CN110090180B

CN110090180B - Cosmetic lithospermum extract and preparation method thereof

Info

Publication number: CN110090180B
Application number: CN201910251358.4A
Authority: CN
Inventors: 董银卯; 琚瑶; 曲召辉
Original assignee: Taihe Kangmei Beijing Research Institute of Traditional Chinese Medicine Co Ltd
Current assignee: Taihe Kangmei Beijing Research Institute of Traditional Chinese Medicine Co Ltd
Priority date: 2019-03-29
Filing date: 2019-03-29
Publication date: 2021-05-07
Anticipated expiration: 2039-03-29
Also published as: CN110090180A

Abstract

The invention discloses a preparation method of a lithospermum extract for cosmetics, which comprises the following specific steps: (1) extracting for the first time: according to the ratio of material to liquid of 1:10: 1: mixing lithospermum raw materials and a first solvent at a speed of 100m/m, and extracting for 0.5-2 h at the temperature of 40-90 ℃; (2) and (3) second extraction: according to the ratio of material to liquid of 1: 10-1: adding a second solvent at the speed of 100m/m, and extracting for 0.5-2 h at the temperature of 40-90 ℃; (3) removing the first solvent; (4) fine filtering to obtain clear extract; wherein the first solvent is one or more of ethanol, petroleum ether and acetone; the second solvent is one or more of white oil, hydrogenated polyisobutene, hydrogenated polydecene, caprylic/capric triglyceride, isostearyl isostearate and vegetable oil. The method for effectively extracting the lithospermum raw material by using the double solvents with different polarities can greatly improve the product quality of the extract, so that the extract has excellent stability when being used as a cosmetic additive.

Description

Cosmetic lithospermum extract and preparation method thereof

Technical Field

The invention relates to a preparation method of a lithospermum extract for cosmetics, in particular to a preparation method of a lithospermum extract which can be added into cosmetics and can keep lasting and stable and an extract obtained by the method.

Background

Lithospermum erythrorhizon (a scientific name) is a perennial herb of the genus Lithospermum of the family Boraginaceae. The lithospermum is a common Chinese medicinal material in China, has cold property, and enters heart and liver meridians. Has the effects of clearing heat, cooling blood, promoting blood circulation, removing toxic substances, promoting eruption, removing ecchymoses and the like. The radix Arnebiae contains large amount of shikonin, which has antiinflammatory, immunity regulating, antibacterial and antiviral effects.

The application value of the lithospermum extract in the field of cosmetics is gradually concerned by technicians in the field, but the lithospermum extract is limited in the field of cosmetics at present, and the analysis reasons are as follows: (1) the extraction efficiency is too low, and the extraction cost is increased due to the too low extraction effect of the characteristics of the plant raw materials, so that a plurality of enterprises preferentially select the low-cost synthetic chemical raw materials to replace the natural plant raw materials so as to increase the 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. Particularly, for the application of oil type cosmetics, the oil type cosmetics are the cosmetic formulations which are currently sought after, but the oil type cosmetics have extremely high requirements on the clarity of products, and the quality and the performance of the products can be influenced once slight precipitation and precipitation occur. Therefore, the cosmetic enterprises urgently need a lithospermum extraction preparation process which is suitable for industrial production and has high extraction rate and good extract stability.

The existing preparation method of the lithospermum extract mainly 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, the ratio of the raw materials to the oil is about 1:3(v/v), the soaking is carried out at normal temperature, the materials need to be repeatedly fed for 2-3 times, and the soaking time needs to be 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

The steam distillation method 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, petroleum ether 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 supercritical fluid, generally supercritical CO, is used for extracting solvent²Has 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 above method still has many drawbacks. Meanwhile, 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 lithospermum extract which is used as a cosmetic additive and has excellent stability and product property.

The second purpose of the invention is to provide a preparation method of the lithospermum extract.

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

a preparation method of a lithospermum extract for cosmetics is disclosed, wherein the lithospermum extract is prepared by the following steps:

(1) extracting for the first time: according to the ratio of material to liquid of 1:10: 1: mixing lithospermum raw materials and a first solvent at a speed of 100m/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, petroleum ether 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 of the ratio of the first extraction liquid to the first extraction liquid is 1:10: 1:50m/m, the extraction effect is better in the range, and the cooperativity with the solvent II is stronger.

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 (1) are more suitable for cooperating with the step (2) which is described below, and the synergistic effect can be generated by the step (2).

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

(3) removing the first solvent;

(4) fine filtering to obtain clear extract;

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 dissolving technical effect of the first solvent and the second solvent is optimal, in order to ensure that the extraction efficiency is higher and the extraction cost is more economic when the two solvents are matched, the temperature and the time of the second extraction are controlled within the condition parameter range, the mutual dissolving and common extraction effect of the first solvent and the second solvent can be improved, and the problems that the extraction efficiency tends to be slow, the extraction cost is increased 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 (2), the preferable range of the ratio of the second extraction to the liquid is 1: 10-1: 50 m/m.

Removing the first solvent in the step (3); the solvent removal method known to those skilled in the art can be applied, and the preferred method proposed in this case is: 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.

Fine filtering in the step (4) to be clear; 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 (2) and the step (3), 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 lithospermum raw material can be pretreated before the first extraction, and the purpose of the pretreatment is to enable an extraction solvent to easily permeate cell walls and further improve the extraction efficiency. The step of pretreatment is not necessary, the high extraction rate of the invention mainly depends on the matching of the first solvent and the second solvent and the process steps and parameters used for the second solvent, and the pretreatment can further shorten the extraction time on the basis of the extraction rate achieved by the invention. 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 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 facilitated, and the stability of the extract is better, and the drying is preferably carried out for 1-2 hours at 50-80 ℃. Other drying means known to those skilled in the art may also be applied here.

A cosmetic radix Arnebiae extract is prepared by the above preparation method.

The beneficial results of the invention are as follows:

the method for effectively extracting the lithospermum raw material by using the double solvents with different polarities can greatly improve the quality of an extract product, so that the lithospermum raw material has excellent stability as a cosmetic additive, has better compatibility with various cosmetic formulation auxiliary materials, can be kept stable for a long time under the conditions of high-temperature and low-temperature illumination and the like when being particularly added into an oil formulation product with higher requirements on the extract, effectively improves the defects of the prior art that the quality and the efficacy of the product are influenced by the precipitation and the precipitation of the extract, and the like, so that the cosmetics are easier to store and transport, have better product quality and have better effect when being used. The method optimizes the extraction steps and the extraction condition parameters according to the optimized coordination of the extraction solvent and the selection of the specific solvent, greatly increases the extraction efficiency of the lithospermum, removes unpleasant odor of the lithospermum extract obtained by extraction in the prior art, and is suitable for adding cosmetics. The extraction method is calculated from the extraction parameters and the extraction cost, and is more suitable for industrial mass production.

Drawings

FIG. 1 is an experimental graph of antioxidant activity of samples 1-24;

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

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

FIG. 4 is a diagram of the extract of Lithospermum erythrorhizon obtained by different methods;

FIG. 5 is a chart showing the effect of the lithospermum extract of the present invention in the solubility test with different oils and fats.

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

TABLE 1 raw materials used in the present invention

TABLE 2 Equipment sources

Example 1

(1) Extracting for the first time: 20g of lithospermum raw material; adding anhydrous ethanol into radix Arnebiae at a material-to-liquid ratio of 1:10m/m, mixing, and extracting at 60 deg.C for 1.5 h;

(2) and (3) second extraction: adding sunflower seed oil according to the feed-liquid ratio of 1:10m/m, and stirring and extracting for 1.5h at the temperature of 60 ℃;

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

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

Example 2

(1) Extracting for the first time: 20g of lithospermum raw material; adding anhydrous petroleum ether according to the feed-liquid ratio of 1:50m/m, mixing, and extracting at 90 deg.C for 0.5 h;

(2) and (3) second extraction: adding white oil (7cSt) according to the feed-liquid ratio of 1:50m/m, and stirring and extracting at 90 ℃ for 0.5 h;

(3) concentrating under reduced pressure at 60 deg.C until petroleum ether is completely removed;

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

Example 3

(1) Extracting for the first time: 20g of lithospermum raw material; adding anhydrous acetone according to the feed-liquid ratio of 1:100m/m, mixing, and extracting at 40 deg.C for 2 h;

(2) and (3) second extraction: adding caprylic acid/capric acid triglyceride according to the feed-liquid ratio of 1:100m/m, and stirring and extracting for 2h at 40 ℃;

(3) concentrating under reduced pressure at 80 deg.C until anhydrous acetone is completely removed;

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

Example 4

(1) Coarse crushing: pulverizing radix Arnebiae to 40 mesh;

(2) high-temperature high-pressure treatment: treating at 120 deg.C under 0.2MPa for 20 min;

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

(5) extracting for the first time: adding absolute ethanol according to the feed-liquid ratio of 1:10m/m, mixing, and extracting at 60 deg.C for 1.5 h;

(6) and (3) second extraction: adding hydrogenated polyisobutene (20cSt) according to the feed-liquid ratio of 1:10m/m, and stirring and extracting for 1.5h at the temperature of 60 ℃;

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

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

Example 5

(1) Coarse crushing: pulverizing radix Arnebiae into 20 mesh;

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

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

(4) extracting for the first time: adding anhydrous acetone according to the feed-liquid ratio of 1:50m/m, mixing, and extracting at 90 deg.C for 0.5 h;

(5) and (3) second extraction: adding hydrogenated polydecene according to the feed-liquid ratio of 1:50m/m, and stirring and extracting for 0.5h at the temperature of 90 ℃;

(6) concentrating under reduced pressure at 60 deg.C until anhydrous acetone is completely removed;

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

Example 6

(1) Coarse crushing: crushing the lithospermum raw material into 60 meshes;

(2) high-temperature high-pressure treatment: treating at 130 deg.C under 0.1MPa for 5 min;

(4) and (3) drying: drying at 80 ℃ for 2 h;

(5) extracting for the first time: adding anhydrous petroleum ether according to the feed-liquid ratio of 1:100m/m, mixing, and extracting at 40 deg.C for 2 h;

(6) and (3) second extraction: adding isostearyl isostearate according to the feed-liquid ratio of 1:100m/m, and stirring and extracting for 2 hours at the temperature of 40 ℃;

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

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

Example 7

(1) Coarse crushing: pulverizing radix Arnebiae into 40 mesh, and mixing;

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

(3) and (3) drying: drying at 80 ℃ for 2 h;

(4) extracting for the first time: adding absolute ethanol according to the feed-liquid ratio of 1:70m/m, mixing, and extracting at 60 ℃ for 2 h;

(5) and (3) second extraction: adding soybean oil according to the feed-liquid ratio of 1:70m/m, and stirring and extracting for 2h at the temperature of 60 ℃;

(6) concentrating under reduced pressure at 60 deg.C until absolute ethanol is completely removed;

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

Example 8

(1) Coarse crushing: crushing the lithospermum raw material into 20 meshes;

(2) high-temperature high-pressure treatment: treating at 100 deg.C under 0.1MPa for 10 min;

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

(4) extracting for the first time: adding absolute ethanol according to the feed-liquid ratio of 1:20m/m, mixing, and extracting at 57 ℃ for 2 h;

(5) and (3) second extraction: adding caprylic acid/capric acid triglyceride according to the feed-liquid ratio of 1:20m/m, and stirring and extracting at 57 ℃ for 2 h;

(6) cooling to below 30 deg.C, and coarse-filtering with 100 mesh sieve;

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

(8) cooling to below 30 deg.C, filtering with filter plate having aperture of 0.45 μm, and fine filtering to obtain clear filtrate.

Example 9

(1) Coarse crushing: pulverizing radix Arnebiae into 40 mesh, and mixing;

(2) high-temperature high-pressure treatment: treating at 120 deg.C under 0.1MPa for 5 min;

(3) and (3) drying: drying at 70 deg.C for 1.5 h;

(4) extracting for the first time: adding a mixed solvent of absolute ethyl alcohol and absolute acetone (the absolute ethyl alcohol and the absolute acetone are compounded according to the mass ratio of 1: 1) according to the feed-liquid ratio of 1:40m/m, mixing, and extracting for 2 hours at the temperature of 60 ℃;

(5) and (3) second extraction: adding a caprylic/capric triglyceride and hydrogenated polyisobutene compound (the caprylic/capric triglyceride and the hydrogenated polyisobutene are compounded according to the mass ratio of 1: 1) according to the feed-liquid ratio of 1:40m/m, and stirring and extracting for 2 hours 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 0.2 μm, and fine filtering to obtain clear filtrate.

Example 10

(1) Coarse crushing: pulverizing radix Arnebiae into 20 mesh;

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

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

(5) extracting for the first time: adding anhydrous acetone and anhydrous petroleum ether mixed solvent (mixed according to the ratio of 1: 1) according to the feed-liquid ratio of 1:70m/m, mixing, and extracting at 90 ℃ for 2 h;

(6) and (3) second extraction: adding a hydrogenated polydecene and macadamia nut oil compound according to the feed-liquid ratio of 1:70m/m (the hydrogenated polydecene and the macadamia nut oil compound are mixed according to the mass ratio of 1: 1), and stirring and extracting for 2 hours at the temperature of 90 ℃;

(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

(1) Coarse crushing: pulverizing radix Arnebiae to 40 mesh;

(3) high-temperature high-pressure treatment: treating at 120 deg.C under 0.1MPa for 25 min;

(4) and (3) drying: drying at 50 deg.C for 2 h;

(5) extracting for the first time: adding a mixed solvent of absolute ethyl alcohol and absolute petroleum ether (the absolute ethyl alcohol and the absolute petroleum ether are compounded according to the mass ratio of 1: 1) according to the feed-liquid ratio of 1:20m/m, mixing, and extracting for 1.5 hours at the temperature of 60 ℃;

(6) and (3) second extraction: adding a mixed solvent of white oil (16cSt) and isostearyl isostearate (the two are compounded according to the mass ratio of 1: 1) according to the feed-liquid ratio of 1:20m/m, and stirring and extracting for 1.5h at the temperature of 60 ℃;

(7) cooling to below 40 deg.C, and coarse filtering with 60 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 having pore diameter of 4 μm, and fine filtering to obtain clear filtrate.

Example 12

(1) Coarse crushing: pulverizing radix Arnebiae into 100 mesh;

(3) high-temperature high-pressure treatment: treating at 110 deg.C under 0.1MPa for 15 min;

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

(5) extracting for the first time: adding absolute ethanol according to the feed-liquid ratio of 1:50m/m, mixing, and extracting at 80 deg.C for 1.5 h;

(6) and (3) second extraction: adding a mixed solvent of sweet almond oil and oat oil (the two are compounded according to the mass ratio of 1: 1) according to the material-liquid ratio of 1:50m/m, and stirring and extracting for 1.5h at the temperature of 80 ℃;

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

(9) cooling to below 40 deg.C, filtering with filter plate having aperture of 0.2 μm, and fine filtering to obtain clear filtrate.

Example 13

(1) Coarse crushing: pulverizing radix Arnebiae to 40 mesh;

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

(4) and (3) drying: drying at 80 deg.C for 1 h;

(5) extracting for the first time: adding anhydrous petroleum ether according to the feed-liquid ratio of 1:30m/m, mixing, and extracting at 55 deg.C for 1 h;

(6) and (3) second extraction: adding grape seed oil according to the feed-liquid ratio of 1:30m/m, and stirring and extracting for 1h at the temperature of 55 ℃;

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

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

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 petroleum ether. The inventor considers that the technical effect already meets the requirement of the present application, 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 the solvent screening experiment part, namely samples 1-24 selected by the solvent. The raw materials of the samples 1-24 are all lithospermum, the preparation method is the same, and only the extraction solvents are different.

The preparation method of the sample 1-24 comprises the following steps:

(1) coarse crushing: crushing the lithospermum raw material into 20 meshes, and uniformly mixing;

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

(4) extracting for the first time: adding a first solvent according to the feed-liquid ratio of 1:20m/m, mixing, and extracting at 57 ℃ for 2 hours;

(5) and (3) second extraction: adding a second solvent according to the feed-liquid ratio of 1:20m/m, and stirring and extracting for 2 hours at the temperature of 57 ℃;

(6) cooling to below 30 deg.C, and coarse-filtering with 100 mesh sieve;

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

(8) cooling to below 30 deg.C, filtering with filter plate having aperture of 0.45 μm, and fine filtering to obtain clear filtrate. The solvents used for samples 1-24 are shown in Table 3.

TABLE 3 sample solvent table

Sample number	Solvent one	Solvent II
			1	Petroleum ether	Sunflower seed oil
2	Ethanol	Sunflower seed oil
			3	Acetone (II)	Sunflower seed oil
4	Petroleum ether	Caprylic/capric triglyceride
			5	Ethanol	Caprylic/capric triglyceride
6	Acetone (II)	Caprylic/capric triglyceride
			7	Petroleum ether	Isostearyl isostearate
8	Ethanol	Isostearyl isostearate
			9	Acetone (II)	Isostearyl isostearate
10	Petroleum ether	White oil (26cSt)
			11	Ethanol	White oil (26cSt)
12	Acetone (II)	White oil (26cSt)
			13	Petroleum ether	White oil (32cSt)
14	Ethanol	White oil (32cSt)
			15	Acetone (II)	White oil (32cSt)
16	Petroleum ether	Hydrogenated polydecene (30cSt)
			17	Ethanol	Hydrogenated polydecene (30cSt)
18	Acetone (II)	Hydrogenated polydecene (30cSt)
			19	Petroleum ether	Hydrogenated polydecene (46cSt)
20	Ethanol	Hydrogenated polydecene (46cSt)
			21	Acetone (II)	Hydrogenated polydecene (46cSt)
22	Petroleum ether	Polydimethylsiloxane (PMX200, 6cSt)
			23	Ethanol	Polydimethylsiloxane (PMX200, 6cSt)
24	Acetone (II)	Polydimethylsiloxane (PMX200, 6cSt)

3. And (3) testing results:

the content of the part is to screen a second solvent, wherein the first solvent is fixed into ethanol, petroleum ether 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.

(2) Stability experiments, see table 4.

TABLE 4 comparison of stability of different solvent extracts

II, experimental results:

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 petroleum ether, 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 petroleum ether respectively in a compounding manner, and have good extraction effects.

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

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 petroleum ether, and all have better extraction effects.

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 petroleum ether, 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 petroleum ether 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 petroleum ether 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 22-24 are prepared by compounding and extracting polydimethylsiloxane (silicone oil, PMX200, 6cSt) with ethanol, acetone and petroleum ether 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 second solvent of the present invention further comprises white oil (samples 13 to 15) having a kinematic viscosity (40 ℃) of more than 30cSt, hydrogenated polydecene (samples 19 to 21) having a kinematic viscosity (40 ℃) of more than 30cSt, and 6cSt polydimethylsiloxane PMX200 (samples 22 to 24). According to the experiments, the vegetable oil, the caprylic/capric triglyceride, the isostearyl isostearate, the white oil with the kinematic viscosity (40 ℃) of less than or equal to 30cSt, the hydrogenated polyisobutene and the hydrogenated polydecene all have good extraction effects by respectively carrying out compound extraction with the solvent I (ethanol, acetone and petroleum ether), 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.

Thirdly, determining extraction parameters

1. Second extraction temperature selection experiment: the second step is the synergistic extraction of the solvent and the solvent, so the extraction in the step is very important, and the extraction temperature in the second 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 preparation process comprises the following specific steps:

(1) weighing 50g of lithospermum;

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

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

(5) and (3) second extraction: adding caprylic acid/capric acid triglyceride according to the feed-liquid ratio of 1:20m/m, wherein the extraction temperature is shown in Table 5, and stirring and extracting for 2 h;

(6) cooling to below 30 deg.C, and coarse-filtering with 100 mesh sieve;

TABLE 5

Sample number	Step (5) extraction temperature
		25	35℃
26	40℃
		27	57℃
28	75℃
		29	90℃
30	95℃

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 when the temperature of the extract is between 40 and 90 ℃, and is too low when 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 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 ℃, 57 ℃, 75 ℃, 90 ℃ and 95 ℃, the DPPH and the stability of the product are better, the extraction effect at the temperature of 40-90 ℃ is poor, the extraction effect at the temperature of 95 ℃ is poor, the stability of the product is poor due to overhigh temperature, discoloration and peculiar smell occur, therefore, the final extraction temperature is recommended to be in the range of 40-90 ℃, and the measured DPPH value is 57 ℃ highest under the condition of consistent stability, and the optimal extraction temperature in the invention is 57 ℃.

2. And (3) extracting the material-liquid ratio experiment for the second time: the second step is the synergic extraction of the solvent I and the solvent II, the extraction in the step is crucial, the extraction material-liquid ratio in the second step directly influences the intersolubility of the solvent I and the solvent II, and the extraction efficiency of the extraction is matched

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

(1) weighing 50g of lithospermum;

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

(4) extracting for the first time: adding ethanol according to the feed-liquid ratio of 1:20m/m, mixing, and extracting at 57 deg.C for 2 h;

(5) and (3) second extraction: adding caprylic capric triglyceride according to the material-liquid ratio in the table 7, extracting at the temperature of 57 ℃, and stirring and extracting for 1 h;

(6) cooling to below 30 deg.C, and coarse-filtering with 100 mesh sieve;

TABLE 7

Sample number	Material to liquid ratio in step (4)
		31	1:2
32	1:10
		33	1:20
34	1:50
		35	1:100
36	1:150

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. Therefore, the ratio of the materials to the liquid is 1: 10-1: 100, the extraction efficiency is high, and the extraction ratio is 1: 20-1: 50 the extraction efficiency is best.

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

The main component of the lithospermum is alkannin which is a natural pigment, so that the content of the alkannin can be judged to be more or less from the color depth, and then the extracted lithospermum extract is subjected to the determination of the content of the alkannin. Quantitative analysis the differences between different methods for extracting shikonin.

In the experiment, the lithospermum extract prepared in the embodiment 8 of the invention is compared with the comparative examples, four comparative examples for extracting the lithospermum extract in the prior art are set in the experiment, and the preparation process and the parameters of the comparative examples are as follows:

comparative example 1

(1) Selecting foreign matters from radix Arnebiae, and pulverizing into powder with JP-400B-8 type high-speed multifunctional pulverizer;

(2) oil extraction: weighing 20g of lithospermum, extracting 400g of caprylic acid/capric acid triglyceride according to the material-liquid ratio of 1:20m/m for 2h under stirring at 57 ℃;

(3) the aperture of the filter plate is 0.45 mu m, and the filter plate is finely filtered until the filtrate is clear, so that a sample is obtained.

Comparative example 2

(2) high-temperature high-pressure treatment: treating at 121 deg.C under 0.1MPa for 10 min;

(3) and (3) drying: drying at 40 deg.C for 1.5 h;

(4) oil extraction: weighing 20g of lithospermum, extracting 400g of caprylic acid/capric acid triglyceride according to the material-liquid ratio of 1:20m/m for 2h under stirring at 57 ℃;

(5) the aperture of the filter plate is 0.45 mu m, and the filter plate is finely filtered until the filtrate is clear, so that a sample is obtained.

Comparative example 3

(2) oil extraction: weighing 20g of lithospermum, extracting 400g of caprylic acid/capric acid triglyceride according to the material-liquid ratio of 1:20m/m for 2h under stirring at 120 ℃;

Comparative example 4

(2) solvent extraction: weighing 20g of lithospermum, extracting 400g of absolute ethanol according to the material-liquid ratio of 1:20m/m for 2 hours under stirring at 60 ℃;

The experimental results are as follows: the extract of Lithospermum erythrorhizon obtained by different methods is shown in FIG. 4, and the content of alkannin is shown in Table 8. The content of the alkannin in the example 8 is equivalent to that in the comparative example 4, is much higher than that in the comparative examples 1-3, and is respectively 2.8 times, 2.5 times and 1.6 times of those in the comparative examples 1, 2.5 times and 3 times, so that the alkannin extraction efficiency can be obviously improved. Comparative example 4 has a high extraction rate, but the extract has unpleasant odor, which severely limits the use of the extract of lithospermum erythrorhizon in cosmetics. On the premise of ensuring the extraction efficiency, the solvent I and the solvent II are matched with each other to selectively extract the alkannin and eliminate bad flavor substances, and the obtained extract keeps the characteristic smell of the lithospermum extract without other bad smells, thereby being greatly convenient for the application of the extract in cosmetics.

TABLE 8 comparison of the results of the different methods for extracting arnebia euchroma (Royle) Johnston samples

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

1. For comparing stability in oil type cosmetics

(1) The experimental method comprises the following steps: 30.0g of sample liquid and 270.0g of oil which is a common auxiliary material of oil cosmetics, heating to about 50 ℃, stirring to dissolve for 20min, standing and cooling for 1h, and observing the dissolution condition of the sample in the 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. The prepared samples were equally divided into five portions, placed in dark (room temperature cassette), refrigerated (4 ℃ freezer), illuminated (28 ℃ light incubator), hot (45 ℃ oven), frozen (-15 ℃ freezer) and recorded for 30 days stability.

(2) The sample preparation process comprises the following steps: same as the five experimental samples.

TABLE 9 comparison of stability of samples from different processes

(3) And (4) experimental conclusion: as shown in table 9.

Sample 1 (comparative example 1) itself was a fat extract, and therefore turbidity was excellent in the oily cosmetic adjuvant, and it was found in the 30-day stability test that it had a small amount of precipitate and had a slight odor indicating sample deterioration; when the sample 2 (comparative example 2) is pretreated, the adopted pressure is too high, so that the compatibility of the extracted lithospermum oil and the oil is poor, and precipitates and peculiar smell are generated in a stability experiment for 30 days, which indicates that the sample is deteriorated; the extraction temperature of the sample 3 (comparative example 3) is 120 ℃, the extraction temperature is too high, so that the compatibility of the extracted lithospermum oil and the oil is poor, and a large amount of precipitates and peculiar smell are generated in a stability experiment for 30 days, which indicates that the sample is deteriorated; sample 4 (comparative example 4) was an alcohol-soluble extract and had poor compatibility with fats and oils, and a large amount of precipitates were observed in the 30-day stability test, indicating that the stability of the sample was poor. Sample 5 (example 8) was extracted using solvent one and solvent two in combination, and the extraction process was optimized, resulting in good compatibility of the active ingredient with oils and fats, which are common adjuvants for cosmetics. The stability test for 30 days shows that the appearance is clear and transparent, and the smell is normal, which shows that the stability of the extract oil type cosmetic additive prepared by the scheme is superior to that of the

samples

1, 2, 3 and 4. Even better than the extracts obtained by oil extraction.

The same comparison was made by the inventors with other examples of the invention, leading to the same conclusions.

2. The lithospermum extract of the invention is compatible with different oils and fats

The experimental method comprises the following steps: the lithospermum extract prepared in the embodiment 8 of the invention is respectively dissolved in 10 kinds of auxiliary grease commonly used in the market, and the product stability is observed for 30 days under the condition. The 10 auxiliary greases were: octyl methicone, olive oil, isohexadecane, macadamia oil, ethylhexyl palmitate, isononyl isononanoate, white oil, isostearyl isostearate, polydimethylsiloxane, hydrogenated polyisobutene.

The experimental results are as follows: as shown in fig. 5, fig. 5 is a graph showing that whether or not the phenomena of delamination, precipitation, impurities, etc. occur after 30 days of adding the lithospermum extract can be visually observed, and fig. 5 is an auxiliary oil map after adding the lithospermum extract. Observation results of 30 days after the lithospermum extract is added show that no precipitation, delamination, impurities and the like occur, and the color is clear and transparent, which shows that the stability of the lithospermum extract added into the oil-taking type skin care product is good.

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

According to the following table, under the conditions of the same feed-liquid ratio, extraction temperature and extraction time, the content of the alkannin in the embodiment 8 of the invention is far higher than that in the comparative examples 1-3. If the same alkannin content is to be achieved, theoretically, when the extraction temperature and the extraction time are not changed, the ratio of the material to the liquid is at least increased to 1: 7; when the ratio of material to liquid and the extraction time are not changed, the extraction temperature may need to reach 150-180 ℃; when the ratio of the material to the liquid and the extraction temperature are not changed, the extraction time needs to be prolonged to 4-6 h. Therefore, the preparation method is more suitable for industrial mass production. Since the extract of comparative example 4 has unpleasant odor, it is excluded from the preparation of cosmetic extracts, and if it is desired to add it as a cosmetic, it is necessary to perform deodorization treatment, which often has a low success rate, and if it is successfully deodorized, the active ingredients of the arnebia root extract will be greatly lost, and the deodorization process will increase the preparation cost and time.

TABLE 10 comparison of Process parameters/costs for different extraction methods

Seventh, the efficacy experiment of the oil type cosmetics prepared by the invention

1. The test method comprises the following steps: selecting 10 (8-10 weeks) male nude mice with different sizes, and randomly classifying the mice into 1#2#3#4#5#6#7#8 #; firstly, 3cm by 3cm test parts of the skin on the left side and the right side of a nude mouse are continuously pasted and quickly torn off for a plurality of times by using an adhesive tape until the skin has a small blood spot, and the sticking and tearing are stopped. Immediately dissecting skin tissues of a test part in the model group and the normal group, and taking a picture of pathological section microscopic examination; smearing samples on each sample group respectively, smearing the samples once a day, continuously smearing the samples for four days, killing animals, dissecting skin tissues of a test part, and taking a photograph of pathological section microscopic examination; the control group was not smeared with any sample, and four days later, the animals were sacrificed and dissected to take skin tissues of the test sites, and pathological section microscopic examination was performed to take a photograph.

2. Test conditions laboratory temperature: relative humidity at 20-24 ℃: 60 to 70 percent

3. Test samples: the lithospermum extract of the embodiment 8 of the invention is added into the samples 1-4, and the addition amount is shown in a table 11; and 5-8 adding the lithospermum extract in the comparative example.

The formula and preparation process of the emulsion used in the test

TABLE 11 emulsion formulation

The preparation process of the emulsion for the test comprises the following steps:

(1) preparing in advance: preparing the F-phase sodium hydroxide into a 10% aqueous solution in advance;

(2) adding carbomer 940 into water for soaking phase A, and rapidly stirring to completely hydrate carbomer 940;

(3) adding B phase KELTROL CG-T into glycerol and butanediol, stirring, slowly adding water, and stirring;

(4) adding the phase B and the phase C into the phase A, uniformly stirring, and heating the phase A to 55-60 ℃ for later use;

(5) uniformly mixing the phase D raw materials, and heating to 80-85 ℃ to completely dissolve the phase D raw materials;

(6) stirring phase D, cooling to 55-60 deg.C;

(7) homogenizing phase A (3000 rpm), adding D, E into phase A, and homogenizing for 5 min;

(8) stirring at 55-60 deg.C for half an hour;

(9) stirring and cooling, adding phase F at 50-55 deg.C, neutralizing to pH 5.0-5.5, and stirring;

(10) adding the G-phase raw material at the temperature of below 45 ℃, and uniformly stirring;

(11) filtering and discharging at the temperature below 38 ℃.

4. And (3) test results:

TABLE 12 Effect of different samples on skin Barrier Damage repair

As can be seen from the above table, the lithospermum extract of the invention has obvious repairing effect on the cuticle of the epidermis of the skin.

Claims

1. A preparation method of a lithospermum extract for cosmetics is characterized by comprising the following steps:

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

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

(3) removing the first solvent;

(4) fine filtering to obtain clear extract;

the first solvent is one or a mixture of ethanol, petroleum ether 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 ℃;

the lithospermum erythrorhizon is pretreated before the first extraction, and the pretreatment comprises the following steps:

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

(2) high-temperature high-pressure treatment;

(3) drying;

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; the drying condition is drying for 1-2 h at 50-80 ℃.

2. The method according to claim 1, wherein the fine filtration in step (4) further comprises a cooling step of cooling to a temperature of 40 ℃ or lower.

3. The preparation method according to any one of claims 1 or 2, characterized by further comprising 60-100 mesh coarse filtration between the step (2) and the step (3).

4. A method as claimed in claim 3, wherein the straining is preceded by a cooling step to below 40 ℃.

5. A cosmetic comfrey extract characterized in that the extract is prepared by the preparation method according to any one of claims 1 to 4.