CN109512732B

CN109512732B - External plant extract and cosmetic with skin barrier repairing effect and preparation method thereof

Info

Publication number: CN109512732B
Application number: CN201711194842.5A
Authority: CN
Inventors: 董银卯; 孟宏; 刘宇红; 曲召辉
Original assignee: Nutri Woods Bio Tech Beijing Co ltd
Current assignee: Nutri Woods Bio Tech Beijing Co ltd
Priority date: 2017-11-24
Filing date: 2017-11-24
Publication date: 2021-03-30
Anticipated expiration: 2037-11-24
Also published as: CN109512732A

Abstract

The invention discloses an external plant extract with the effect of repairing skin barriers. The external plant extract is prepared from the following raw materials in parts by weight by the following method: (1) weighing the raw materials according to the following weight part ratio, and mixing uniformly; 1-10 parts of safflower carthamus, 1-10 parts of gardenia, 1-10 parts of Hangzhou white chrysanthemum and 1-10 parts of prunus mume; (2) extracting for the first time: according to the material-liquid ratio of 1: mixing the raw material and the solvent I at the temperature of 10-100 m/m, and extracting for 0.5-2 h at the temperature of 40-90 ℃; (3) and (3) second extraction: according to the material-liquid ratio of 1: adding a second solvent at the speed of 10-100 m/m, and extracting for 0.5-2 h at the temperature of 40-90 ℃; (4) removing the first solvent; (5) fine filtering to obtain clear extract; the first solvent is one or a mixture of ethanol, chloroform and acetone; the second solvent is one or more of white oil, hydrogenated polyisobutene, hydrogenated polydecene, caprylic/capric triglyceride, isostearyl isostearate and vegetable oil.

Description

External plant extract and cosmetic with skin barrier repairing effect and preparation method thereof

Technical Field

The invention relates to an external plant extract, in particular to an external plant extract with the effect of repairing skin barriers, an efficient preparation method and cosmetics prepared from the plant extract.

Background

The skin covers the surface of the human body and is the first line of defense of the human body. Healthy skin has two barrier effects: (1) resist the entry of external mechanical, physical, chemical and biological harmful substances, irritants and the like, and protect all important internal organs in the body; (2) preventing loss of nutrients and water in body, maintaining water content of skin, and moistening skin.

However, when the skin is stimulated by sunlight, ultraviolet radiation or cosmetics, drugs (such as hormones, etc.) and other factors, the skin barrier is damaged, so that the skin's self-defense ability is insufficient, thereby causing problems such as impaired epidermal barrier function, telangiectasia, thinning of inflammatory skin, flushing of the face, pigmentation, etc.

At present, the main method for repairing the skin barrier function is to adopt a humectant, the skin moisturizer mainly comprises an oil blocking humectant, a hydrophilic matrix hygroscopic humectant, a hydration humectant and the like, but the simple moisturizing cannot fundamentally solve the repairing problem of the damaged skin barrier function after being damaged.

Plant extracts have many advantages as cosmetic additives, such as natural components, low irritation, excellent efficacy, etc., and thus, the use of plant extracts as efficacy additives in cosmetics is increasing. The effective components of the plant material include oil-soluble components such as fatty acid, sterol, lignan, esters, polyene, pyrrole derivatives, ketones, quinones, etc., and some non-oil-soluble substances such as saccharides, amino acids, proteins, etc. The current main reasons for the application of plant extracts in the cosmetic field are (1) too low extraction efficiency, and the increase of extraction cost is caused by too low extraction effect due to the characteristics of plant raw materials, so that many enterprises preferentially select low-cost synthetic chemical raw materials to replace natural plant raw materials so as to increase economic benefit. (2) The stability of the plant material extract is poor. Plant raw materials are often not good in stability in various dosage forms of the added and evolved cosmetics, and are easy to deteriorate, separate out or precipitate in the storage and transportation processes, so that the product spoilage is increased, the cost is increased, the effect is directly influenced, and the use experience of consumers is reduced. In particular, for oil type cosmetics, the oil type cosmetics have extremely high requirements on clarity, and once slight precipitation and precipitation occur, the quality and the performance of the product can be influenced. Therefore, a plant extract preparation process which is suitable for industrial production and has high extraction rate and good extract stability is urgently needed by cosmetic enterprises at present.

The extraction method of the functional components of the existing plant raw materials is introduced as follows, and the existing preparation process comprises the following steps:

1. soaking and extracting

The flower and plant soaking oil has a long history of application, and ancient Egyptics and ancient Hispanics have learned to absorb the odor of petals and herbs with oil and fat for use as medicines or cosmetics. The soaking oil is usually vegetable oil as a solvent, and the ratio of the raw materials to the oil is about 1: 3(v/v), soaking at normal temperature, repeatedly feeding for 2-3 times, and soaking for 1-3 months. The soaking oil has good compatibility when used in cosmetic oil dosage forms, but the method has low extraction efficiency and long extraction time, and is not beneficial to industrial production.

2. Direct high-temperature extraction of oil

Ancient books such as Puji prescription and Taiping Shenghui prescription record a lot of ointments, which are prepared by frying Chinese herbs with oil and fat to remove dregs, and are used for treating skin diseases or beautifying. Until now, folk still keep many prescriptions and proved prescriptions, and sesame oil is heated and decocted in the traditional Chinese medicine to obtain medicinal oil for relieving various uncomfortable symptoms of skin. Therefore, direct high-temperature decoction by using oil is one of the traditional extraction methods, but the method is more original, has low extraction efficiency, can not effectively extract active ingredients in plants, has long time consumption, serious material waste, low extraction efficiency and the like, and seriously restricts industrial production.

3. Steam distillation process

Steam distillation is a common method for extracting plant essential oil, but the method is only suitable for extracting volatile components of aromatic substances in plants, and the nonvolatile components cannot be extracted and utilized.

4. Solvent extraction

Solvent extraction is a common method for producing plant extracts, generally takes ethanol, acetone, chloroform and the like as solvents, and has the characteristics of simple equipment, high extraction rate and the like. However, the extract prepared by the method has higher requirements on the formulation of cosmetics, is not suitable for being added into all formulations, and particularly has poor solubility in oil-type cosmetics, so that the plant extract can be precipitated after being added into the pure oil-type cosmetics, the product quality is seriously influenced, and the application of the plant extract in the pure oil-type cosmetics is restricted.

5. Supercritical extraction

Supercritical extraction is a new technique which has been developed in recent years, and the solvent is extracted by supercritical extractionFluid, typically supercritical CO²Has the advantages of no toxicity, no harm, high extraction rate, high extract purity and the like. But the equipment is complex, the input cost is high, the extraction cost is high, and the industrialized mass production is limited. And the compatibility of the extract obtained by supercritical extraction with oil is poor, so that the application of the extract in oil type cosmetics is influenced.

The existing method has a plurality of defects, and simultaneously, the problems of high preparation cost, environmental pollution caused by organic solvent discharge and the like are gradually highlighted due to the limitation of extraction efficiency. Therefore, there is a great need in the art to solve the above-mentioned problems in the preparation of plant extracts for the addition of cosmetic and care products.

Disclosure of Invention

The invention aims to provide a plant composition with the effect of repairing skin barriers, a preparation method thereof and an obtained plant extract.

The second purpose of the invention is to provide a preparation method of the plant extract with high extraction rate and stable extract property.

The third purpose of the invention is to propose a cosmetic prepared from the plant extract.

The invention idea is as follows: the composition selected by the invention utilizes the composing principle of 'monarch, minister, assistant and guide' to mix the four plant raw materials, the raw materials act synergistically, and the novel preparation method can play a role in repairing skin barriers and improving skin tolerance.

In order to realize the purpose of the invention, the invention adopts the following technical scheme:

an external plant extract with the effect of repairing skin barriers is prepared from the following raw materials in parts by weight by the following method:

(1) weighing the raw materials according to the following weight part ratio, and mixing uniformly;

1-10 parts of safflower carthamus, 1-10 parts of gardenia, 1-10 parts of Hangzhou white chrysanthemum and 1-10 parts of prunus mume;

(2) extracting for the first time: according to the material-liquid ratio of 1: mixing the raw material and the solvent I at the temperature of 10-100 m/m, and extracting for 0.5-2 h at the temperature of 40-90 ℃;

the first solvent used in the invention is one or a mixture of ethanol, chloroform and acetone.

The feed-liquid ratio and the extraction temperature have a crucial influence on the extraction efficiency and the extraction cost, and the feed-liquid ratio and the extraction parameters which are more matched with the physicochemical properties of the first extraction solvent can be selected according to the physicochemical properties of the first extraction solvent, so that the extraction efficiency can be improved, and the cooperativity with the next extraction solvent can be enhanced. The plant raw material and the solvent are contacted more fully in the feed liquid ratio range, the active ingredients in the plant raw material are easier to extract, the extraction efficiency is higher, meanwhile, the waste of the solvent and the plant raw material is not caused, and the extraction cost is more economic. The preferable range value of the ratio of the first extraction material to the liquid is 1: 10-50 m/m, better extraction effect in the range, and stronger synergy with the solvent II.

The extraction temperature and the extraction time are preferably 40-90 ℃ for 0.5-2 h. The extraction temperature and time directly influence the property of the extract, and improper extraction temperature and time can cause oxidative denaturation of plant raw materials, loss of volatile components, change of the property of thermosensitive components and the like in the extraction process, so that the solubility and the material exchange rate of the effective components of the extract in a solvent are optimal, and the effect of the extract is excellent and stable.

The condition parameters of the step (2) are more suitable for matching the step (3) and can generate synergistic effect with the step (3).

(3) And (3) second extraction: according to the material-liquid ratio of 1: adding a second solvent at the speed of 10-100 m/m, and extracting for 0.5-2 h at the temperature of 40-90 ℃;

the second solvent used in the invention is one or a mixture of more of the following raw materials: white oil with kinematic viscosity (40 ℃) less than or equal to 30cSt, and white oils 3#, 5#, 7#, 10#, 15#, and 26# are recommended; hydrogenated polyisobutene having a kinematic viscosity (40 ℃) of less than or equal to 30cSt, preferably hydrogenated polyisobutene Parleam 6, Parleam EX; hydrogenated polydecene with a kinematic viscosity (40 ℃) of less than or equal to 30cSt, preferably PAO2, PAO4 and PAO 6; caprylic/capric triglyceride, isostearyl isostearate and vegetable oil. The vegetable oil is preferably soybean oil, sunflower seed oil, sesame oil, macadamia nut oil, sweet almond oil, olive oil, grape seed oil, oat oil, or tea oil.

The combination of the second solvent and the first solvent is particularly important for the technical effect of the invention, and the inventor verifies through experiments that the two solvents cannot be completely dissolved with each other, and the complete dissolution can ensure better extraction efficiency, but the added product has poor stability and is easy to have adverse conditions such as precipitation and the like. The two solvents cannot be completely immiscible, and the immiscible solvents cannot play a role in synergy, so that the extraction efficiency is very low and the stability of the extract is poor. Therefore, the mutual dissolution technical effect of the first solvent and the second solvent is optimal, in order to ensure that the extraction cost is more economic due to the higher extraction efficiency of the two solvents, the temperature and the time of the second extraction are controlled within the condition parameter range, the extraction effect of the mutual dissolution and the common extraction of the first solvent and the second solvent can be simultaneously improved, and the problems that the extraction efficiency tends to slowly increase the extraction cost and the like can be effectively avoided. According to the characteristics of the second solvent, the extraction temperature is not suitable to be too high, is optimally controlled below 90 ℃, is not too low, and is lower than 40 ℃, so that the solubility of the functional components in the second solvent and the compatibility of the first solvent and the second solvent are influenced, and the extraction efficiency is further influenced.

According to the description of the method, the selection of the solvent I and the solvent II is particularly important, the combination of the solvent I and the solvent II needs to be synergistic to improve the extraction efficiency of the plant raw materials, in order to adapt to industrial production, the extraction process needs to be short, the quality of the extract needs to be high, namely the addition stability is good, and the extraction cost also needs to be low. Therefore, the inventor of the present invention has experimentally verified that if the polarity of the solvent of the present invention is greater than that of the solvent one, the extraction efficiency and the stability of the extract are poor. The inventor surprisingly found that if the solvent is more polar than the solvent II, the first solvent and the second solvent can be partially dissolved with each other under certain conditions, which can enhance the solubility of the active ingredient in the second solvent, so that some substances which are originally insoluble in the oil or have poor solubility in the oil can be well dissolved in the second solvent. The two extracts are combined for extraction, so that all conditions required by the extraction of the plant raw materials of the cosmetics can be met, the extraction efficiency of the plant active ingredients is greatly improved, the obtained extract has stable property and excellent compatibility with other raw materials of the cosmetics.

In the invention, one of the solvents can be selected for single solvent extraction, or multiple solvents can be compounded and extracted according to the characteristics of the plant raw materials which are actually extracted, and the compounding ratio among the solvents can be compounded according to the experience of a person skilled in the art or the actual needs in any ratio without specific limitation. Because the second solvent is characterized by the great influence of water on the stability of the second solvent, the first solvent is preferably an anhydrous system, such as ethanol, and is preferably anhydrous ethanol.

The solvent II is an extraction solvent with weaker polarity than the solvent I, is mild and non-irritant, and has good compatibility with functional components in plant raw materials. The second solvent can be one of the solvents mentioned above for single solvent extraction, or can be a multi-solvent compound extraction according to the characteristics of the plant raw material actually extracted, and the compounding ratio between the solvents can be any ratio according to the experience of the person skilled in the art or the actual needs, and is not particularly limited.

In the step (3), the preferable range of the ratio of the second extraction material to the liquid is 1:10 to 50 m/m.

(4) Removing the first solvent; the methods for removing the solvent known to those skilled in the art can be applied herein, and the preferred methods proposed in the present invention are: concentrating under reduced pressure at 40-80 deg.C until the solvent is completely removed, wherein the reduced pressure range is generally controlled to 0.01MPa to minus 0.15 MPa. The first solvent may have certain irritation to skin, and the removal of the first solvent can make the product performance milder, safe and has no toxic or side effect. The first solvent can also be removed by membrane concentration, ultrafiltration, reverse osmosis, pervaporation and the like.

(5) Fine filtering to clarify; the purpose of the step is to enable the final extract to be more stable and clear, and a filter plate with the aperture of 0.2-10 mu m is used in the fine filtration process for filtration.

In order to facilitate the steps of reduced pressure concentration and fine filtration and protect reduced pressure concentration and fine filtration equipment better, a coarse filtration step can be added between the step (3) and the step (4), wherein the coarse filtration condition is 60-100 meshes coarse filtration, and raw material residues are filtered. In order to keep the stability of the filtered feed liquid, a cooling step can be added before coarse filtration, and the feed liquid is cooled to 40 ℃ or below 40 ℃ and then coarse filtration is optimally carried out.

The plant material may also be pretreated prior to the first extraction in order to facilitate the penetration of the cell walls by the extraction solvent and to further increase the extraction efficiency. The step of pretreatment is not necessary, the extraction rate of the invention is high and mainly depends on the matching of the first solvent and the second solvent and the process steps and parameters used for the second solvent, the pretreatment can further shorten the extraction time on the basis of the extraction rate achieved by the invention, but the pretreatment step can also not be used for the plant raw materials which are inconvenient to pretreat. The steps of pretreatment recommended by the inventors are as follows, and other steps known to those skilled in the art to achieve the purpose of pretreatment may be applied thereto.

(1) Coarse crushing: crushing the raw materials to 20-60 meshes; the pulverizing step can be performed by pulverizing equipment known in the art, such as a cutting machine, a wall breaking machine, a pulverizer, etc., and can be performed at one time or step by step from coarse to fine.

(2) The high temperature and high pressure treatment is carried out, wherein the high temperature is generally at least equal to or higher than 100 ℃, and the temperature is preferably controlled to be 100-130 ℃. The high pressure is more than 0.1Mpa, and the effect is best when the pressure is controlled within the range of 0.1-0.2 Mpa. The treatment time is not longer, preferably within 30 min. The main components of the plant cell wall are cellulose and pectin, the invention adopts high-temperature and high-pressure pretreatment of raw materials, and water vapor is utilized to destroy hydrogen bonds among polysaccharide molecules, so that the cell wall structure is loose, the solvent can enter through the cell wall in the subsequent extraction process, and the extraction efficiency is better.

(3) Drying, the purpose of drying is to remove redundant water vapor after high temperature and high pressure, the later extraction process is more favorably carried out, the extract is more stable, and the drying is preferably carried out for 1-2 h at the temperature of 50-80 ℃. Other drying means known to those skilled in the art may also be applied here.

The application of the plant extract in preparing cosmetics with skin barrier repairing effect is provided.

A cosmetic with skin barrier repairing effect is prepared from the plant extract and auxiliary materials acceptable in the field of cosmetics.

The external skin care oil with the effect of repairing skin barriers is prepared from the following raw materials in parts by weight:

1-4 parts of phytosterol ester, 0.2-0.5 part of bisabolol, 5-10 parts of sunflower seed oil, 5-10 parts of perilla seed oil, 65-85 parts of the plant extract and 0.1-0.3 part of butylated hydroxytoluene.

The preparation method of the external skin care oil comprises the following steps:

(1) weighing the raw materials according to the proportion;

(2) adding phytosterol ester and butylated hydroxytoluene into the external plant extract, heating and stirring at 50-60 ℃ to dissolve for 20-40 min;

(3) and cooling to 30-40 ℃, adding the bisabolol, the sunflower seed oil and the perilla seed oil, and uniformly stirring to obtain the composition.

The cosmetic is an oil type cosmetic, and other dosage forms such as cream, toner, emulsion, spray and the like can also be prepared by utilizing the conventional method and auxiliary materials in the field of the plant extract and skin care products. The plant extract can also achieve the effects after being simply crushed and mixed for external use, and the preparation method is not limited in the invention.

The recommended use method of the preparation of the invention is as follows: applying on human skin surface by smearing method, and gently massaging until absorption.

The beneficial results of the invention are as follows:

according to the invention, the safflower, the gardenia, the chrysanthemum morifolium and the flos Pruni mume are combined and matched, the optimal compatibility dosage is given, the components act synergistically, and the novel method for effectively extracting the plant raw materials of the cosmetics by using the double solvents with different polarities is combined, so that the extraction efficiency of the obtained plant extract is more excellent than that of the prior art, the extraction rate is greatly improved, and the final skin barrier repairing effect is more remarkable than that of the extract extracted by the prior art. The invention provides a novel method for effectively extracting plant raw materials for cosmetics by using double solvents with different polarities, which optimizes extraction steps and extraction condition parameters according to the optimized matching of an extraction solvent and the selection of a specific solvent, so that the extraction efficiency of the plant raw materials is greatly increased, the evaluation of the plant extraction efficiency is mainly evaluated by the antioxidant and anti-inflammatory effects of the plant raw materials, the main effects of plant extracts added into the cosmetics are also two, and the extracts extracted by the method are far superior to the extracts extracted by the prior art in the two effects through effect experiments. The extraction method effectively shortens the extraction time, has high extraction efficiency, uses conventional and cheap equipment, effectively reduces the preparation cost, and is very suitable for large-scale industrial production. The plant extract obtained by the invention has more stable components and better compatibility with auxiliary materials of various formulations of cosmetics, and particularly when the plant extract is added into oil-containing cosmetics, the defects of precipitation, precipitation and the like of the extract in the prior art, which influence the quality and the efficacy of products, are effectively overcome, so that the cosmetics are easier to store and transport, the product quality is better, and the effect is better when the plant extract is used. The invention effectively reduces the dosage of organic solvent in the prior art, reduces the pollution to the environment, and is more economic and environment-friendly.

Drawings

FIG. 1 is a graph of the evaluation of the DPPH clearance rate of the extraction effect of samples 1-24;

FIG. 2 is a graph of the evaluation of DPPH clearance rate of 25-30 extraction effect samples;

FIG. 3 is a graph of the DPPH clearance evaluation of the extraction effect of samples 31-36;

FIG. 4 is a diagram of DPPH clearance evaluation in a composition screening experiment;

FIG. 5 is a graph showing the TEWL measurement results in the tape damage test.

Detailed Description

In order to make the extraction method of the present invention more detailed for those skilled in the art, the inventors provide the following specific examples, and all the reagents involved are well known in the art and commercially available, and the instruments involved are also well known and available to those skilled in the art. In order to ensure the stability of the second solvent and the extract, each solvent used in the first solvent is an anhydrous solvent in the present embodiment. The following examples are not to be construed as limiting the claims in any way.

The raw materials and equipment purchasers used in the embodiment of the present invention are shown in tables 1 and 2.

Table 1 materials used in the invention

TABLE 2 Instrument used in the present invention

Example 1

2g of safflower, 4g of gardenia, 4g of Hangzhou white chrysanthemum and 6g of prunus mume;

(2) extracting for the first time: according to the material-liquid ratio of 1: adding ethanol at a ratio of 20m/m, mixing, and extracting at 55 deg.C for 2 hr;

(3) and (3) second extraction: according to the material-liquid ratio of 1: adding sunflower seed oil at a concentration of 20m/m, and extracting at 55 deg.C under stirring for 2 hr;

(4) concentrating under reduced pressure at 40 deg.C until ethanol is completely removed;

(5) filtering with filter plate with aperture of 10 μm, and filtering to obtain clear filtrate.

Example 2

6g of safflower, 1g of gardenia, 6g of Hangzhou white chrysanthemum and 4g of prunus mume;

(2) extracting for the first time: according to the material-liquid ratio of 1: adding ethanol at a concentration of 10m/m, mixing, and extracting at 40 deg.C for 1 hr;

(3) and (3) second extraction: according to the material-liquid ratio of 1: adding hydrogenated polyisobutene (20cSt) at the concentration of 10m/m, and stirring and extracting for 1h at the temperature of 40 ℃;

(4) concentrating under reduced pressure at 50 deg.C until ethanol is completely removed;

(5) filtering with filter plate with aperture of 1 μm, and filtering to obtain clear filtrate.

Example 3

8g of safflower, 6g of gardenia, 1g of Hangzhou white chrysanthemum and 1g of plum blossom;

(2) extracting for the first time: according to the material-liquid ratio of 1: adding anhydrous ethanol at 40m/m, mixing, and extracting at 90 deg.C for 0.5 h;

(3) and (3) second extraction: according to the material-liquid ratio of 1: adding caprylic acid/capric acid triglyceride at 40m/m, and stirring and extracting at 90 deg.C for 0.5 h;

(4) concentrating under reduced pressure at 80 deg.C until ethanol is completely removed;

(5) filtering with filter plate with pore diameter of 0.2 μm, and filtering to obtain clear filtrate.

Example 4

(1) Weighing the raw materials according to the following weight part ratio;

10g of safflower, 5g of gardenia, 4g of Hangzhou white chrysanthemum and 1g of plum blossom;

(2) coarse crushing: crushing the raw materials to 20 meshes and uniformly mixing;

(3) high-temperature high-pressure treatment: treating at 120 deg.C under 0.2MPa for 15 min;

(4) and (3) drying: drying at 50 deg.C for 1 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding chloroform at 60m/m, mixing, and extracting at 65 deg.C for 1 hr;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding white oil (7cSt) at 60m/m, and stirring and extracting at 65 deg.C for 1 h;

(7) concentrating under reduced pressure at 40 deg.C until chloroform is completely removed;

(8) filtering with filter plate with pore diameter of 0.2 μm, and filtering to obtain clear filtrate.

Example 5

(1) Weighing the raw materials according to the following weight part ratio;

5g of safflower, 10g of gardenia, 1g of Hangzhou white chrysanthemum and 10g of plum blossom;

(2) coarse crushing: crushing the raw materials to 40 meshes and uniformly mixing;

(3) high-temperature high-pressure treatment: treating at 120 deg.C under 0.1MPa for 15 min;

(4) and (3) drying: drying at 60 ℃ for 2 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding 50m/m chloroform, mixing, and extracting at 85 deg.C for 0.5 hr;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding caprylic acid/capric acid triglyceride at 50m/m, and stirring and extracting at 85 deg.C for 0.5 h;

(7) concentrating under reduced pressure at 60 deg.C until chloroform is completely removed;

(8) filtering with filter plate with aperture of 10 μm, and filtering to obtain clear filtrate.

Example 6

(1) Weighing the raw materials according to the following weight part ratio;

2g of safflower, 1g of gardenia, 10g of Hangzhou white chrysanthemum and 3g of prunus mume;

(2) coarse crushing: crushing the raw materials to 60 meshes and uniformly mixing;

(3) high-temperature high-pressure treatment: treating at 100 deg.C under 0.1MPa for 30 min;

(4) and (3) drying: drying at 75 deg.C for 1.5 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding chloroform at 60m/m, mixing, and extracting at 90 deg.C for 2 hr;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding hydrogenated polydecene (30cSt) at 60m/m, and stirring and extracting at 90 ℃ for 2 hours;

(7) concentrating under reduced pressure at 80 deg.C until chloroform is completely removed;

(8) filtering with filter plate with aperture of 6 μm, and filtering to obtain clear filtrate.

Example 7

(1) Weighing the raw materials according to the following weight part ratio;

5g of safflower, 3g of gardenia, 1g of Hangzhou white chrysanthemum and 1g of plum blossom;

(2) coarse crushing: crushing the raw materials to 30 meshes and mixing uniformly;

(3) high-temperature high-pressure treatment: treating at 100 deg.C under 0.2MPa for 10 min;

(4) and (3) drying: drying at 70 deg.C for 1 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding acetone at 70m/m, mixing, and extracting at 70 deg.C for 1 hr;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding isostearyl isostearate at a concentration of 70m/m, and stirring and extracting at 70 deg.C for 1 h;

(7) concentrating under reduced pressure at 45 deg.C until acetone is completely removed;

(8) filtering with filter plate with aperture of 2 μm, and filtering to obtain clear filtrate.

Example 8

(1) Weighing the raw materials according to the following weight part ratio;

3g of safflower, 5g of gardenia, 4g of Hangzhou white chrysanthemum and 3g of plum blossom;

(2) coarse crushing: crushing the raw materials to 50 meshes and uniformly mixing;

(3) high-temperature high-pressure treatment: treating at 110 deg.C under 0.1MPa for 20 min;

(4) and (3) drying: drying at 60 deg.C for 1 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding acetone at 35m/m, mixing, and extracting at 65 deg.C for 2 hr;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding soybean oil at 35m/m, and stirring and extracting at 65 ℃ for 2 h;

(7) concentrating under reduced pressure at 50 deg.C until acetone is completely removed;

(8) filtering with filter plate with pore diameter of 4 μm, and filtering to obtain clear filtrate.

Example 9

3g of safflower, 2g of gardenia, 1g of Hangzhou white chrysanthemum and 3g of plum blossom;

(3) high-temperature high-pressure treatment: treating at 130 deg.C under 0.1MPa for 30 min;

(4) and (3) drying: drying at 65 ℃ for 2 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding 55m/m chloroform-ethanol mixed solution (chloroform-ethanol is compounded according to the mass ratio of 1: 1), mixing, and extracting for 2h at 65 ℃;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding sesame oil at a concentration of 55m/m, and extracting at 65 deg.C under stirring for 2 hr;

(7) concentrating under reduced pressure at 55 deg.C until the solvent is completely removed;

(8) filtering with filter plate with aperture of 8 μm, and filtering to obtain clear filtrate.

Example 10

1g of safflower, 6g of gardenia, 5g of Hangzhou white chrysanthemum and 5g of plum blossom;

(2) coarse crushing: crushing the raw materials to 40 meshes, and uniformly mixing;

(3) high-temperature high-pressure treatment: treating at 110 deg.C under 0.2MPa for 30 min;

(4) and (3) drying: drying at 60 deg.C for 1.5 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding 30m/m ethanol, mixing, and extracting at 80 deg.C for 1 hr;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding caprylic acid/capric acid triglyceride at 10m/m, and stirring and extracting at 80 deg.C for 2 hr;

(7) cooling to below 40 deg.C, and coarse filtering with 60 mesh;

(8) concentrating under reduced pressure at 60 deg.C until the solvent is completely removed;

(9) cooling to below 40 deg.C, filtering with filter plate having aperture of 10 μm, and fine filtering to obtain clear filtrate.

Example 11

6g of safflower, 3g of gardenia, 5g of Hangzhou white chrysanthemum and 1g of plum blossom;

(3) high-temperature high-pressure treatment: treating at 110 deg.C under 0.2MPa for 15 min;

(4) and (3) drying: drying at 75 ℃ for 1 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding a chloroform and acetone mixed solvent (the chloroform and the acetone are compounded according to the mass ratio of 1: 1) at 95m/m, mixing, and extracting for 1h at 40 ℃;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding a caprylic/capric triglyceride and hydrogenated polydecene (17cSt) compound (the two are compounded according to a mass ratio of 1: 1) at 95m/m, and stirring and extracting for 1h at 40 ℃;

(7) cooling to below 40 deg.C, and coarse-filtering with 80 mesh;

(8) concentrating under reduced pressure at 70 deg.C until the solvent is completely removed;

(9) cooling to below 40 deg.C, filtering with filter plate with aperture of 1 μm, and fine filtering to obtain clear filtrate.

Example 12

8g of safflower, 1g of gardenia, 1g of Hangzhou white chrysanthemum and 3g of prunus mume;

(2) coarse crushing: crushing the raw materials to 60 meshes;

(2) high-temperature high-pressure treatment: treating at 130 deg.C under 0.2MPa for 10 min;

(3) and (3) drying: drying at 80 deg.C for 1.5 h;

(4) extracting for the first time: according to the material-liquid ratio of 1: adding mixed solvent of ethanol and acetone (mixed at a ratio of 1: 1) at 34m/m, mixing, and extracting at 80 deg.C for 1 hr;

(5) and (3) second extraction: according to the material-liquid ratio of 1: adding a compound of olive oil and macadamia nut oil (the two are compounded according to the mass ratio of 1: 1) at the speed of 35m/m, and stirring and extracting for 1h at the temperature of 60 ℃;

(6) cooling to below 40 deg.C, and coarse-filtering with 100 mesh sieve;

(7) concentrating under reduced pressure at 80 deg.C until the solvent is completely removed;

(8) cooling to below 40 deg.C, filtering with filter plate having aperture of 6 μm, and fine filtering to obtain clear filtrate.

Example 13

4g of safflower, 3g of gardenia, 10g of Hangzhou white chrysanthemum and 1g of plum blossom;

(2) coarse crushing: crushing the raw materials to 30 meshes;

(3) high-temperature high-pressure treatment: treating at 100 deg.C under 0.2MPa for 30 min;

(4) and (3) drying: drying at 60 deg.C for 1 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding a chloroform-ethanol mixed solvent (the chloroform-ethanol mixed solvent and the ethanol mixed solvent are compounded according to the mass ratio of 1: 1) at the speed of 15m/m, mixing, and extracting for 1.5h at the temperature of 70 ℃;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding a mixed solvent of white oil (16cSt) and hydrogenated polyisobutene (11cSt) at a mass ratio of 1:1 into the mixture of the white oil and the hydrogenated polyisobutene at a concentration of 15m/m, and stirring and extracting the mixture for 1.5 hours at the temperature of 70 ℃;

(7) cooling to below 40 deg.C, and coarse filtering with 90 mesh sieve;

(8) concentrating under reduced pressure at 80 deg.C until the solvent is completely removed;

(9) cooling to below 40 deg.C, filtering with filter plate having aperture of 5 μm, and fine filtering to obtain clear filtrate.

Example 14

1g of safflower, 10g of gardenia, 2g of Hangzhou white chrysanthemum and 5g of prunus mume;

(2) coarse crushing: crushing the raw materials to 40 meshes;

(3) high-temperature high-pressure treatment: treating at 110 deg.C under 0.2MPa for 10 min;

(4) and (3) drying: drying at 40 ℃ for 1 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding 35m/m ethanol, mixing, and extracting at 90 deg.C for 1 hr;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding a grape seed oil and oat oil mixed solvent (the two are compounded according to the mass ratio of 1: 1) at 35m/m, and stirring and extracting for 0.5h at 50 ℃;

(7) cooling to below 40 deg.C, and coarse filtering with 90 mesh sieve;

Example 15

1g of safflower, 5g of gardenia, 5g of Hangzhou white chrysanthemum and 10g of plum blossom;

(2) coarse crushing: crushing the raw materials to 40 meshes;

(3) high-temperature high-pressure treatment: treating at 130 deg.C under 0.2MPa for 10 min;

(4) and (3) drying: drying at 70 deg.C for 1 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding chloroform at 65m/m, mixing, and extracting at 70 deg.C for 1 hr;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding sweet almond oil at 65m/m, and stirring and extracting at 70 deg.C for 1 hr;

(7) cooling to below 40 deg.C, and coarse filtering with 90 mesh sieve;

(9) cooling to below 40 deg.C, filtering with filter plate having aperture of 0.5 μm, and fine filtering to obtain clear filtrate.

Example 16 cosmetic oil formulation having skin Barrier repairing Effect

(1) Weighing the raw materials according to the following mixture ratio;

1g of phytosterol ester, 0.3g of bisabolol, 6g of sunflower seed oil, 10g of perilla seed oil, 65g of plant extract prepared in example 1 and 0.2g of butylated hydroxytoluene.

(2) Adding phytosterol ester and butylated hydroxytoluene into the topical plant extract, heating and stirring at 50 deg.C for dissolving for 30 min;

(3) cooling to 40 deg.C, adding bisabolol, oleum Helianthi and Perilla seed oil, and stirring.

Example 17 oil-based cosmetic having skin Barrier repairing Effect

(1) Weighing the raw materials according to the proportion;

3g of phytosterol ester, 0.2g of bisabolol, 5g of sunflower seed oil, 6g of perilla seed oil, 70g of plant extract prepared in example 10 and 0.1g of butylated hydroxytoluene.

(2) Adding phytosterol ester and butylated hydroxytoluene into the topical plant extract, heating and stirring at 60 deg.C for dissolving for 20 min;

(3) cooling to 30 deg.C, adding bisabolol, oleum Helianthi and Perilla seed oil, and stirring.

Example 18 cosmetic oil formulation having skin Barrier repairing Effect

(1) Weighing the raw materials according to the proportion;

4g of phytosterol ester, 0.5g of bisabolol, 10g of sunflower seed oil, 5g of perilla seed oil, 85g of plant extract prepared in example 15 and 0.3g of butylated hydroxytoluene.

(2) Adding phytosterol ester and butylated hydroxytoluene into the topical plant extract, heating and stirring at 55 deg.C for dissolving for 40 min;

(3) cooling to 35 deg.C, adding bisabolol, oleum Helianthi and Perilla seed oil, and stirring.

Efficacy test of the invention

The cooperation of the solvent I and the solvent II, the optimized extraction process and the extraction parameters of the invention are combined, the synergistic effect can be achieved, the extraction rate is higher, the property of the extract is more excellent and more stable, the extraction cost is lower, and the method is suitable for industrial application.

Selection of solvent one and solvent two of the present invention

1. The solvent I is a representative solvent which is commonly used for plant extraction, has good compatibility with various active ingredients and high extraction rate; considering that the extraction effect of the solvent one is better than that of the solvent two, the extraction effect is finally determined to be ethanol, acetone and chloroform. The inventor considers that the technical effects already meet the requirements of the invention, so that the further screening of the first solvent is not needed, and the workload for selecting the second solvent is reduced.

2. The selection process of the second solvent is briefly described as follows:

the second solvent is selected from solvent with polarity less than that of the first solvent, and oil is preferably selected as the second solvent.

(1) Vegetable oil: the properties of the vegetable oils are similar, so only one is selected as a representative, and the vegetable oils are respectively compounded and extracted with three solvents of the solvent I, and have better effects;

(2) white oil: selecting two kinds of white oil (generally, the numerical values near the critical value, such as 26 and 32) within and outside a limited viscosity range, and respectively compounding and extracting the white oil with three solvents of the first solvent, wherein the white oil within the viscosity range has a good effect, and the white oil outside the viscosity range has a poor effect;

(3) hydrogenated polyisobutene, hydrogenated polydecene: both of these are olefin polymers, only one of them is selected as a representative, and the white oil screening work is repeated, namely, the experiments are respectively carried out in the limited viscosity range and outside the viscosity range (generally, the values near the critical value, such as 26 and 32), so that different extraction effects are obtained;

(4) caprylic/capric triglyceride: the extract is compounded and extracted with three solvents of the first solvent, and has better effect;

(5) isostearyl isostearate: the extract is compounded and extracted with three solvents of the first solvent, and has better effect;

(6) polydimethylsiloxane (silicone oil): the silicon oil is a silicon chain, has poor dissolving effect on active ingredients of the carbon chain, and has poor extraction effect when being compounded with the solvent I respectively.

The above is an experimental idea of the solvent screening part, namely samples 1-24 of the solvent selection part. The raw materials and preparation methods of samples 1-24 were the same, except for the extraction solvents.

The preparation method comprises the following steps:

3g of safflower, 6g of gardenia, 5g of Hangzhou white chrysanthemum and 5g of plum blossom;

(2) coarse crushing: crushing the raw materials to 40 meshes;

(4) and (3) drying: drying at 60 deg.C for 1.5 h;

(5) extracting for the first time: according to the material-liquid ratio of 1: adding a first solvent at a concentration of 30m/m, mixing, and extracting at 80 ℃ for 1 h;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding a second solvent at the concentration of 10m/m, and stirring and extracting for 2 hours at the temperature of 80 ℃;

(7) cooling to below 40 deg.C, and coarse-filtering with 60 mesh sieve to obtain filtrate;

The solvents used in samples 1-24 are shown in Table 3

TABLE 3 sample solvent table

3. And (3) testing results:

the content of the part is to screen a second solvent, wherein the first solvent is fixed into ethanol, chloroform and acetone.

(1) DPPH free radical scavenging experiments: the components of the plant extract are complex, and the analysis and quantification of the effective components of the extract are difficult, so that the extraction efficiency of the effective components is evaluated by the detection of antioxidant activity by a person skilled in the art, and the extract prepared by the process with good extraction efficiency has more excellent antioxidant activity. Antioxidant activity is generally evaluated using DPPH free radical scavenging experiments. DPPH (2, 2-biphenyl-1-picrylhydrazino) is a stable organic nitrogen free radical and is widely applied to in vitro antioxidant capacity research. Based on the characteristic absorption peak of DPPH at about 515nm, the antioxidant provides hydrogen atoms to reduce single electrons on DPPH to weaken the color, and the degree of free radical scavenging is evaluated according to the reduction of the light absorption value.

The results of the antioxidant activity test of samples 1-24 are shown in FIG. 1.

(1) Stability experiments, see table 4.

TABLE 4 comparison of stability of different solvent extracts

The experimental results are as follows:

1. samples 1-3 are prepared by extracting vegetable oil (the vegetable oil is similar in nature, and only sunflower seed oil is taken as an example) with a solvent I in a compounding manner, and the vegetable oil is compounded with ethanol, acetone and chloroform, so that the good extraction effect is achieved.

2. Samples 4-6 are prepared by extracting caprylic acid/capric acid triglyceride with ethanol, acetone and chloroform respectively in a compounding manner, and have good extraction effect.

3. Samples 7-9 are prepared by extracting isostearyl isostearate with ethanol, acetone and chloroform respectively in a compounding manner, and have good extraction effect.

4. Samples 10-12 are white oil (26cSt, which meets the requirement of the invention that the kinematic viscosity is less than or equal to 30cSt), and are respectively compounded and extracted with ethanol, acetone and chloroform, and the extraction effect is better.

5. Samples 13-15 are white oil (32cSt, which does not meet the requirement of the invention that the kinematic viscosity is less than or equal to 30cSt), and are respectively compounded and extracted with ethanol, acetone and chloroform, and the extraction effect is poor.

6. Samples 10 to 15 are the results of comparing the white oil having a kinematic viscosity of 30cSt or less with the white oil having a kinematic viscosity of more than 30cSt, and the reason for selecting the white oil having a kinematic viscosity of 30cSt or less is shown by the difference in extraction effect.

7. Samples 16-18 are prepared by respectively extracting hydrogenated polydecene (30cSt, which meets the requirement of the invention that the kinematic viscosity is less than or equal to 30cSt) with ethanol, acetone and chloroform in a compounding way, and have good extraction effect.

8. Samples 19-21 are prepared by respectively extracting hydrogenated polydecene (46cSt, which does not meet the requirement of the invention that the kinematic viscosity is less than or equal to 30cSt) with ethanol, acetone and chloroform in a compounding manner, and the extraction effect is poor.

9. Samples 16-21 are similar to white oil and are a comparison of hydrogenated polydecene with kinematic viscosity of 30cSt or less with those with kinematic viscosity of > 30cSt, and the reason for selecting hydrogenated polydecene with kinematic viscosity of 30cSt or less is illustrated by the difference in extraction effect. In addition, since both hydrogenated polydecene and hydrogenated polyisobutene are polymers, the description will be made by taking hydrogenated polydecene as an example.

10. Samples 21-24 are prepared by compounding and extracting polydimethylsiloxane (silicone oil, PMX200, 6cSt) with ethanol, acetone and chloroform respectively, and the silicone oil has a silicon chain structure and has poor dissolving effect on active ingredients of a carbon chain, so that the extraction effect is poor, and the DPPH clearance rate is very low; the poor compatibility also leads to poor stability, manifested as turbidity of the sample or precipitation (precipitation) of the active ingredient.

Through the above experiments, the solvent II preferred by the present invention comprises vegetable oil (samples 1 to 3), caprylic/capric triglyceride (samples 4 to 6), isostearyl isostearate (samples 7 to 9), white oil (samples 10 to 12) with a kinematic viscosity (40 ℃) of less than or equal to 30cSt, hydrogenated polyisobutene (which is an olefin polymer with hydrogenated polydecene, and only hydrogenated polydecene is taken as an example for experiments) with a kinematic viscosity (40 ℃) of less than or equal to 30cSt, and hydrogenated polydecene (samples 16 to 18) with a kinematic viscosity (40 ℃) of less than or equal to 30 cSt.

The solvent II used as a comparative example comprises white oil (samples 13-15) with kinematic viscosity (40 ℃) higher than 30cSt, hydrogenated polydecene (samples 19-21) with kinematic viscosity (40 ℃) higher than 30cSt, and 6cSt polydimethylsiloxane PMX200 (samples 21-24).

According to the comparative experiments, the vegetable oil, caprylic/capric triglyceride, isostearyl isostearate, white oil with the kinematic viscosity (40 ℃) of less than or equal to 30cSt, hydrogenated polyisobutene and hydrogenated polydecene all have good extraction effects by respectively carrying out compound extraction with the solvent I (ethanol, acetone and chloroform), and the extracted product has good stability, so that the solvent II is suitable to be used as the solvent II of the invention and matched with the solvent I to realize the extraction process of the invention. White oil with kinematic viscosity (40 ℃) more than 30cSt, hydrogenated polyisobutene and hydrogenated polydecene are not suitable for the solvent II of the invention because the viscosity is increased, which is not beneficial to the mass transfer in the extraction process, and the extraction effect is not ideal. The silicon oil (polydimethylsiloxane) has poor compatibility with carbon chain active ingredients in plants due to the structural difference, so that the extraction efficiency is low, and the stability of the extracted product is poor, so that the silicon oil (polydimethylsiloxane) is not suitable to be used as the solvent II.

Secondly, determining the extracted parameters of the invention

1. Temperature parameter selection experiment: the second extraction step is solvent-solvent synergistic extraction, so the extraction in the step is very important, and the extraction temperature in the second extraction step directly influences the intersolubility degree and the extraction efficiency of the two solvents.

In this experiment, the first solvent is exemplified by ethanol, and the second solvent is exemplified by caprylic/capric triglyceride.

The specific preparation process is as in experiment one, and the specific steps are as follows:

(4) and (3) drying: drying at 60 deg.C for 1.5 h;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding caprylic acid/capric acid triglyceride at a concentration of 10m/m, wherein the extraction temperature is shown in Table 5, and stirring for 2 h;

TABLE 5

The extraction effect of the sample 25-30 is evaluated by DPPH clearance, and the experimental method is shown in DPPH free radical clearance experiment. The results are shown in FIG. 2. Therefore, the extraction efficiency is highest at the temperature of the extract of 40-90 ℃, is too low under the condition that the temperature is lower than 40 ℃ or higher than 90 ℃, and if poor temperature is adopted, the extraction rate can be improved only by prolonging the extraction time, so that the economic benefit of the extraction process on industrial application is influenced. The extraction temperature is 80 deg.C, and the extraction efficiency is optimal.

The stability test methods of the samples 25-30 are shown in stability comparison, and the results are shown in Table 6.

TABLE 6 comparison of stability of samples taken at different temperatures

The content of the part is to screen the technological parameters of the second extraction step, taking the temperature as an example, under six temperature conditions of 30 ℃, 40 ℃, 60 ℃, 80 ℃, 90 ℃ and 95 ℃, the DPPH and the stability of the product are better, the extraction effect at 30 ℃ is poor, the extraction effect at 95 ℃ is poor, the stability of the product is poor due to overhigh temperature, discoloration and peculiar smell occur, so the final extraction temperature is recommended to be in the range of 40-90 ℃, and the optimal extraction temperature is 80 ℃.

2. And (3) performing a second extraction material-liquid ratio parameter selection experiment: the extraction material-liquid ratio directly influences the intersolubility of the first solvent and the second solvent and the extraction efficiency of the matched extraction

(4) and (3) drying: drying at 60 deg.C for 1.5 h;

(6) and (3) second extraction: adding caprylic acid/capric acid triglyceride according to the feed-liquid ratio shown in Table 7, and stirring and extracting at 80 deg.C for 2 h;

TABLE 7

The extraction effect of the samples 31-36 is evaluated by DPPH clearance, and the experimental method is shown in DPPH free radical clearance experiment. The results are shown in FIG. 3. It can be seen that, when the feed-liquid ratio is 1:10 ~ 100 extraction efficiency height, and 1: 10-50 of the extraction efficiency is high.

Thirdly, the raw material medicines and compatibility selection of the composition are optimized

The selection thought of the raw material medicine of the invention is as follows: according to the thought of 'holism, syndrome differentiation and synthesis' in the traditional Chinese medicine and the formula principle of 'monarch, minister, assistant and guide', the saffron, the gardenia, the Hangzhou white chrysanthemum and the flos Pruni mume are combined, the monarch drug activates blood and dissipates stasis, the minister drug clears heat and cools blood, and the monarch drug and the minister drug are mutually used and have synergistic effect; adjuvant drugs for clearing away heat and toxic materials, dispelling wind and dissipating heat; guiding the drugs to nourish yin and promote the production of body fluid. The whole formula removes inflammatory factors by activating blood and cooling blood, clearing away heat and toxic materials, dispelling wind and dissipating heat, and nourishing yin and promoting the production of body fluid to care skin and supplement moisture, so that symptoms such as skin redness and mild discomfort are relieved, skin barriers are repaired, and skin tolerance is improved. And the improvement of the preparation method is combined, so that the extraction efficiency of the active ingredients is obviously improved, and the high-efficiency plant extract is obtained.

The preparation methods of the samples in the experiment are the same, the total mass of the raw material medicines is 10g, and the components and compatibility of the formula of each sample are different, which is detailed in table 8. The preparation method comprises the following steps:

(1) weighing the raw materials according to the weight part ratio in the table 8, and uniformly mixing;

(4) and (3) drying: drying at 60 deg.C for 1.5 h;

(6) and (3) second extraction: according to the material-liquid ratio of 1: adding caprylic/capric triglyceride into 10m/m, and extracting at 80 deg.C for 2 hr;

TABLE 8

The effects of the 1-11 formula of the sample are evaluated by DPPH clearance and adhesive tape damage tests.

DPPH free radical scavenging assay:

the test methods are described above for DPPH radical scavenging.

The test results are shown in fig. 4, and the results show that the DPPH clearance rate of the formula and the dosage of the sample 5 (the formula of the invention) is highest, the effect is best, the raw materials of the formula of the samples 1-4 and 6-11 are lacked or the proportion is not in the range of the proportion of the invention, the DPPH clearance rate is lower, and the effect is not good.

2. Tape damage test:

a mouse epidermis damage (adhesive tape damage) model is established, the recovery effect of the plant extract on the damaged epidermis is investigated, and the repair effect is represented.

Tape damage test method: continuously sticking and rapidly tearing off the skin by using an adhesive tape for a plurality of times until the skin of the mouse has small blood spots, respectively smearing each sample once a day for 4d, and respectively measuring the percutaneous water loss (TEWL) after smearing for 0d, 2d and 4 d.

The sample for animal experiments is an external repair barrier skin care composition preparation added with the plant extract of the invention with the mass percentage of 5.0 percent, and the formula table is shown in the following table.

TABLE 9 formulation of barrier-repairing skin care composition

The samples are samples 1-11 in Table 8; the blank group is a model group without smearing any sample after the skin is damaged; the normal group was a model group with no tape damage to the skin.

The skin injury repair test results (shown in table 10) show that the transdermal water dispersion loss of the skin care preparation containing 5.0% of the sample 5 (the formula of the invention) is far less than that of other groups, namely, the formula (sample 5) used in the invention has the effect of rapidly and more excellent repairing skin barrier compared with other groups (samples 1-4 and samples 6-11), and can better promote the repair and healing of skin injury.

TABLE 10 different formulations of extract tape Damage test TEWL values

Fourthly, the extraction efficiency of the method of the invention is compared with that of the prior art

The components of the plant extract are complex, and the analysis and quantification of the effective components of the extract are difficult, so that the extraction efficiency of the effective components is evaluated by detecting the antioxidant activity and the anti-inflammatory activity by a person skilled in the art, and the extract prepared by the process with good extraction efficiency has more excellent efficacy.

Antioxidant activity is generally evaluated using DPPH free radical scavenging experiments. DPPH (2, 2-biphenyl-1-picrylhydrazino) is a stable organic nitrogen free radical and is widely applied to in vitro antioxidant capacity research. Based on the characteristic absorption peak of DPPH at about 515nm, the antioxidant provides hydrogen atoms to reduce single electrons on DPPH to weaken the color, and the degree of free radical scavenging is evaluated according to the reduction of the light absorption value.

Anti-inflammatory activity is generally assessed experimentally by inhibiting hyaluronidase. Hyaluronidase is a participant of anaphylactic reaction, and researches show that hyaluronidase has strong correlation with inflammation and allergy, and a hyaluronidase in-vitro inhibition test is often used as a method for measuring the antiallergic activity. The antiallergic activity takes the hyaluronidase inhibition rate as an index, and the higher the hyaluronidase inhibition rate is, the stronger the antiallergic activity is.

The sample preparation for the efficacy test of the present invention is as follows

Sample 1 (prior art grease two extractions): weighing 3g of safflower, 6g of gardenia, 5g of Hangzhou white chrysanthemum and 5g of flos Pruni mume, crushing to 40 meshes, treating at the temperature of 110 ℃ for 30min under the pressure of 0.2MPa, and drying at the temperature of 60 ℃ for 1.5 h; the material-liquid ratio is 1: 30(m/m), adding 100g of caprylic/capric triglyceride, and stirring and extracting at 80 ℃ for 1 h; the material-liquid ratio is 1:10 (m/m), adding 300g of caprylic/capric triglyceride again, and stirring and extracting at 80 ℃ for 2 h; cooling to below 40 deg.C, filtering with filter plate having aperture of 10 μm, and fine filtering to clarify.

Sample 2 (prior art ethanol double extraction): weighing 3g of safflower, 6g of gardenia, 5g of Hangzhou white chrysanthemum and 5g of flos Pruni mume, crushing to 40 meshes, treating at the temperature of 110 ℃ for 30min under the pressure of 0.2MPa, and drying at the temperature of 60 ℃ for 1.5 h; the material-liquid ratio is 1: 30(m/m), adding 100g of absolute ethyl alcohol, and stirring and extracting at 80 ℃ for 1 h; the material-liquid ratio is 1:10 (m/m), adding 300g of absolute ethyl alcohol again, and stirring and extracting for 2h at 80 ℃; cooling to below 40 deg.C, and filtering to obtain filtrate; concentrating under reduced pressure at 60 deg.C; filtering with filter plate with aperture of 10 μm, and fine filtering to obtain the final product.

Sample 3 (two extractions with solvent one less polar than solvent two): 3g of safflower, 6g of gardenia, 5g of Hangzhou white chrysanthemum and 5g of flos Pruni mume, crushing to 40 meshes, treating at the temperature of 110 ℃ for 30min under the pressure of 0.2MPa, and drying at the temperature of 60 ℃ for 1.5 h; the material-liquid ratio is 1: 30(m/m), adding 300g of cyclohexane, and stirring and extracting at 80 ℃ for 1 h; the material-liquid ratio is 1:10 (m/m), adding 900g of butanediol, and stirring and extracting for 2 hours at 80 ℃; cooling to below 40 deg.C, and filtering to obtain filtrate; concentrating under reduced pressure at 60 deg.C to remove cyclohexane; filtering with filter plate with aperture of 10 μm, and fine filtering to obtain extract.

Sample 4: example 10.

DPPH radical scavenging experiment

(1) The experimental method comprises the following steps: taking 1mL of DPPH solution and 1mL of sample solution, fully oscillating and uniformly mixing, standing for 30min, and measuring the absorbance of the mixture by using a microplate reader at the wavelength of 517 nm.

DPPH free radical clearance calculation formula:

DPPH free radical clearance [ (B + C) -A ]/B100%

In the formula: a is the OD value of the sample solution mixed with the DPPH solution, B is the OD value of the absolute ethyl alcohol mixed with the DPPH solution, and C is the OD value of the absolute ethyl alcohol mixed with the sample solution.

(1) And (4) experimental conclusion: as shown in table 11.

TABLE 11 comparison of DPPH clearance for samples prepared by different procedures

Sample name	Test concentration%	Clearance rate%
			Sample
1	5	31
			Sample 2	5	45
Sample 3	5	24
			Sample 4 (example 10)	5	87

The sample 1 is directly extracted by adopting grease, and because the grease has large molecular weight, is not easy to pass through cell walls and cell membranes to extract intracellular active ingredients, has high viscosity, is not beneficial to substance transfer in the extraction process, and has low DPPH clearance rate.

The sample 2 is extracted by ethanol, the ethanol is an excellent solvent, and a large amount of water-soluble polysaccharide is dissolved out while the oil-soluble active ingredients are extracted; during concentration, part of oil-soluble active ingredients are wrapped by viscous substances such as polysaccharide and the like and separated out to form precipitates, so that loss of the active ingredients is caused, and the DPPH clearance rate is low.

Sample 3 is extracted by two-step double solvents, but the polarity of solvent 1 (compared with solvent 2) is weaker, the polarity of solvent 2 (compared with solvent 1) is stronger, the interaction between solvent 1 and cell membranes is weak, the two solvents are not favorable for entering cells to extract active ingredients, the synergistic effect between the two solvents is damaged, the extraction rate is reduced, and the DPPH clearance rate is lower.

Example 10 the DPPH clearance for the samples prepared is significantly higher than for

samples

1, 2 and 3 and far better than the sum of the effects of

samples

1 and 2.

The inventors have made the same comparison with other examples and reached the same conclusion.

2. Experiment for inhibiting hyaluronidase

(1) The experimental method comprises the following steps: 0.1mL of 0.25mmol/L calcium chloride solution and 0.5mL of hyaluronidase solution are cultured for 20min at 37 ℃; adding 0.5mL of sample solution, and continuing to culture at 37 ℃ for 20 min; adding 0.5mL of hyaluronic acid sodium solution, keeping the temperature at 37 ℃ for 30min, and standing at normal temperature for 5 min; adding 0.1mL of 0.4mol/L sodium hydroxide solution and 0.5mL of acetylacetone solution, heating in a boiling water bath for 15min, and immediately cooling with ice water for 5 min; adding 1.0mL of Ellisib reagent, diluting with 3.0mL of absolute ethanol, standing for 20min for color development, and measuring the absorbance at 555nm by using a microplate reader.

The hyaluronidase inhibition rate calculation formula is as follows:

hyaluronidase inhibition [ (A-B) - (C-D) ]/(A-D) × 100%

In the formula: a is the absorbance of the control solution (the sample solution is replaced by acetic acid buffer solution), B is the absorbance of the control blank solution (the sample solution and the enzyme solution are replaced by acetic acid buffer solution), C is the absorbance value of the sample solution, and D is the absorbance of the sample blank solution (the enzyme solution is replaced by acetic acid buffer solution).

(2) And (4) experimental conclusion: as shown in the table below.

TABLE 12 comparison of hyaluronidase inhibition ratios for samples prepared by different processes

Sample name	Test concentration%	Inhibition ratio%
			Sample
1	5	13
			Sample 2	5	44
Sample 3	5	21
			Sample 4 (example 10)	5	64

The sample 1 is directly extracted by adopting the grease, and the molecular weight of the grease is large, the grease is difficult to pass through cell walls and cell membranes to extract intracellular active ingredients, and the viscosity is high, so that the substance transfer in the extraction process is not facilitated, and the hyaluronidase inhibition rate is low.

The sample 2 is extracted by ethanol, the ethanol is an excellent solvent, and a large amount of water-soluble polysaccharide is dissolved out while the oil-soluble active ingredients are extracted; during concentration, the oil soluble active ingredients are separated out from the part wrapped by the viscous substances such as polysaccharide and the like to form precipitates, so that the loss of the active ingredients is caused, and the hyaluronidase inhibition rate is low.

Sample 3 is extracted by two-step double solvents, but the polarity of solvent 1 (compared with solvent 2) is weaker, the polarity of solvent 2 (compared with solvent 1) is stronger, the interaction between solvent 1 and cell membrane is weak, so that the two solvents are not favorable for entering cells to extract active ingredients, the synergistic effect between the two solvents is damaged, the extraction rate is reduced, and the hyaluronidase inhibition rate is low.

Example 10 the prepared sample has a hyaluronidase inhibition rate significantly higher than that of

samples

1, 2 and 3 and far better than the sum of the effects of

samples

1 and 2.

Compared with the prior art, the stability of the extract obtained by the invention in oil type cosmetics is higher

1. Used for clarity comparison in oil type cosmetics

(1) The experimental method comprises the following steps: heating 3.0g of sample liquid and 27.0g of oil as common adjuvant of oil cosmetic to 50 deg.C, stirring for dissolving for 20min, standing, cooling for 1 hr, and observing the dissolution of sample in oil. The compatibility of the sample and the grease is good, and the dissolved sample is clear and transparent; if the sample is poorly compatible with the oil, the sample becomes cloudy after dissolution. Therefore, the solubility of the sample in the oil and fat can be characterized by the turbidity after the dissolution.

Turbidity is an optical property due to scattering of light by minute particles in a liquid, and the amount of scattered light increases as the turbidity increases. In the experiment, a HI93414 high-precision data type turbidity measuring instrument is adopted to detect the turbidity of the sample. Lower values of the measured values prove that lower turbidity proves better clarity and good product stability.

(2) The sample preparation process comprises the following steps: same as the DPPH radical scavenging experimental sample.

TABLE 13 turbidity comparison of samples from different processes

(3) And (4) experimental conclusion: as shown in the above table.

Sample 1 is a fat extract by itself, and therefore turbidity is excellent in oil-type cosmetic accessories; sample 2 is an alcohol-soluble extract, and has poor compatibility with oils and fats, and therefore has high turbidity. The extraction solvent of sample 3 reverses the polarity of the solvent of the present invention, resulting in a final product with a stronger solvent polarity and poor compatibility with oils and fats, resulting in high turbidity. The sample 4 is extracted by matching the solvent I and the solvent II, and the extraction process is optimized, so that the compatibility of the active ingredients and the cosmetic common auxiliary material oil is good, the turbidity is lower, and even better than that of the extract obtained by oil extraction.

2. Stability test

(1) The experimental method comprises the following steps: 10g of sample liquid and 190g of caprylic/capric triglyceride are heated to about 50 ℃, stirred and dissolved for 20min, the prepared sample is evenly divided into five parts, and the five parts are respectively placed in dark (room temperature dark box), refrigeration (4 ℃ refrigerator), illumination (28 ℃ illumination incubator), heat (45 ℃ oven) and freezing (-15 ℃ refrigerator) under five conditions, and the stability is observed on days 7, 14 and 30 respectively.

(2) Sample information:

samples

1, 2, 3 and 4 above.

TABLE 14 comparison of stability of samples from different processes

(3) And (4) experimental conclusion: as shown in the above table.

Sample 1 (oil extraction) was found to have a small amount of precipitation in the 30 day stability test and a slight off-flavor indicating sample deterioration. Sample 2 (ethanol extraction) was found to have a large amount of precipitate in the 30-day stability test, indicating that the stability of the sample was poor. In the 30-day stability test, it can be seen that sample 3 (in the case where solvent one is less polar than solvent two) has a large amount of precipitate on its appearance, indicating that the stability of the sample is poor. Sample 4 (example 10) the 30-day stability test showed a clear and transparent appearance and a normal odor, indicating that the extracts prepared according to the invention have better stability than

samples

1, 2 and 3.

Sixthly, the method of the invention is compared with the prior art

According to the DPPH free radical scavenging experiment results, the extraction efficiency of the present invention (sample 4) is much higher than that of the direct extraction of oil (sample 1) and the ethanol extraction (sample 2) when the extraction conditions are the same (material-to-liquid ratio, extraction temperature, extraction time).

TABLE 15 cost comparison of the present invention with the prior art industrial application

As can be seen from the above table, the extraction efficiency of the present invention is far superior to that of

samples

1 and 2. If the same extraction efficiency as the present invention is desired, the amount needs to be increased to two times, so that the present invention has less raw material usage and thus lower preparation, storage and transportation costs compared to the existing extraction processes. Compared with the prior art, the invention has the advantages of saving cost, reducing material and energy consumption. Is very suitable for the industrial mass production of energy conservation and emission reduction at present.

Seventh, efficacy experiment

1. Tape damage test

TABLE 16 repair Barrier skin care composition formulation

Name of raw materials	Addition amount (%)
		Caprylic/capric triglyceride	50
Hydrogenated polyisobutenes	30
		White oil-16	15
Sample (I)	5

The samples were sample 1 (oil extraction), sample 2 (ethanol extraction), sample 3 (two extractions with a polarity of solvent one less than solvent two) and sample 4 (example 10), example 16, example 17, example 18; the blank group is a model group without smearing any sample after the skin is damaged; the normal group was a model group with no tape damage to the skin; the commercial offer is a skin care formulation containing 5.0% ceramide 3, and the formula table is shown in the following table. Examples 16, 17 and 18 are oil-based products that can be used alone or as additives as in this experiment, and the specific methods of use do not affect the final results.

TABLE 17 skin care formulations for the group of marketed contestants

Name of raw materials	Addition amount (%)
		Caprylic/capric triglyceride	50
Hydrogenated polyisobutenes	30
		White oil-16	15
Ceramide 3	5

The results of the skin lesion repair test (as shown in FIG. 5) show that 5.0% of the examples (example 10),

Example 16, example 17, example 18) formulations had much lower transdermal water dispersion than other groups, thus indicating that the external barrier repair skin care formulation of the present invention has a rapid and superior efficacy of repairing skin barrier, promoting skin damage repair and healing, compared to the prior art.

2. Human body test

The skin protection barrier function of the sample is inspected by measuring the percutaneous water loss through a human body trial for 4 h.

The percutaneous water loss test method comprises the following steps: the samples were tested using a CK official hydroscope with skin percutaneous water loss (TEWL) as an index under the test conditions of 25 + -2 deg.C and 50 + -10% humidity. The samples for the human body test and the samples for the tape damage test, the blank group addition sample was caprylic/capric triglyceride, and the formula table is shown in table 16. The measurement results are shown in Table 18.

TABLE 18 human efficacy test results for formulations with 5.0% sample addition- -arm meridian water dispersible data

The tests prove that after the external skin care preparation prepared from the extract disclosed by the embodiment of the invention is used by a subject, the water dispersion of the skin of the arm shows a reduction trend, and the external skin care preparation prepared by the invention has an obvious function of repairing skin barriers.

(3) Human body patch test

The safety of the plant extract of the present invention was evaluated with reference to technical specifications for cosmetic safety (2015 edition), chapter seventh, section 2, test method for closed patches on human skin.

The tested part is the back, 33 volunteers continue to stick the spots for 24 hours, and the test object spot tester is removed and then observed for 30min and 24 hours respectively.

The samples for the human body patch test were sample 1 (oil extraction), sample 2 (ethanol extraction), sample 3 (two extractions in the case where the polarity of the first solvent was smaller than that of the second solvent), and example 10, example 16, example 17, and example 18, and the percentage of the amount of the added sample was 20%, and the formula table is shown in the following table.

Table 19 formulation of barrier repair skin care composition for use in the patch test

Name of raw materials	Addition amount (%)
		Caprylic/capric triglyceride	35
Hydrogenated polyisobutenes	30
		White oil-16	15
Sample (I)	20

The results of the human patch test are shown in the table below. And (4) judging the standard: and (3) suspicious reaction: only faint erythema. Weak positive reaction (erythema reaction): erythema, infiltration, edema, and possibly pimples. Strong positive reaction (erythema reaction): erythema, infiltration, edema, and possibly pimples; the reaction may be beyond the test area. Very strong positive reaction (erythema reaction): obvious erythema, severe infiltration, edema, and fusional herpes; the reaction goes beyond the test area.

TABLE 20 observations 0.5 hours after plaque tester removal

Table 21 observations 24 hours after plaque tester removal

The number of the self-check participated in is 33, the number of the effective people is 31 in 0.5h, and the number of the effective people is 30 in 24 h.

The result of 0.5h shows that the spot tester and the dry filter paper sheet have 5 adverse reactions; adverse reactions appear in the spot tester 2 cases; 1 case of adverse reactions occurred in sample 1 (oil extract), sample 2 (ethanol extract), and sample 3 (extract in case that the polarity of the solvent one is smaller than that of the solvent two); no adverse reactions occurred in samples 4 (example 10), 5 (example 16), 6 (example 17), and 7 (example 18).

The 24h result shows that 1 adverse reaction occurs in the spot tester + the dry filter paper sheet, the spot tester, the sample 1 (oil extract), the sample 2 (ethanol extract) and the sample 3 (extract under the condition that the polarity of the solvent one is less than that of the solvent two); no adverse reactions occurred in samples 4 (example 10), 5 (example 16), 6 (example 17), and 7 (example 18).

The results of 0.5h and 24h were combined and according to the requirements of 2007 "cosmetic hygiene code", the following conclusions were drawn: the extract of the invention has no adverse reaction to human skin, and can be used for treating the skin allergy.

Claims

1. The external plant extract with the effect of repairing skin barriers is characterized by being prepared from the following raw materials in parts by weight:

(2) extracting for the first time: mixing the raw material and the solvent I according to the feed-liquid ratio of 1: 10-100 m/m, and extracting at 40-90 ℃ for 0.5-2 h;

(3) and (3) second extraction: adding a second solvent according to the feed-liquid ratio of 1: 10-100 m/m, and extracting for 0.5-2 h at 40-90 ℃;

(4) removing the first solvent;

(5) fine filtering to obtain clear extract;

the first solvent is one or a mixture of ethanol, chloroform and acetone;

the second solvent is one or a mixture of more of white oil, hydrogenated polyisobutene, hydrogenated polydecene, caprylic/capric triglyceride, isostearyl isostearate and vegetable oil;

the kinematic viscosity of the white oil, the hydrogenated polyisobutene and the hydrogenated polydecene is less than or equal to 30cSt at 40 ℃.

2. The external plant extract with skin barrier repair effect according to claim 1, wherein the ratio of the material to the liquid in the step (2) is 1: 10-50 m/m.

3. The external plant extract with skin barrier repair effect according to claim 1, wherein the ratio of the material to the liquid in the step (3) is 1: 10-50 m/m.

4. The topical plant extract for skin barrier repair according to claim 1, wherein the concentration in step (4) is performed at 40-80 ℃ under reduced pressure until the first solvent is completely removed.

5. The extract of a plant for external use having skin barrier repair effect according to claim 1, wherein the fine filtration in step (5) is performed using a filter plate having a pore size of 0.2 to 10 μm.

6. The topical plant extract with skin barrier repair effect of claim 1, further comprising a cooling step of cooling to below 40 ℃ before the fine filtration in step (5).

7. The external plant extract with skin barrier repair effect according to any one of claims 1 to 6, further comprising 60-100 mesh coarse filtration between the step (3) and the step (4).

8. The topical plant extract with skin barrier repair effect of claim 7, further comprising a cooling step of cooling to below 40 ℃ before the coarse filtration.

9. The topical plant extract for skin barrier repair according to any one of claims 1 to 6, wherein the plant material is pretreated before the first extraction, and the pretreatment comprises the steps of:

(1) coarse crushing: crushing the raw materials to 20-60 meshes;

(2) high-temperature high-pressure treatment; the conditions of high temperature and high pressure are as follows: treating the coarsely crushed raw materials for 5-30 min at 100-130 ℃ under 0.1-0.2 MPa;

(3) and (5) drying.

10. The external plant extract with skin barrier repair effect according to claim 9, wherein the drying condition is drying at 50-80 ℃ for 1-2 h.

11. The topical plant extract for skin barrier repair according to claim 7, wherein the plant material is pretreated before the first extraction, and the pretreatment comprises the steps of:

(1) coarse crushing: crushing the raw materials to 20-60 meshes;

(2) high-temperature high-pressure treatment; the high-temperature high-pressure treatment conditions are as follows: treating the coarsely crushed raw materials for 5-30 min under the conditions of 0.1-0.2 MPa and 100-130 ℃;

(3) and (5) drying.

12. The external plant extract with skin barrier repair effect according to claim 11, wherein the drying condition is drying at 50-80 ℃ for 1-2 h.

13. Use of the plant extract according to any one of claims 1 to 6 for the preparation of a cosmetic having skin barrier repair efficacy.

14. Use of the plant extract of claim 7 for the preparation of a cosmetic having skin barrier repair efficacy.

15. A cosmetic having skin barrier repair effect, which is prepared from the plant extract according to any one of claims 1 to 6 and cosmetically acceptable adjuvants.

16. The cosmetic of claim 15, wherein the cosmetic is an oil-based cosmetic.

17. A cosmetic with skin barrier repairing effect is characterized in that the cosmetic is prepared from the plant extract as claimed in claim 7 and auxiliary materials commonly used in the field of cosmetics.

18. A cosmetic with skin barrier repairing effect is characterized in that the cosmetic is prepared from the plant extract as claimed in claim 8 and auxiliary materials commonly used in the field of cosmetics.

19. A cosmetic with skin barrier repairing effect is characterized in that the cosmetic is prepared from the plant extract as claimed in claim 9 and auxiliary materials commonly used in the field of cosmetics.

20. A cosmetic with skin barrier repairing effect is characterized in that the cosmetic is prepared from the plant extract as claimed in claim 12 and auxiliary materials commonly used in the field of cosmetics.

21. The cosmetic with the effect of repairing skin barriers is characterized by being prepared from the following raw materials in parts by weight:

1-4 parts of phytosterol ester, 0.2-0.5 part of bisabolol, 5-10 parts of sunflower seed oil, 5-10 parts of perilla seed oil, 65-85 parts of the plant extract as claimed in any one of claims 1-6, and 0.1-0.3 part of butylated hydroxytoluene.

22. A method of preparing the cosmetic of claim 21, comprising the steps of:

(1) weighing the raw materials according to the proportion of claim 21;

(2) adding phytosterol ester and butylated hydroxytoluene into the plant extract, heating and stirring at 50-60 ℃ to dissolve for 20-40 min;