CN113318025A - Preparation method of Artocarpus heterophyllus extract and moisturizing and repairing composition - Google Patents

Abstract

A method for preparing Artocarpus heterophyllus extract comprises the following steps: 1) putting Artocarpus mollis into a mortar, adding ethanol, grinding and crushing to obtain powder A; 2) placing the Artocarpus heterophyllus in inert atmosphere for heat treatment; mixing the heat-treated Artocarpus mollis with ethanol at a certain proportion, grinding, and adding hyaluronic acid dropwise during grinding; obtaining powder B; 3) mixing powder A, B, water and ethanol at a certain proportion, ultrasonic extracting, and vacuum filtering; 4) placing the filter residue in an oxygen environment for thermal oxidation treatment; uniformly mixing the millettia subjected to thermal oxidation treatment with millettia, ethanol, ascorbic acid and EDTA according to a certain proportion, and grinding and crushing to obtain powder C; 5) adding the powder C into the filtrate, mixing, performing secondary ultrasonic extraction, and performing suction filtration to obtain filtrate to obtain Artocarpus millettii extractive solution. According to the invention, the components of the Artocarpus heterophyllus are fully extracted through the treatment processes of grinding, heat treatment, ultrasonic extraction, thermal oxidation treatment and the like, so that the components of the Artocarpus heterophyllus are fully and reasonably utilized.

Description

Preparation method of Artocarpus heterophyllus extract and moisturizing and repairing composition

Technical Field

The invention belongs to the field of skin care products, and particularly relates to a preparation method of a millettia extract and a moisturizing and repairing composition

Background

The skin is the outermost layer structure of the human body, is the largest organ of the human body, is a sensory organ of the nervous system and an effector, can reflexively cause the change of the skin to external stimulation, and can be more and more quickly lost along with the continuous fading of the physiological function of the human body under the influence of adverse factors such as pollution, pressure, ultraviolet rays and the like, the phenomenon of skin damage frequently occurs, the skin aging can be accelerated, signs such as wrinkles, color spots, skin looseness, chin contour change and the like can be generated in advance, and the signs can be continuously worsened and even different degrees of inflammation can be generated, 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 eliminated, 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 skin repairing cream can help repair skin matrixes and promote self repair and renewal of the skin structures, and rich antioxidant ingredients can help the skin to resist environmental pressure, slow down aging, and be 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.

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 keeping moisture and supplementing water, reduce ultraviolet light damage, and rapidly adapt to the change of weather. 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, and reasonable utilization of the millettia components cannot be realized, and the cost is high.

Disclosure of Invention

Based on the defects and shortcomings in the prior art, the invention aims to provide a method for preparing a millettia extract, which comprehensively extracts various components of the millettia according to the characteristics of the different components and can realize the full and reasonable utilization of the millettia components.

The composition can realize good moisturizing and repairing effects by fully extracting the Artocarpus heterophyllus and scientifically matching the Artocarpus heterophyllus extract and other components.

In order to achieve the purpose, the invention adopts the technical scheme that:

a method for preparing Artocarpus heterophyllus extract comprises the following steps:

1) putting the Artocarpus heterophyllus in a 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) placing the Artocarpus mollis in a sealed inert gas atmosphere environment, carrying out treatment heat treatment at the temperature of 120-230 ℃ for 10-15 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 1-3:1, grinding and crushing, and dropwise adding hyaluronic acid of which the mass is 10-15% 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: 1.0-1.5: uniformly mixing the components in a ratio of 30-40:10-20, 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 the temperature of 300-360 ℃ 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 the millettia to the ethanol to the ascorbic acid to the EDTA of 2-5:0.8-1:0.1-0.2:0.05-0.1, and grinding to obtain millettia powder C;

5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate in an amount which is 10-30% 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.

Preferably, 1 to 5 percent of dipotassium glycyrrhizinate in mass of the extract of the millettia speciosa is added into the filtrate in the step 3.

Preferably, the ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-500W.

Preferably, the ethanol is absolute ethanol or 95% ethanol.

Preferably, the mortar is agate mortar.

The invention also provides a moisturizing and repairing composition containing the millettia extract, which comprises the following components in percentage by mass: the composite material comprises the following components in percentage by mass: 1 to 4 percent of millettia extract, 0.01 to 1 percent of sodium hyaluronate, 0.01 to 0.1 percent of carbomer, 0.01 to 1 percent of xanthan gum T, 0.05 to 2 percent of oat glucan powder, 0.01 to 0.1 percent of arginine, 0.1 to 3 percent of saccharomyces bicolor extract, 0.1 to 0.8 percent of p-hydroxyacetophenone, 1 to 10 percent of butanediol, 1 to 8 percent of glycerin, 0.1 to 0.9 percent of 1, 2-hexanediol, 0.5 to 3 percent of soothing agent and the balance of water.

The Artocarpus heterophyllus extract is prepared by the above preparation method.

The soothing agent consists of the following components: 7-15% of a field mint extract, 10-18% of a sophora flavescens extract, 10-18% of a purslane extract, 1-6% of a chamomile extract, 2-7% of an aloe barbadensis flower extract, 7-12% of a geranium extract, 10-20% of butanediol, 7-15% of glycerol, 0.1-1% of 1, 2-hexanediol, 0.01-0.5% of p-hydroxyacetophenone, and the balance of water.

Preferably, the sodium hyaluronate consists of high molecular weight sodium hyaluronate and low molecular weight sodium hyaluronate according to a ratio of 1: 2; the high molecular weight sodium hyaluronate is 100 kilodaltons of sodium hyaluronate, and the low molecular weight sodium hyaluronate is 20 kilodaltons of sodium hyaluronate.

Preferably, the paint consists of the following components in percentage by mass: 1.96% of millettia extract, 0.147% of sodium hyaluronate, 0.069% of carbomer, 0.049% of xanthan gum T, 0.098% of oat glucan powder, 0.083% of arginine, 0.98% of schizosaccharomyces cerevisiae extract, 0.29% of p-hydroxyacetophenone, 3.92% of butanediol, 2.94% of glycerol, 0.69% of 1, 2-hexanediol, 1.47% of a soothing agent and the balance of water.

Preferably, the soothing agent consists of the following components:

9% of a field mint extract, 12% of a sophora flavescens extract, 12% of a purslane extract, 3% of a chamomile extract, 5% of an aloe barbadensis flower extract, 9% of a geranium extract, 15% of butanediol, 10% of glycerol, 0.51, 2-hexanediol, 0.3% of p-hydroxyacetophenone, and the balance of water.

The invention has the beneficial effects that:

1. according to the preparation method of the extract of the Artocarpus heterophyllus, the components of the Artocarpus heterophyllus are fully extracted through the treatment processes of grinding, heat treatment and grinding, ultrasonic extraction, thermal oxidation treatment of filter residues, secondary ultrasonic extraction and the like, so that the components of the Artocarpus heterophyllus are fully and reasonably utilized.

2. The preparation method adopted by the invention is characterized in that dipotassium glycyrrhizinate is added in the preparation process, so that the dipotassium glycyrrhizinate and the components of the millettia are mutually promoted to be absorbed by the skin, the synergistic effect is achieved, and the moisturizing, repairing and moisturizing effects are enhanced.

3. 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 the residue, and the full absorption of the skin to all the components can be improved by reasonable proportioning.

4. The soothing agent added in the invention can relieve and condition skin imbalance caused by long-time pressure, relieve redness, fever and stabbing pain, and keep the skin stable.

5. According to the invention, through scientific compatibility of the components, the synergistic interaction effect among the components is realized, the long-acting moisturizing and repairing effect can be realized, and the moisturizing and repairing effect can be kept fresh and cool, and the moisturizing and repairing effect is 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 method for preparing Artocarpus heterophyllus 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 2.3: 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 130 ℃ for 15 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 3:1, 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 effect of the millettia speciosa is enhanced.

3) Mixing the millettia speciosa powder A, the millettia speciosa powder B, water and ethanol uniformly according to the proportion of 10:1.0:40:20, adding dipotassium glycyrrhizinate accounting for 5% of the mass of the millettia speciosa extract, and carrying out 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 for 16 minutes at 320 ℃, 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 2:1:0.1:0.05, 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% 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 320 ℃ in a sealed oxygen atmosphere environment; after cooling, grinding and extracting by using 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 all components in the Artocarpus heterophyllus.

The ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.

Example 2:

a method for preparing Artocarpus heterophyllus 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 5: 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 1.5:1, 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 10:1.2:34:16, adding dipotassium glycyrrhizinate accounting for 1.5% 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, performing 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 5:0.9:0.15:0.08, and grinding and crushing to obtain millettia powder C;

5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate by 28% 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 3:

a method for preparing Artocarpus heterophyllus 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 4.2: 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 13 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 5:1, grinding and crushing, and dropwise adding hyaluronic acid with the mass of 12% 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 ratio of 10:1.4:32:17, adding dipotassium glycyrrhizinate 1.5 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, performing 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 5:0.9:0.15:0.08, 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 4:

a method for preparing Artocarpus heterophyllus 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 1.6: 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 142 ℃ for 14 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 3.3:1, 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 10:1.42:38:17, adding dipotassium glycyrrhizinate 1.5 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, performing thermal oxidation treatment at 334 ℃ 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 3.8:0.92:0.17:0.06, 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 5:

a moisturizing and repairing composition containing a millettia extract comprises the following components in percentage by mass: 2.3% of millettia extract, 0.5% of sodium hyaluronate, 0.01% of carbomer, 0.7% of xanthan gum T, 1% of oat glucan powder, 0.02% of arginine, 3% of saccharomyces bifidus extract, 0.1% of p-hydroxyacetophenone, 1.2% of butanediol, 8% of glycerol, 0.9% of 1, 2-hexanediol, 0.6% of a soothing agent and the balance of water;

the soothing agent consists of the following components: 13% of a field mint extract, 17% of a sophora flavescens extract, 10.4% of a purslane extract, 5.7% of a golden chamomile extract, 6.5% of an aloe barbadensis flower extract, 11% of a pelargonium roseum extract, 12.8% of butanediol, 13% of glycerol, 0.71% of 1, 2-hexanediol, 0.27% of p-hydroxyacetophenone, and the balance of water.

The extract of Artocarpus heterophyllus was prepared as in example 1.

Example 6:

a moisturizing and repairing composition containing a millettia extract comprises the following components in percentage by mass: 1.44% of millettia extract, 0.84% of sodium hyaluronate, 0.038% of carbomer, 0.15% of xanthan gum T, 2% of oat glucan powder, 0.047% of arginine, 0.12% of saccharomyces cerevisiae extract, 0.43% of p-hydroxyacetophenone, 7.6% of butanediol, 1.8% of glycerol, 0.2% of 1, 2-hexanediol, 2.5% of a soothing agent and the balance of water.

The soothing agent consists of the following components: 10% of a field mint extract, 15.44% of a sophora flavescens extract, 13.8% of a purslane extract, 1.87% of a golden chamomile extract, 4.3% of an aloe barbadensis flower extract, 11.5% of a geranium extract, 10.6% of butanediol, 7% of glycerol, 0.8% of 1, 2-hexanediol, 0.02% of p-hydroxyacetophenone and the balance of water.

The extract of Artocarpus heterophyllus prepared in example 2 was used as the extract of Artocarpus heterophyllus.

Example 7:

a moisturizing and repairing composition containing Artocarpus heterophyllus extract comprises 3.24% of Artocarpus heterophyllus extract, 0.1% of sodium hyaluronate, 0.05% of carbomer, 0.54% of xanthan gum T, 0.05% of oat glucan powder, 0.06% of arginine, 2.1% of Saccharomyces bifidus extract, 0.74% of p-hydroxyacetophenone, 9% of butanediol, 4% of glycerol, 0.4% of 1, 2-hexanediol, 1.8% of a soothing agent and the balance of water;

the soothing agent consists of the following components: 12% of a field mint extract, 11% of a sophora flavescens extract, 15% of a purslane extract, 4% of a chamomile extract, 2% of an aloe barbadensis flower extract, 8% of a geranium extract, 20% of butanediol, 15% of glycerol, 0.12% of 1, 2-hexanediol, 0.5% of p-hydroxyacetophenone, and the balance of water.

The extract of Artocarpus heterophyllus was prepared in example 3.

Example 8:

a moisturizing and repairing composition containing a millettia extract comprises the following components in percentage by mass: 1.96% of millettia extract, 0.147% of sodium hyaluronate, 0.069% of carbomer, 0.049% of xanthan gum T, 0.098% of oat glucan powder, 0.083% of arginine, 0.98% of schizosaccharomyces cerevisiae extract, 0.29% of p-hydroxyacetophenone, 3.92% of butanediol, 2.94% of glycerol, 0.69% of 1, 2-hexanediol, 1.47% of a soothing agent and the balance of water.

The soothing agent consists of the following components:

9% of a field mint extract, 12% of a sophora flavescens extract, 12% of a purslane extract, 3% of a chamomile extract, 5% of an aloe barbadensis flower extract, 9% of a geranium extract, 15% of butanediol, 10% of glycerol, 0.51, 2-hexanediol, 0.3% of p-hydroxyacetophenone, and the balance of water.

The extract of Artocarpus heterophyllus was prepared in example 4.

Comparative example 1:

a moisturizing and repairing composition containing a millettia extract, which is different from the composition in example 8 in that the preparation steps of the millettia extract only comprise step 1 and step 3, the mass ratio of the millettia powder B in the step 3 is 0, and the obtained first filtrate is the millettia extract.

Comparative example 2:

a moisturizing and repairing composition containing a millettia extract, which is different from the composition in example 8 in that the millettia extract is prepared only by the steps 1-3, and the first filtrate is the millettia extract.

Comparative example 3:

a moisturizing and repairing composition containing an extract of millettia speciosa, which is different from example 8 in that the extract of millettia speciosa is prepared without heat treatment in step 2.

Comparative example 4:

a moisturizing and repairing composition containing an extract of millettia speciosa, which is different from example 8 in that the extract of millettia speciosa is prepared without performing thermal oxidation treatment in step 5.

Comparative example 5:

a moisturizing and repairing composition containing a millettia extract, which is different from example 8 in that hyaluronic acid of 14% of the quality of the millettia added in step 2 of the preparation step of the millettia extract is added after suction filtration in step 5.

Comparative example 6:

a moisturizing and repairing composition containing an extract of melaleuca molle, which is different from example 8 in that dipotassium glycyrrhizinate is not added in step 3 of the preparation step of the extract of melaleuca molle.

Comparative example 7:

a moisturizing and repairing composition containing Artocarpus heterophyllus extract is different from that in example 8 in that no soothing agent is added

Performance test

200 healthy female volunteers were randomly selected for testing (age 25-55 years, meeting the volunteer selection criteria of the subject) and divided into eight groups. After each group of volunteers cleaned their face in the morning and evening, the moisturizing and healing compositions corresponding to examples 5-8 and comparative examples 1-7 were applied to the facial skin at 3-5 drops each time, and the following tests were performed.

1. Sensory evaluation

The moisturizing repair compositions of examples 5 to 8 and comparative examples 1 to 7 were subjected to sensory evaluation by volunteers according to the feeling of use, and evaluated for freshness, moisture, and comfort. The above effects were evaluated using 10 ranks, each set averaging the evaluation values, shown in table 1:

table 1 sensory evaluation results of moisturizing repair compositions of examples 5 to 8 and comparative examples 1 to 7

	Degree of freshness	Degree of water wettability	Comfort level	Overall evaluation
					Example 5	8.6	8.5	8.9	8.67
Example 6	9.0	8.6	8.9	8.83
					Example 7	9.0	9.1	8.9	9.00
Example 8	9.1	9.3	9.4	9.27
					Comparative example 1	6.4	6.3	7.4	6.70
Comparative example 2	7.6	8.0	8.3	7.97
					Comparative example 3	7.7	7.5	8.1	7.77
Comparative example 4	7.8	8.1	8.4	8.10
					Comparative example 5	7.5	7.0	8.2	7.57
Comparative example 6	7.3	7.8	8.1	7.73
					Comparative example 7	6.7	7.4	6.9	7.00

Comparing examples 5-8 with comparative examples 1-2, it can be seen that the millettia extract of the present 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 use experience of the user is improved.

Comparing examples 5-8 with comparative example 3, it can be seen that the heat treatment of 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-retention degree and improve the use experience of users.

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 use experience of the user is improved by proper proportioning. 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 of suitable quality in step 2 according to the present invention can improve the freshness, moisture and comfort of the user in use.

Comparing examples 5-8 with comparative example 6, it can be seen that the dipotassium glycyrrhizinate added during the extraction of the extract of the millettia speciosa can be compatible with the millettia speciosa and synergically enhance the use experience of users.

Comparing examples 5-8 with comparative example 7, it can be seen that the added soothing agent can significantly improve the refreshing degree and comfort of the user during use, and improve the use experience.

2. Skin moisture content test: the amount of water lost between the skin cutin smeared for 1 hour and the skin cutin smeared for 8 hours was measured by a Skicon-200EX type flat skin hygrometer, and the results are shown in Table 2.

3. Percutaneous water loss: the water loss after 1 hour after the skin is smeared and 8 hours after the skin is smeared is detected according to T/ZHCA003-2018 'cosmetic influence transdermal water loss test method', and the result is shown in Table 2.

TABLE 2 compositions of examples 5-8 and comparative examples 1-7 moisture retention Performance test

As can be seen from comparative examples 5 to 8, example 8 exhibited the best moisturizing effect.

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 moisturizing effect of the composition by reasonably matching the millettia extract extracted by different extraction methods.

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 moisturizing effect of the composition 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 moisturizing effect of the composition can be improved by proper proportioning.

Comparing examples 5 to 8 with comparative example 5, it can be seen that the addition of hyaluronic acid of an appropriate quality during the extraction process of step 2 according to the present invention can improve the moisturizing effect of the composition.

Comparing examples 5-8 with comparative example 6, it can be seen that the dipotassium glycyrrhizinate added during the extraction of the extract of the millettia speciosa can be compatible with the millettia speciosa and synergistically enhance the moisturizing effect of the composition.

Comparing examples 5-8 with comparative example 7, it can be seen that the added soothing agent can improve the moisturizing effect of the composition through reasonable proportioning.

4. Skin barrier function repair test: the TEWL values were measured on the cheek area using a Tewameter TM300 after 1,2 and 4 weeks of continuous use in volunteers, with the baseline 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 3 results of skin barrier function repair test in examples 5 to 8 and comparative examples 1 to 7

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 improves the absorption of the skin to each component and improves the repair effect of the composition to the skin barrier by reasonably matching the millettia extract extracted by 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 Artocarpus heterophyllus and improve the repairing effect of the composition by reasonable proportioning during the extraction of Artocarpus heterophyllus of the present invention.

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 repair effect of the composition can be 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 repairing effect of the composition.

Comparing examples 5-8 with comparative example 6, it can be seen that the dipotassium glycyrrhizinate added during the extraction of the extract of the millettia speciosa can be compatible with the millettia speciosa and synergistically enhance the repair effect of the composition.

Comparing examples 5-8 with comparative example 7, it can be seen that the added soothing agent of the present invention can improve the repairing effect of the composition by reasonable proportioning.

The foregoing has outlined rather broadly the preferred embodiments and principles of the present invention and it will be appreciated that those skilled in the art may devise variations of the present invention that are within the spirit and scope of the appended claims.

Claims (9)

1. The preparation method of the millettia extract is characterized by comprising the following steps:

1) putting the Artocarpus heterophyllus in a 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) placing the Artocarpus mollis in a sealed inert gas atmosphere environment, carrying out treatment heat treatment at the temperature of 120-230 ℃ for 10-15 minutes, and then cooling to room temperature; uniformly mixing the heat-treated millettia speciosa with ethanol according to the mass ratio of 1-3:1, grinding and crushing, and dropwise adding hyaluronic acid of which the mass is 10-15% 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: 1.0-1.5: uniformly mixing the components in a ratio of 30-40:10-20, 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 the temperature of 300-360 ℃ 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 the millettia to the ethanol to the ascorbic acid to the EDTA of 2-5:0.8-1:0.1-0.2:0.05-0.1, and grinding to obtain millettia powder C;

5) adding the obtained Artocarpus heterophyllus powder C into the first filtrate in an amount which is 10-30% 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.

2. The method for preparing an extracting solution of Artocarpus heterophyllus according to claim 1, wherein 1% -5% dipotassium glycyrrhizinate by mass of the extracting solution of Artocarpus heterophyllus is added to the filtrate of step 3.

3. The method as claimed in claim 1, wherein the ultrasonic leaching time is 10-15min, the frequency is 20kHz-40kHz, and the power is 200-.

4. The method of claim 1, wherein the ethanol is absolute ethanol or 95% ethanol.

5. The method for preparing the extract of Artocarpus millettii Schneid according to claim 1, wherein the mortar is agate mortar.

6. The moisturizing and repairing composition containing the millettia extract is characterized by comprising the following components in percentage by mass: 1 to 4 percent of millettia extract, 0.01 to 1 percent of sodium hyaluronate, 0.01 to 0.1 percent of carbomer, 0.01 to 1 percent of xanthan gum T, 0.05 to 2 percent of oat glucan powder, 0.01 to 0.1 percent of arginine, 0.1 to 3 percent of saccharomyces bicolor extract, 0.1 to 0.8 percent of p-hydroxyacetophenone, 1 to 10 percent of butanediol, 1 to 8 percent of glycerin, 0.1 to 0.9 percent of 1, 2-hexanediol, 0.5 to 3 percent of soothing agent and the balance of water;

the preparation method of the extract of Artocarpus heterophyllus according to any one of claims 1-5;

the soothing agent consists of the following components: 7-15% of a field mint extract, 10-18% of a sophora flavescens extract, 10-18% of a purslane extract, 1-6% of a chamomile extract, 2-7% of an aloe barbadensis flower extract, 7-12% of a geranium extract, 10-20% of butanediol, 7-15% of glycerol, 0.1-1% of 1, 2-hexanediol, 0.01-0.5% of p-hydroxyacetophenone, and the balance of water.

7. The moisturizing and repairing composition containing extract of millettia speciosa as claimed in claim 6, wherein the sodium hyaluronate is prepared from high molecular weight sodium hyaluronate and low molecular weight sodium hyaluronate in a ratio of 1: 2; the high molecular weight sodium hyaluronate is 100 kilodaltons of sodium hyaluronate, and the low molecular weight sodium hyaluronate is 20 kilodaltons of sodium hyaluronate.

8. The moisturizing and repairing composition containing the extract of Artocarpus heterophyllus as claimed in claim 6, which is characterized by comprising the following components in percentage by mass: 1.96% of millettia extract, 0.147% of sodium hyaluronate, 0.069% of carbomer, 0.049% of xanthan gum T, 0.098% of oat glucan powder, 0.083% of arginine, 0.98% of schizosaccharomyces cerevisiae extract, 0.29% of p-hydroxyacetophenone, 3.92% of butanediol, 2.94% of glycerol, 0.69% of 1, 2-hexanediol, 1.47% of a soothing agent and the balance of water.

9. The moisturizing and repairing composition containing the extract of Artocarpus heterophyllus as claimed in claim 6, wherein the soothing agent is composed of the following components:

9% of a field mint extract, 12% of a sophora flavescens extract, 12% of a purslane extract, 3% of a chamomile extract, 5% of an aloe barbadensis flower extract, 9% of a geranium extract, 15% of butanediol, 10% of glycerol, 0.51, 2-hexanediol, 0.3% of p-hydroxyacetophenone, and the balance of water.