair emulsion.
It can be seen from comparison of examples 5 to 8 and comparative example 9 that the addition of the extract of Artocarpus heterophyllus of the present invention can improve the repair effect of the anti-inflammatory repair emulsion.
Comparing examples 5-8 with comparative examples 7 and 9, it can be seen that the repair effect of the anti-inflammatory repair emulsion can be greatly improved by simultaneously adding the millettia extract and the corn germ extract.
3. Anti-inflammatory function test: after 2 and 4 weeks of continuous use, the skin surface pox inflammation condition is taken as a standard:
and (4) invalidation: no obvious change of pox inflammation
Slight: slight decrease in pox inflammation
It is obvious that: clear elimination of pox inflammation
The test results are shown in table 3.
Table 3: results of anti-inflammatory repair test for examples 5-8 and comparative examples 1-9
Comparative examples 5 to 8 show that example 8 has the best anti-inflammatory effect on pox inflammation on the skin surface.
Comparing examples 5-8 with comparative examples 1-2, it can be seen that the millettia extract liquid extracted by different extraction methods is reasonably matched, so that the absorption of the skin to each component is improved, and the anti-inflammatory repair effect of the anti-inflammatory repair emulsion on the pox inflammation on the surface of the skin is improved.
Comparing examples 5-8 with comparative example 3, it can be seen that, in the extraction of the millettia extract of the present invention, the heat treatment in step 2 can promote the extraction of the millettia active component, and the anti-inflammatory repair effect of the anti-inflammatory repair emulsion on the pox inflammation on the skin surface can be improved through reasonable proportion.
Comparing examples 5-8 with comparative example 4, it can be seen that in the extraction of the extract of millettia speciosa of the present invention, the thermal oxidation treatment in step 4 can further extract trace metal elements in the millettia speciosa, and the anti-inflammatory repair effect of the anti-inflammatory repair emulsion on the pox inflammation on the skin surface can be improved by proper proportion.
Comparing examples 5-8 with comparative example 5, it can be seen that the addition of hyaluronic acid with appropriate quality in the extraction process of step 2 can promote the extraction of the active components of Artocarpus heterophyllus and improve the repair effect of the anti-inflammatory repair emulsion.
Comparing examples 5-8 with comparative example 6, it can be seen that the dipotassium glycyrrhizate added during the extraction of the extract of the millettia speciosa of the invention can be compatible with the millettia speciosa and synergistically enhance the anti-inflammatory repair effect of the anti-inflammatory repair emulsion on the pox inflammation on the skin surface.
As can be seen from the comparison of examples 5-8 and comparative example 7, the addition of the corn germ extract solution of the invention can improve the anti-inflammatory repair effect of the anti-inflammatory repair emulsion on the pox inflammation on the skin surface.
Comparing examples 5-8 with comparative example 8, it can be seen that the corn germ extract prepared by the energization activation method of the invention can improve the anti-inflammatory repair effect of the anti-inflammatory repair emulsion on pox inflammation on the skin surface.
It can be seen from comparative examples 5 to 8 and comparative example 9 that the addition of the extract solution of Artocarpus heterophyllus of the present invention can enhance the anti-inflammatory repair effect of the anti-inflammatory repair emulsion.
As can be seen from the comparison of examples 5-8 and comparative examples 7 and 9, the anti-inflammatory repair effect of the anti-inflammatory repair emulsion can be greatly improved by simultaneously adding the millettia extract and the corn germ extract.
The foregoing has outlined rather broadly the preferred embodiments and principles of the present invention and it will be apparent to those skilled in the art that various changes in the detailed description may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The preparation method of the corn germ extracting solution is characterized by comprising the following steps:
a) mashing corn germs, uniformly mixing the corn germs, ethanol, butanediol and water according to the mass ratio of 8:1-4:0.5-1:20-30, and adding 0.5-3% of compound protease of the corn germs for enzymolysis to obtain an enzymolysis liquid;
b) b, performing ultrasonic extraction on the enzymatic hydrolysate obtained in the step a, and performing suction filtration to obtain filtrate;
c) adding 5-8% of sodium citrate and 1-3% of potassium chloride into the filtrate;
d) and (b) taking a cathode electrode and an anode electrode which are both platinum electrodes, taking the filtrate obtained in the step b) as catholyte, taking an aqueous solution of sodium citrate with the mass concentration of 5% -8% and potassium chloride with the mass concentration of 1% -3% as anolyte, separating the cathode and the anode by using an anion exchange membrane, and electrifying and activating to obtain the corn germ extracting solution.
2. The method for preparing the corn germ extracting solution according to claim 1, wherein the compound protease is papain, trypsin, carboxypeptidase and neutral protease in a ratio of 1:1:3:2, the enzymolysis time is 40-80min, and the enzymolysis temperature is 34-39 ℃.
3. The method for preparing corn germ extract as claimed in claim 1, wherein the current density for activation by electrification is 1-20A/m2The temperature is 20-50 ℃.
4. The method for preparing the corn germ extracting solution as claimed in claim 1, wherein the ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.
5. The anti-inflammatory repair emulsion containing the corn germ extracting solution is characterized by comprising the following components in percentage by mass: 0.2% -2.6% of millettia extract, 0.8% -1.7% of corn germ extract, 0.15% -2.2% of magnesium ascorbyl phosphate, 0.1% -5% of hyaluronic acid, 0.1% -0.5% of succinic acid, 0.1% -0.8% of disteardimonium hectorite, 0.2% -0.9% of methylparaben, 2% -4% of glyceryl stearate PEG-75, 0.1% -2.3% of polysorbate-80, 0.1% -0.6% of stearyl alcohol, 0.1% -3% of butanediol, 3% -10% of glycerol and the balance of water;
the corn germ extract is prepared by the method of any one of claims 1 to 4.
6. The anti-inflammatory and repairing emulsion containing corn germ extracting solution according to claim 5,
the preparation method of the millettia extract comprises the following steps:
1) putting the Artocarpus heterophyllus in a mortar, and mixing according to the mass ratio of Artocarpus heterophyllus to ethanol of 2.5-3.5: adding ethanol according to the proportion of 1, grinding and crushing to obtain Artocarpus millefolius powder A;
2) putting the Artocarpus mollis into a sealed inert gas atmosphere environment, carrying out treatment heat treatment at 130-200 ℃ for 8-13 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 1.5-2.8:1, grinding and crushing, and dropwise adding hyaluronic acid of which the mass is 12-17% of that of the millettia speciosa in the grinding process; obtaining Artocarpus heterophyllus powder B;
3) mixing Artocarpus heterophyllus powder A, Artocarpus heterophyllus powder B, water and ethanol at a ratio of 10: 0.9-1.4: uniformly mixing the components in a ratio of 40-50:12-16, and performing ultrasonic extraction; respectively obtaining a first filtrate and a first filter residue after suction filtration;
4) placing the first filter residue after suction filtration in a sealed oxygen atmosphere environment, performing thermal oxidation treatment at 310-340 ℃ for 15-18 minutes, and then cooling to room temperature; uniformly mixing the millettia subjected to thermal oxidation treatment according to the mass ratio of 2.4-3.4:0.7-1.2:0.1-0.3:0.05-0.1 of the millettia, and grinding and crushing to obtain millettia powder C;
5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate in an amount which is 12-25% of the mass of the Artocarpus heterophyllus powder A in the step 3, uniformly mixing, performing secondary ultrasonic extraction, and performing suction filtration to obtain a second filtrate and a second filter residue respectively, wherein the second filtrate is Artocarpus heterophyllus extract.
7. The anti-inflammatory and repairing emulsion containing corn germ extracting solution as claimed in claim 6, wherein dipotassium glycyrrhizinate is added to the filtrate of step 3 in an amount of 2.1% -4.3% by mass of the extract of Artocarpus heterophyllus.
8. The anti-inflammatory and repair emulsion comprising corn germ extract as claimed in claim 6, wherein the mortar is agate mortar.
9. The anti-inflammatory repair emulsion containing the corn germ extracting solution as claimed in claim 6, which is characterized by comprising the following components in percentage by mass: 0.84% of millettia extract, 1.3% of corn germ extract, 0.76% of magnesium ascorbyl phosphate, 0.23% of hyaluronic acid, 0.34% of succinic acid, 0.66% of disteardimonium hectorite, 0.68% of methylparaben, 2.46% of glyceryl stearate PEG-75, 0.44% of polysorbate-80, 0.54% of stearyl alcohol, 1.48% of butanediol, 8% of glycerin, and the balance of water.
10. The anti-inflammatory and repairing emulsion containing corn germ extracting solution as claimed in claim 6, wherein the ethanol is absolute ethanol or 95% ethanol.
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