CN113181089A - Soothing and repairing composition and preparation method and application thereof - Google Patents
Soothing and repairing composition and preparation method and application thereof Download PDFInfo
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- CN113181089A CN113181089A CN202110305740.6A CN202110305740A CN113181089A CN 113181089 A CN113181089 A CN 113181089A CN 202110305740 A CN202110305740 A CN 202110305740A CN 113181089 A CN113181089 A CN 113181089A
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Classifications
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
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Abstract
The invention discloses a soothing and repairing composition and a preparation method thereof, and belongs to the field of plant extraction research. The composition comprises purslane, fructus kochiae, duckweed, honeysuckle, dark plum and herba schizonepetae, and the skin problem induced by various factors such as environment, region, night, pressure, season change and the like is solved through the interaction of the components and multi-channel effect. The soothing and repairing composition has the effects of immediately relieving skin redness, pruritus and stabbing pain, removing free radicals, resisting inflammation, improving skin tolerance, repairing skin barriers and the like. It is applied in cosmetics and expected to have the effects of anti-irritation, skin soothing, antioxidation, anti-inflammation, skin barrier repair and the like.
Description
Technical Field
The invention relates to the field of plant extraction research, and particularly relates to a soothing and repairing composition and a preparation method and application thereof.
Background
With the rapid development of social urbanization and industrialization, environmental pollution and cosmetic stimulation cause more and more problems such as sensitive muscles, mask faces and hormone faces. Due to epidemic situations, people need to wear the mask every day, so that various skin problems are aggravated, and great troubles are brought to consumers both physically and psychologically. These skin problems have many similar symptoms, accompanied by impaired skin barrier function, skin intolerance, skin inflammation, etc., and the repair mechanism is complicated, requiring multi-channel synergy. Simply speaking, the skin-care product has the effects of repairing barriers, inhibiting bacteria, diminishing inflammation, relieving swelling and itching, improving skin tolerance and the like and simultaneously acts on the skin, the problem cannot be fundamentally solved by single-channel mechanism repair, the symptoms can be relieved only once, and the skin-care product is easy to repeatedly do.
Patent (CN 112137932A) discloses an anti-allergy remedy composition, which comprises extracts of KOCHIA SCOPARIA (KOCHIA SCOPARIA), CHAMOMILLA RECUTITA (CHAMOMILLA RECUTITA), salviae miltiorrhizae (salviae miltiorrhizae) root, purslane (PORTULACA OLERACEA), and PIPER METHYSTICUM (PIPER METHYSTICUM) leaf/root/stem. However, the composition only relieves the symptoms of the problem skin from the perspective of relieving the skin from redness, dryness, itching, burning, stinging, and the like.
Therefore, in view of the current situation that the action path is single and the skin problem cannot be fundamentally solved, it is very necessary to develop a plant extract which can relieve the problem skin through the synergistic action of multiple paths.
Disclosure of Invention
The invention mainly aims to provide a soothing and repairing composition and a preparation method thereof.
The soothing and repairing composition has the effects of immediately relieving skin redness, pruritus and stabbing pain, removing free radicals, resisting inflammation, improving skin tolerance, repairing skin barriers and the like.
Therefore, the technical scheme provided by the application is as follows:
in a first aspect, the present invention provides a soothing and repairing composition.
According to the invention, the soothing and repairing composition comprises the following components in parts by weight: 5-40 parts of purslane, 1-30 parts of fructus kochiae, 5-20 parts of duckweed, 1-20 parts of honeysuckle, 3-15 parts of dark plum and 1-10 parts of schizonepeta.
According to the present invention, the soothing repair composition is prepared by a preparation method comprising the steps of:
(1) pretreating raw materials;
(2) extracting the total raw materials and deionized water according to a certain material-liquid ratio to obtain an extracting solution;
(3) filtering the extracting solution in the step (2) to obtain a crude filtrate;
(4) fine filtering the coarse filtrate obtained in the step (3) to obtain filtrate;
(5) and (5) sterilizing.
According to the invention, the weight ratio of the total weight of the raw materials to water in step (2) of the preparation method is 1:15-1:70 (m/m) (based on the dry weight of the raw materials).
According to the invention, the weight ratio of the total weight of the raw materials to water in step (2) of the preparation process may be 1:15 (m/m), 1:16 (m/m), 1:17 (m/m), 1:18 (m/m), 1:19 (m/m), 1:20 (m/m), 1:25 (m/m), 1:30 (m/m), 1:35 (m/m), 1:40 (m/m), 1:45 (m/m), 1:50 (m/m), 1:55 (m/m), 1:60 (m/m), 1:65 (m/m), 1:70 (m/m).
According to some embodiments of the invention, the weight ratio of the total weight of the starting materials to water in step (2) of the preparation process is from 1:20 to 1:50 (m/m) (based on dry weight of the starting materials).
According to the invention, the extraction temperature in step (2) of the preparation method is 100-130 ℃.
According to some embodiments of the invention, the extraction temperature in step (2) of the preparation method is 110 ℃.
According to the invention, the extraction pressure in step (2) of the preparation method is 0.1-0.3 MPa.
According to some embodiments of the invention, the extraction pressure in step (2) of the preparation process is 0.15 MPa.
According to the invention, the extraction time in step (2) of the preparation method is 1-3 h.
According to some embodiments of the invention, the extraction time in step (2) of the preparation method is 1.5 h.
According to the invention, in the step (3) of the preparation method, the filter cloth is filtered by 60-100 meshes.
According to the invention, in the preparation method, the medicine residue is filtered off by rough filtration in the step (3).
According to the invention, the fine filtration mode in the step (4) of the preparation method is plate-and-frame filtration.
According to the invention, in the step (4), the aperture of the fine filter plate frame filter plate is 0.3-0.5 μm.
According to the invention, in the step (4), the fine filter plate frame filter plate is SCP-1120 type.
According to the present invention, the sterilization mode in the step (5) of the production method is a conventional sterilization mode.
According to the invention, the sterilization mode in the step (5) of the preparation method is high-temperature sterilization.
According to some embodiments of the invention, the sterilization temperature in step (5) of the preparation method is 90-95 ℃.
According to some embodiments of the invention, the sterilization time in step (5) of the preparation method is 30-60 min.
According to some embodiments of the invention, step (5) of the preparation process further comprises adding a preservative.
According to some embodiments of the invention, the preservative added in step (5) of the preparation method is pentanediol, hexanediol.
According to some embodiments of the invention, in step (5), the pentanediol is added in an amount of 1 to 5wt% and the hexanediol is added in an amount of 0.5 to 2wt%, based on the weight of the filtrate.
According to the invention, the raw material pretreatment in the step (1) of the preparation method comprises foreign matter picking and cleaning.
In a second aspect, the present invention provides a method of preparing a soothing and repairing composition according to the first aspect of the present invention.
According to the present invention, the method of preparing the soothing servicing composition comprises the steps of:
(1) pretreating raw materials, namely weighing 5-40 parts of purslane, 1-30 parts of fructus kochiae, 5-20 parts of duckweed, 1-20 parts of honeysuckle, 3-15 parts of dark plum and 1-10 parts of schizonepeta;
(2) extracting the total raw materials and deionized water according to a material-liquid ratio of 1:15-1:70 (m/m) at an extraction temperature of 100-;
(3) filtering the extracting solution obtained in the step (2) by using 60-100 meshes of filter cloth to obtain a crude filtrate;
(4) finely filtering the coarse filtrate obtained in the step (3) by using a plate-and-frame filtration mode, wherein the aperture of a filter plate is 0.3-0.5 mu m, and obtaining filtrate;
(5) and (5) sterilizing.
According to the invention, the weight ratio of the total weight of the raw materials to water in step (2) of the preparation process may be 1:15 (m/m), 1:16 (m/m), 1:17 (m/m), 1:18 (m/m), 1:19 (m/m), 1:20 (m/m), 1:25 (m/m), 1:30 (m/m), 1:35 (m/m), 1:40 (m/m), 1:45 (m/m), 1:50 (m/m), 1:55 (m/m), 1:60 (m/m), 1:65 (m/m), 1:70 (m/m).
According to some embodiments of the invention, the weight ratio of the total weight of the starting materials to water in step (2) of the preparation process is from 1:20 to 1:50 (m/m) (based on dry weight of the starting materials).
According to some embodiments of the invention, the extraction temperature in step (2) of the preparation method is 110 ℃.
According to some embodiments of the invention, the extraction pressure in step (2) of the preparation process is 0.15 MPa.
According to some embodiments of the invention, the extraction time in step (2) of the preparation method is 1.5 h.
According to the invention, in the preparation method, the medicine residue is filtered off by rough filtration in the step (3).
According to the invention, the fine filtration mode in the step (4) of the preparation method is plate-and-frame filtration.
According to the invention, in the step (4), the fine filter plate frame filter plate is SCP-1120 type.
According to the present invention, the sterilization mode in the step (5) of the production method is a conventional sterilization mode.
According to the invention, the sterilization mode in the step (5) of the preparation method is high-temperature sterilization.
According to some embodiments of the invention, the sterilization temperature in step (5) of the preparation method is 90-95 ℃.
According to some embodiments of the invention, the sterilization time in step (5) of the preparation method is 30-60 min.
According to some embodiments of the invention, step (5) of the preparation process further comprises adding a preservative.
According to some embodiments of the invention, the preservative added in step (5) of the preparation method is pentanediol, hexanediol.
According to some embodiments of the invention, in step (5), the pentanediol is added in an amount of 1 to 5wt% and the hexanediol is added in an amount of 0.5 to 2wt%, based on the weight of the filtrate.
According to the invention, the raw material pretreatment in the step (1) of the preparation method comprises foreign matter picking and cleaning.
In a third aspect, the present invention provides the use of a soothing and repairing composition according to the first aspect of the present invention and/or a soothing and repairing composition prepared according to the method of the second aspect of the present invention in the cosmetic and/or dermatological field.
According to the invention, the skin care product is a facial mask, a cream, an emulsion, a skin lotion, a facial cleanser, a shampoo, a hair conditioner or a body wash and the like, and is not limited by dosage forms.
The invention has the advantages of
(1) The soothing and repairing composition comprises six functional components of purslane, fructus kochiae, duckweed, honeysuckle, dark plum and herba schizonepetae, has a multi-channel synergistic effect, and solves the skin problems, such as sensitive muscles, induced by various factors such as environment, regions, staying up all night, pressure, season change and the like through the effects of 'antagonistic stimulation, skin soothing, free radical removal, anti-inflammation, bacteriostasis, skin barrier repairing, skin tolerance improvement and the like'.
(2) The invention adopts a high-temperature high-pressure extraction process, improves the content of functional components such as total sugar, total flavone and polyphenol in the soothing and repairing composition, promotes the expression of the functional components, accelerates the reaction process, improves the utilization rate of raw materials and saves the production cost.
Drawings
FIG. 1 is a graph showing the results of capsaicin challenge experiments;
FIG. 2 is a graph of the assessment of scratchiness after lactic acid stimulation of example 1, example 7, comparative example 3 to comparative example 11;
FIG. 3 is a graph of the assessment of the stinging sensation after lactic acid stimulation for example 1, example 7, comparative example 3 to comparative example 11;
FIG. 4 is a graph of the assessment of the stinging sensation after lactic acid stimulation for example 1, example 7, comparative example 19 to comparative example 20;
FIG. 5 is a graph of the assessment of scratchiness after lactic acid stimulation of example 1, example 7, comparative example 19 to comparative example 20;
FIG. 6 is a graph of ABTS free radical clearance.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples, but the present invention is not limited to the examples.
The sources of the raw materials used in the present invention are shown in Table 1, and the raw materials and the apparatuses used in the present invention are conventional raw materials or apparatuses unless otherwise specified.
TABLE 1 use of raw material sources
Example 1: weighing 30g of purslane, 20g of fructus kochiae, 15g of duckweed, 10g of honeysuckle, 10g of dark plum and 5g of schizonepeta; 4500g of deionized water is added according to the feed-liquid ratio of 1:50 (m/m); extracting at 110 deg.C under 0.15MPa for 1.5 hr; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Example 2: weighing 5g of purslane, 1g of fructus kochiae, 5g of duckweed, 1g of honeysuckle, 3g of dark plum and 1g of herba schizonepetae; 1120g of deionized water is added according to the feed-liquid ratio of 1:70 (m/m); extracting at 100 deg.C under 0.1MPa for 1.5 h; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Example 3: weighing 40g of purslane, 30g of fructus kochiae, 20g of duckweed, 20g of honeysuckle, 15g of dark plum and 10g of schizonepeta; adding 2700g of deionized water according to the feed-liquid ratio of 1:20 (m/m); extracting at 130 deg.C under 0.3MPa for 1.5 hr; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Example 4: weighing 30g of purslane, 20g of fructus kochiae, 15g of duckweed, 10g of honeysuckle, 10g of dark plum and 5g of schizonepeta; adding 1800g of deionized water according to the feed-liquid ratio of 1:20 (m/m); extracting at 110 deg.C under 0.15MPa for 1.5 hr; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Example 5: weighing 30g of purslane, 20g of fructus kochiae, 15g of duckweed, 10g of honeysuckle, 10g of dark plum and 5g of schizonepeta; 4500g of deionized water is added according to the feed-liquid ratio of 1:50 (m/m); extracting at 100 deg.C under 0.1MPa for 1.5 h; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Example 6: weighing 30g of purslane, 20g of fructus kochiae, 15g of duckweed, 10g of honeysuckle, 10g of dark plum and 5g of schizonepeta; adding 1800g of deionized water according to the feed-liquid ratio of 1:20 (m/m); extracting at 130 deg.C under 0.3MPa for 1.5 hr; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Example 7: weighing 20g of purslane, 20g of fructus kochiae, 15g of duckweed, 10g of honeysuckle, 5g of dark plum and 5g of schizonepeta; 3750g of deionized water is added according to the feed-liquid ratio of 1:50 (m/m); extracting at 110 deg.C under 0.15MPa for 1.5 hr; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Comparative example 1
Weighing 30g of purslane, 20g of fructus kochiae, 15g of duckweed, 10g of honeysuckle, 10g of dark plum and 5g of herba schizonepetae, and adding 4500g of deionized water according to the material-liquid ratio of 1:50 (m/m); extracting in water bath at 80 deg.C for 1.5 h; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Comparative example 2
Weighing 30g of purslane, 20g of fructus kochiae, 15g of duckweed, 10g of honeysuckle, 10g of dark plum and 5g of herba schizonepetae, and adding 4500g of deionized water according to the material-liquid ratio of 1:50 (m/m); extracting at 150 deg.C under 0.5MPa for 1.5 h; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Comparative examples 3 to 11
Preparing extracting solutions of comparative examples 3-11 according to the raw materials and the processes of the table 2 respectively; then filtering the extract once by using 100-mesh filter cloth, and then filtering by using a filter plate with the diameter of 0.3-0.5 mu m; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
Table 2 comparative examples 3 to 11 raw material composition ratios and preparation processes
Comparative examples 12 to 17
Preparing extracting solutions of comparative examples 12 to 17 according to the raw materials and the processes of the table 3 respectively; then filtering the extract once by using 100-mesh filter cloth, and then filtering by using a filter plate with the diameter of 0.3-0.5 mu m; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain the composition.
TABLE 3 raw material composition ratios and preparation processes for comparative examples 12 to 17
Comparative example 18
According to comparative example 12: comparative example 13: comparative example 14: comparative example 15: comparative example 16: comparative example 17 extract = 6: 4: 4: 2: 2: 1 taking 4500g of the extract, and mixing and stirring uniformly to obtain a mixed solution.
Comparative example 19
Weighing 1g of purslane, 1g of fructus kochiae, 1g of duckweed, 20g of honeysuckle, 20g of dark plum and 20g of schizonepeta, and adding 3150g of deionized water according to the material-liquid ratio of 1:50 (m/m); extracting at 110 deg.C under 0.15MPa for 1.5 hr; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain extract.
Comparative example 20
Weighing 5g of purslane, 5g of fructus kochiae, 5g of duckweed, 5g of honeysuckle, 20g of dark plum and 20g of herba schizonepetae, and adding 3000g of deionized water according to a material-liquid ratio of 1:50 (m/m); extracting at 110 deg.C under 0.15MPa for 1.5 hr; filtering the extractive solution with 100 mesh filter cloth, and filtering with 0.3-0.5 μm filter plate; adding 2% pentanediol and 1.5% hexanediol for antisepsis, and sterilizing in water bath at 90-95 deg.C for 30min to obtain extract.
Test example 1: basic index test of plant composition by different preparation processes
1.1 measurement of polysaccharide and Total sugar content
The method is carried out by adopting a phenol-sulfuric acid method (specifically referring to the content determination of polysaccharide in tremella [ J ]. Heilongjiang pharmaceutical science, 1999(06): 32-32.).
The value: measured using a pH meter.
Solid content: measured by a solid content instrument.
In order to prevent the influence of concentration multiple error on the content of effective components of the extract, all indexes are measured to be filtrate before concentration.
TABLE 4 basic indices of the plant compositions for the different preparation processes
When the formula composition is prepared by a water extraction method, some light medicinal materials are found to float on the surface of the liquid, and the problem cannot be solved even if the medicinal materials are stirred, so that the medicinal materials are easy to react insufficiently, and the extraction efficiency is greatly reduced. The high temperature and high pressure method is a method for extracting active ingredients under a closed condition with higher pressure intensity, the extraction method can accelerate reaction during reaction, and meanwhile, the closed condition can ensure that water vapor can fully contact each medicinal material, so that the reaction efficiency is improved. As can be seen from Table 4, the high temperature and high pressure treatment improves the total sugar content, total flavone content and polyphenol content of the composition, avoids resource waste caused by insufficient utilization of raw materials, and greatly saves cost, compared with the common water extraction method. Meanwhile, by comparing examples 1, 5-6 and 2, it can be seen that when the temperature and pressure of the high-temperature high-pressure treatment exceed a certain range, the higher temperature and pressure basically do not improve the extraction efficiency of the plants, but the too high pressure not only brings about a potential safety hazard, but also increases energy consumption and causes energy waste. In conclusion, the high-temperature and high-pressure extraction conditions of the invention are that the extraction pressure is 0.1-0.3MPa and the extraction temperature is 100-130 ℃.
TABLE 5 basic indices of extracts of single and combined materials
| pH value | Solids content/% | Color of solution | |
| Example 1 (high temperature and high pressure method) | 4.98 | 2.8 | Dark brown color |
| COMPARATIVE EXAMPLE 12 (purslane) | 5.85 | 1.2 | Earthy yellow |
| COMPARATIVE EXAMPLE 13 (Kochia scoparia) | 5.81 | 1.0 | Brown colour |
| COMPARATIVE EXAMPLE 14 (Duckweed) | 6.10 | 1.0 | Dark brown color |
| COMPARATIVE EXAMPLE 15 (honeysuckle) | 5.29 | 1.6 | Yellow colour |
| COMPARATIVE EXAMPLE 16 (smoked plum) | 2.62 | 1.6 | Brown colour |
| COMPARATIVE EXAMPLE 17 (Schizonepeta tenuifolia) | 5.63 | 0.4 | Light yellow |
| Comparative example 18 (Mixed solution) | 5.21 | 1.3 | Dark brown color |
The traditional Chinese medicine is decocted into two types of single decoction and multiple decoction, wherein the multiple decoction is to simultaneously put all the medicinal materials in a pot for boiling, and the single decoction is to respectively boil each medicinal material and then mix the decoction. To verify the effect of single and multiple simmering on the efficacy of the formula, the data of the relevant indices of example 1 and comparative examples 12-17 were tested and the results are shown in table 5. Compared with the comparative example 18, the solution in the example 1 has similar color and higher solid content, which indicates that certain weak interaction occurs between the medicinal materials during repeated decoction, generates a supermolecule chemical phenomenon and promotes the functional components to be dissolved in the extracting solution. Because the pH value (2.62) of the dark plum extract is too low, the dark plum extract is easy to generate stimulation to skin, and the dark plum extract is abandoned in later experiments.
Capsaicin test
Test samples: example 1, comparative examples 12 to 18
Testing parts: the inner sides of the left and right arms;
selecting the inner sides of the left and right arms of a subject as tested parts, and circularly marking the tested parts in a square area with the specification of 2cm multiplied by 2 cm; washing a tested area (the same area) with clear water, standing the tested area for 10min at the temperature of 20.6-21.2 ℃ and the relative humidity of 43-52%, measuring a blank value of a skin red value by using a Mexamter MX18 (a pigment test probe) of Germany CK company, and then entering a smearing experiment stage; stimulating the tested area with 0.02% capsaicin aqueous solution (about 0.01 mL); continuously stimulating for 15min and 30min, and collecting numerical values; then smearing a test sample (5 wt% solution, about 0.05 mL) on the tested area for 15min, 30min and 45min, and then performing data acquisition; smearing 0.05mL of pure water on the blank control; coating 0.2wt% of Symcalmin Dermax aqueous solution on the positive control group; counting the value measured at each time of the experimental part of the subject, and analyzing the change of the red value.
The change of the skin red value is reflected in the change rule of the skin redness of the experimental area along with the time in the testing period. The greater the value, the greater the degree of redness of the skin. Skin red change rate (%) = (T-T blank)/T blank × 100%.
As can be seen from fig. 1, example 1 has a remarkable effect of repairing skin after stimulation, and can rapidly reduce the redness of skin due to stimulation and repair damaged skin. Comparative example 18 (mixed solution) and comparative example 15 (honeysuckle flower) have certain repairing effect, but the repairing effect is not as good as that of example 1. This is because during the re-decoction process, some weak interaction between the herbs can occur, which can generate supermolecule chemical phenomena to promote the efficacy of the active ingredients.
Test example 2: comparison of efficacy of extracts of formulas at different ratios
Test samples: example 1, example 7, comparative examples 3-11 and comparative examples 19-20, samples were diluted to 5% aqueous solutions.
Testing the population: 120 (18-55 years old, male and female unlimited) volunteers were selected and divided into 12 groups. 10 people per group.
The lactic acid stimulation method was carried out by applying filter paper (about 0.8cm in diameter) soaked with 50. mu.L of 10% lactic acid solution to the nasolabial folds of both sides of the volunteers for 10min and removing the filter paper. A tester coats samples on test areas on two sides simultaneously, the two samples in the same group are randomly distributed on the two sides, the sample coating amount of each area is 0.1mL, before and after the samples are used, the samples are 0min, 0.5min, 2min, 5min, 10min and 15min, and the itching feeling and the stinging feeling at the positions of nasolabial folds on the two sides are subjectively evaluated by volunteers (the total score is 5, the higher the score of the itching feeling and the stabbing feeling is, the score of 0-1 represents no feeling or a little feeling, the score of 1-3 represents slight stimulation, the itching feeling and the stabbing feeling can be felt, the score of 3-5 represents severe stimulation, and the itching feeling and the stabbing feeling are severe). The test samples were evaluated for immediate tingling and itching relief using sensory evaluation of volunteers, with experimental results as shown in fig. 2-5.
As can be seen from fig. 2 to 3, the examples and comparative examples each had the effect of instantly relieving itching and stinging after using the samples. The instant itching and stinging relieving effect of the soothing and repairing composition prepared by combining any five or three raw materials in the compositions in the comparative examples 3-11 is obviously better than the instant itching and stinging relieving effect of the soothing and repairing composition prepared by combining any five or three raw materials in the compositions in the comparative examples 1-11, which shows that the six components of the composition have a synergistic effect, and if one raw material or a plurality of raw materials are removed, the effect of the soothing and repairing composition is greatly reduced.
From FIGS. 4 to 5, however, example 1 had better immediate relief of itching and stinging than comparative examples 19 to 20, indicating that the ratio of the ingredients in the formula may have a different effect on the effect. The embodiment of the invention is the optimal component proportion obtained by multiple experimental screening, because the intermediate experimental process is too much and cannot be put on one by one, and the lists are typical embodiments and comparative examples.
In conclusion, the composition formula, the proportion and the preparation process influence the effect expression of the composition, and six effect components of purslane, fructus kochiae, honeysuckle, duckweed, dark plum and schizonepeta in the composition have synergistic effect through multiple channels, so that unexpected technical effects are generated.
Test example 3: efficacy verification
3.1 scavenging of free radicals
Test samples: example 1, comparative example 8, comparative example 9, comparative example 20.
The experimental method comprises the following steps: the experimental method for scavenging free radicals is as follows: preparation is 7 mmol.L-1ABTS stock solution and 140 mmol. L-1Potassium persulfate stock solution. A certain amount of 7 mmol. multidot.L-1ABTS and 140 mmol. L-1Mixing potassium persulfate, and standing at room temperature in a dark place for a period of time to form ABTS free radical stock solution. A certain amount of ABTS free radical stock solution is taken and diluted by 50% ethanol, so that the light absorption value of the final test negative control is 0.70 +/-0.02.
Free radicals are a very active class of reactive molecular species (often called oxygen radicals because most of them contain free oxygen atoms, unless otherwise specified, free radicals are oxygen radicals) which are products of human metabolism and can also be increased by environmental factors such as pollution, uv light and sunlight. Harmfulness of free radicals to the human body: 1. the electrons of the cell membrane are easily lost, so the cell membrane is extremely vulnerable to free radicals, and once the electrons are deprived by the free radicals, the cell membrane loses elasticity and loses part or all functions, thereby causing cardiovascular diseases (the free radicals are generally considered to be the root cause of all diseases and aging). More serious, the attack of free radicals to genes can damage the molecular structure of the genes and cause gene mutation, thereby causing systematic disorder of the whole life; 2. bad cholesterol in the human body is easily oxidized by free radicals, and after oxidation, foam cells are formed, and the foam cells are attached to the blood vessel wall. After a certain amount of time has elapsed, the blood vessel is blocked or broken into fragments and the fragments are introduced into the blood, and the blood is coagulated to form thrombus when contacting the fragments. Thrombosis can cause vessel occlusion, coronary heart disease if it occurs in the coronary arteries supplying the heart's blood, and stroke if it occurs in the brain. That is, the chief culprit in atherosclerosis is the oxidation of these free radicals by bad cholesterol; 3. free radicals act on the enzymatic system in the human body, resulting in the release of collagenase and scleroelastase, which act on collagen and scleroelastin in the skin and cause them to undergo excessive cross-linking and degradation, with consequent loss of elasticity and appearance of wrinkles.
The soothing and repairing composition of the invention has good effect of scavenging free radicals, as shown in fig. 6, the concentration of the extract of example 1 is 0.5% and 2.0%, and the scavenging rate of the extract on free radicals can reach 100%. The clearance rate of the soothing and repairing composition of example 1 of the invention on free radicals is higher than that of the soothing and repairing composition obtained in comparative example 8, comparative example 9 and comparative example 20, which shows that the combination of six effective components of purslane, fructus kochiae, honeysuckle, duckweed, dark plum and herba schizonepetae of the invention produces obvious synergistic interaction, and different components promote each other, thus having better effect of clearing free radicals.
Repairing barrier and relieving swelling
The experimental method comprises the following steps: 100 skin itch, red swelling, dry desquamation volunteers were recruited and divided into 4 groups of 25 persons, and after normal skin cleaning and caring, the test samples of example 1, comparative example 8, comparative example 9, and comparative example 20 (all 5% aqueous solution) were applied for 7 days.
Table 6 example 1 the composition improves skin effects
| Improving skin itch | Improving skin redness and swelling | Improving dry skin desquamation | |
| Use for 15 minutes | 24/25 human, 96% | 2/25 human, 8% | 1/25 human, 4% |
| It can be used for 1-3 |
25/25 human, 100% | 20/25 human, 80% | 18/25 human, 72% |
| It is used for 7 |
25/25 human, 100% | 25/25 human, 100% | 25/25 human, 100% |
Table 7 skin improvement effect of comparative example 8 composition
| Improving skin itch | Improving skin redness and swelling | Improving dry skin desquamation | |
| Use for 15 |
5/25 human, 20% | 0/25 human, 0% | 2/25 human, 20% |
| It can be used for 1-3 days | 12/25 human, 48% | 3/25 human, 12% | 10/25 human, 40% |
| It is used for 7 days | 21/25 human, 84% | 7/25 human, 28% | 20/25 human, 80% |
Table 8 skin improving effect of comparative example 9 composition
| Improving skin itch | Improving skin redness and swelling | Improving dry skin desquamation | |
| Use for 15 |
3/25 human, 12% | 0/25 human, 0% | 2/25 human, 8% |
| It can be used for 1-3 |
5/25 human, 20% | 2/25 human, 8% | 5/25 human, 20% |
| It is used for 7 days | 12/25 human, 48% | 8/25 human, 32% | 13/25 human, 52% |
TABLE 9 skin improvement effect of comparative example 20 composition
| Improving skin itch | Improving skin redness and swelling | Improving dry skin desquamation | |
| Use for 15 minutes | 13/25 human, 52% | 0/25 human, 0% | 3/25 human, 20% |
| It can be used for 1-3 days | 18/25 human, 72% | 4/25 human, 16% | 9/25 human, 36% |
| It is used for 7 |
20/25 human, 80% | 11/25 human, 44% | 14/25 human, 56% |
The volunteers can improve the skin pruritus feeling by applying the paint in example 1 for 15min, and the skin pruritus feeling is up to 96%, while the effect of the comparative example is obviously lower, and the highest improvement rate is only 52%. After 1-3 days of use, most of the volunteers of example 1 improved the redness and swelling of the skin up to 80%, while the comparative examples did not improve the effect by more than 16%. The dry skin peeling phenomenon of 75% of volunteers was improved after 1 to 3 days using example 1, while the improvement effect of the comparative example was not more than 40%. The symptoms of itching, redness and swelling, and dry desquamation of the skin of 100% of volunteers 7 days after using example 1 can be improved, while the improvement effect of the comparative example is obviously inferior to that of example 1. And the volunteer feedback of example 1 was used, and then the skin allergy phenomenon was reduced and the feeling was not so stimulated when other products were used, which also indicates that the formulation has a good barrier repair effect. While the other groups used volunteers of the comparative example, no feedback was given to the improvement of the skin barrier function. According to the invention, six functional components of purslane, fructus kochiae, honeysuckle, duckweed, dark plum and herba schizonepetae are combined to generate an obvious synergistic effect, so that the skin itching, redness and swelling, dryness and desquamation symptoms can be better relieved, and the skin barrier repairing effect is achieved.
In order to better verify other effects of the formula, the anti-inflammatory and antibacterial effect detection is further carried out on the soothing and repairing composition.
Anti-inflammatory assay
Lipopolysaccharide (LPS) is adopted for induction, an action object is RAW264.7, general body inflammation is simulated, and a tested inflammatory factor is IL-1 beta. IL-1 beta plays an important role in immune regulation and inflammatory reaction processes, is considered to be one of main endogenous mediators causing fever reaction in the inflammatory reaction process, and once the content of inflammatory factors in skin cells is increased and the skin temperature is higher than normal temperature, the skin inflammatory reaction is aggravated and the body inflammatory cascade reaction is initiated.
Test samples: example 1, comparative example 8, comparative example 20;
the experimental method comprises the following steps: anti-inflammatory assays were performed using LPS-induced RAW264.7 cell inflammation model:
(1) inoculation: cells were seeded into 24-well plates at 37 ℃ with 5% CO2The incubator is incubated for 18-24 h.
(2) Preparing liquid: the test substances and positive controls were formulated according to table 10.
(3) Sample feeding: grouping and concentration setting were tested according to table 10, and samples were given in groups of 3 replicate wells per treatment group after 18-24h of cell plating growth in 24-well plates. In group 1, cell culture medium containing 0.1% DMSO was added to both blank and negative controls, and cell culture medium containing 0.001% dexamethasone was added to the positive control; in group 2, the blank control and the negative control were added with cell culture medium, and the sample group was added with cell culture medium containing samples at corresponding concentrations at 37 ℃ with 5% CO2The incubator continues to culture for 18-24 h.
Table 10 experimental groupings and concentration settings
(4) And (3) LPS induction: after culturing for 24h, sucking out the culture medium in the plate, adding PBS for light washing once, adding cell culture medium into a blank control group, adding cell culture medium containing LPS into a negative control group, a sample group and a positive control group, and culturing at 37 ℃ with 5% CO2The incubator continues to culture for 24h and then collects the supernatant.
(5) Detecting the content of IL-1 beta: cell supernatants from each well were taken and assayed for the content of the cytokine IL-1. beta. according to the ELISA kit protocol, the results are shown in Table 11.
TABLE 11 detection of inflammatory factor IL-1. beta. expression
LPS induction (LPS +) caused a significant increase in the expression of the inflammatory factor IL-1 β compared to the BC (LPS-) group: (P<0.01), indicating that LPS induces molding success; compared with SC (0.1% DMSO, LPS +), dexamethasone in the PC (dexamethasone) group can significantly reduce the expression quantity of IL-1 beta at the administration concentration of 0.001%P<0.01), which indicates that the detection result is valid.
The effect of the detection result of the expression of the inflammatory factor IL-1 beta of the soothing and repairing composition is shown in Table 11, and compared with the NC (LPS +) group, the soothing and repairing composition has significant inhibition effect on the expression of the inflammatory factor IL-1 beta within the concentration ranges of 0.08%, 0.16% and 0.31%; at a concentration of 0.08%, the soothing and repairing composition of the invention has a significant inhibitory effect on the expression of the inflammatory factor IL-1 β, compared to comparative example 8 and comparative example 20.
Bacteriostatic effect
The antibacterial effect of the soothing repairing composition is detected according to the evaluation method of the antibacterial and bacteriostatic effects of QB/T2738-.
TABLE 12 bacteriostatic effect of soothing and repairing compositions of the present invention
As shown in table 12, the soothing and repairing composition of the present invention has a good bacteriostatic effect against staphylococcus epidermidis and staphylococcus aureus.
Safety feature
In order to ensure the safety of the formula, a chick embryo chorioallantoic membrane test and a rabbit corneal epithelial cell in-vitro short-time exposure test are carried out, and the test result shows that the chick embryo chorioallantoic membrane test has no irritation. The result of the erythrocyte hemolytic blood coagulation test shows that the blood coagulation phenomenon does not occur.
In conclusion, the soothing and repairing composition comprises six functional components of purslane, fructus kochiae, duckweed, honeysuckle, dark plum and herba schizonepetae, has a multi-channel synergistic effect, and solves the skin problems, such as sensitive muscles, induced by various factors such as environment, regions, night-out, pressure and season change through the effects of 'antagonistic stimulation, skin soothing, free radical removal, anti-inflammation, bacteriostasis, skin barrier repairing, skin tolerance improvement and the like'. In terms of safety, has very reliable safety, and can be safely applied to the field of cosmetics.
The above examples are given for the purpose of illustrating the invention clearly and not for the purpose of limiting the same, and it will be apparent to those skilled in the art that, in light of the foregoing description, numerous modifications and variations can be made in the form and details of the embodiments of the invention described herein, and it is not intended to be exhaustive or to limit the invention to the precise forms disclosed.
Claims (9)
1. The soothing and repairing composition is characterized by comprising the following components in parts by weight: 5-40 parts of purslane, 1-30 parts of fructus kochiae, 5-20 parts of duckweed, 1-20 parts of honeysuckle, 3-15 parts of dark plum and 1-10 parts of schizonepeta.
2. A soothing servicing composition according to claim 1, wherein the soothing servicing composition is prepared by a preparation process comprising the steps of:
(1) pretreating raw materials;
(2) extracting the total raw materials and deionized water according to a certain material-liquid ratio to obtain an extracting solution;
(3) filtering the extracting solution in the step (2) to obtain a crude filtrate;
(4) fine filtering the coarse filtrate obtained in the step (3) to obtain filtrate;
(5) and (5) sterilizing.
3. A soothing servicing composition according to claim 2, characterized in that the weight ratio of the total weight of the raw materials to water in step (2) of the preparation process is 1:15-1:70 (m/m) (based on dry weight of the raw materials).
4. A soothing servicing composition according to claim 2, characterized in that the extraction temperature in step (2) of the preparation process is 100-.
5. A soothing servicing composition according to claim 2, characterized in that the filtration cloth in step (3) of the preparation method is 60-100 mesh.
6. A soothing and repairing composition as claimed in claim 2, wherein the fine filtration mode in step (4) of the preparation method is plate and frame filtration, and/or the pore size of the filter plate is 0.3-0.5 μm.
7. A method of preparing a soothing and repairing composition, comprising the steps of:
(1) pretreating raw materials, namely weighing 5-40 parts of purslane, 1-30 parts of fructus kochiae, 5-20 parts of duckweed, 1-20 parts of honeysuckle, 3-15 parts of dark plum and 1-10 parts of schizonepeta;
(2) extracting the total raw materials and deionized water according to a material-liquid ratio of 1:15-1:70 (m/m) at an extraction temperature of 100-;
(3) filtering the extracting solution in the step (2) by using 60-100 meshes of filter cloth to obtain crude filtrate;
(4) finely filtering the coarse filtrate obtained in the step (3) by using a plate-and-frame filtration mode, wherein the aperture of a filter plate is 0.2-10 mu m, and obtaining filtrate;
(5) and (5) sterilizing.
8. Use of a soothing repairing composition according to any of claims 1 to 6 or a soothing repairing composition prepared according to the process for preparing a soothing repairing composition according to claim 7 in the field of cosmetics and/or skin care.
9. Use according to claim 8, characterized in that the soothing and repairing composition is used for preparing cosmetics and/or skin care products with the effects of soothing skin, scavenging free radicals, resisting inflammation, improving skin tolerance and repairing skin barrier.
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| CN202110305740.6A CN113181089B (en) | 2021-03-23 | 2021-03-23 | Soothing and repairing composition and preparation method and application thereof |
| PCT/CN2022/081927 WO2022199510A1 (en) | 2021-03-23 | 2022-03-21 | Alleviating and repairing composition, and preparation method therefor and use thereof |
| KR1020237034944A KR102700722B1 (en) | 2021-03-23 | 2022-03-21 | Composition for relaxation and recovery and its preparation method and application |
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| CN113318166A (en) * | 2021-06-30 | 2021-08-31 | 植然天成(北京)生物科技有限公司 | Plant composition and preparation method and application thereof |
| CN114533612A (en) * | 2022-02-17 | 2022-05-27 | 广东芭薇生物科技股份有限公司 | Composition with effects of relieving, removing red and repairing and application thereof |
| WO2022199510A1 (en) * | 2021-03-23 | 2022-09-29 | 太和康美(北京)中医研究院有限公司 | Alleviating and repairing composition, and preparation method therefor and use thereof |
| WO2022252761A1 (en) * | 2021-05-31 | 2022-12-08 | 植然天成(北京)生物科技有限公司 | Soothing repair cream and preparation method therefor |
| CN116270350A (en) * | 2023-03-24 | 2023-06-23 | 北京工商大学 | Flower composition and preparation method and application thereof |
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| CN113181089B (en) | 2022-10-11 |
| KR20230149856A (en) | 2023-10-27 |
| KR102700722B1 (en) | 2024-08-29 |
| WO2022199510A1 (en) | 2022-09-29 |
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