CN109512732A

CN109512732A - Have effects that repair exterior-applied plant extract, cosmetics of skin barrier and preparation method thereof

Info

Publication number: CN109512732A
Application number: CN201711194842.5A
Authority: CN
Inventors: 董银卯; 孟宏; 刘宇红; 曲召辉
Original assignee: Beijing Orient Miao Sen Bio Tech Ltd
Current assignee: Beijing Orient Miao Sen Bio Tech Ltd
Priority date: 2017-11-24
Filing date: 2017-11-24
Publication date: 2019-03-26
Anticipated expiration: 2037-11-24
Also published as: CN109512732B

Abstract

Have effects that repair the exterior-applied plant extract of skin barrier the invention discloses a kind of.The exterior-applied plant extract is prepared by the raw material that following weight parts match through following methods: (1) weighing each raw material according to following weight parts proportion, mix；Safflower 1~10, gardenia 1~10, FLOS CHRYSANTHEMI ALBA from Haizhou of China 1~10, armeniaca mume 1~10；(2) it extracts for the first time: being 1:10~100m/m mixed raw material and solvent one according to solid-liquid ratio, extract 0.5~2h under the conditions of 40~90 DEG C；(3) it extracts for second: being that solvent two is added in 1:10~100m/m according to solid-liquid ratio, extract 0.5~2h under the conditions of 40~90 DEG C；(4) solvent one is removed；(5) refined filtration is to clarification to get extract；Solvent one is one of ethyl alcohol, chloroform and acetone or a variety of mixing；Solvent two is one of white oil, Parleam, Nexbase 2004, caprylic/capric triglyceride, isostearyl isostearate ester and vegetable oil or a variety of mixing.

Description

Have effects that repair exterior-applied plant extract, cosmetics and its preparation of skin barrier Method

Technical field

The present invention relates to a kind of exterior-applied plant extracts, specifically a kind of to have effects that repair the external application of skin barrier Plant extracts, efficient preparation method and the cosmetics being prepared by the plant extracts.

Background technique

Skin covers human body surface, is the first line of defence of human body.The skin of health has both sides barrier action: (1) External mechanical, physical, the chemically entrance with biological nuisance, stimulant etc. are resisted, is protected intracorporal each important Internal organs；(2) loss for preventing endotrophic substance, moisture etc. maintains the water content of skin, makes skin moisturizing.

However, when skin is stimulated by sunlight, ultraviolet radiation or cosmetics, drug (such as hormone) and other factors When, it will lead to skin barrier and be damaged, so that skin self-defense scarce capacity, to occur as epidermal barrier function is impaired, hair The problems such as thin blood vessel dilatation, inflammation thinning of skin, flush, pigmentation.

The main method for repairing skin barrier function at present is using moisturizer, and skin moisturizer mainly has grease envelope at present Moisturizer, hydrophilic matrix moisture-absorption humectant, hydration moisturizer etc. are closed, but simple moisturizing can not fundamentally solve impaired skin Reparation problem after skin barrier function damage.

Plant extracts has many advantages as cosmetic additive agent, as plant extracts ingredient is natural, irritation is low and Effect brilliance etc., therefore, plant extracts as functional additive in cosmetics using increasing.In plant material Functional component has the oil-soluble ingredients such as fatty acid, sterol, lignanoid, esters, polyenoid class, azole derivatives, ketone, quinones, removes It can also be containing some as the non-oil soluble material such as carbohydrate, amino acid, protein except this.Plant extracts is led in cosmetics at present Domain applies the main reason for stranded to have (1) extraction efficiency too low, and due to the characteristic of plant material, extraction effect is too low to be caused to extract The increase of cost, therefore many enterprises preferentially select the synthesis chemical raw material of low cost to replace natural plant raw material, to increase Economic benefit.(2) stability of plant material extract is bad.Plant material is in being added to each dosage form of cosmetics, often surely It is qualitative bad, easily occur in storage and transportational process it is rotten, be precipitated or the phenomenon that precipitating, not only make product rate increase of addling At increased costs, effect also will have a direct impact on, consumer's use feeling is caused to decline.Come especially for oil-type cosmetics Say, oil-type cosmetics have high requirement to clarity, once occur it is slight be precipitated and precipitating will affect product quality and Performance.Therefore Management of Cosmetics Enterprises is badly in need of the plant a kind of suitable for industrial, recovery rate is high, extract stability is good at present Extract preparation process.

The extracting method of existing plant material functional component is described below, current existing preparation process has following several:

1. soak extraction

Flowers and plants, which impregnate oil, has long applicating history, and ancient Egyptian and Greeks have learned with fat absorption petal With the smell of medicinal herbs, used as drug or cosmetics.The common vegetable oil of oil is impregnated as solvent, and the ratio of raw material and grease is about For 1:3 (v/v), soak at room temperature needs to feed intake repeatedly 2~3 times, and soaking time needs 1~3 month.Oil is impregnated in cosmetics oil There is preferable compatibility when using in dosage form, but such method extraction efficiency is low, and extraction time is longer to be unfavorable for industrial production.

2. the direct high temperature of grease extracts

In the ancient books such as Prescriptions for Universal Relief, peaceful holy benevolent prescriptions, many ointment are described, coke is decocted with Chinese medicine and oil, rouge and goes dregs, for controlling Treat skin disease or beauty.So far civil still to remain many classical prescriptions, proved recipe, sesame oil is heated into decocting herb and obtains medicine oil, is used In the various malaise symptoms for alleviating skin.So being decocted using the direct high temperature of grease is also one of traditional extraction process, but this Kind of method is more original, extraction efficiency is low, cannot effectively extract active constituent in plant, and time-consuming, and material waste is serious, mentions Low efficiency etc. is taken seriously to constrain industrialized production.

3. steam distillation

It is that plants essential oil extracts common method, but such method is only applicable to extract fragrance in plant that vapor, which steams method, The effumability ingredient of class, then can not extraction and application without volatile component.

4. extract by solvents

Solvent extraction is to produce the common method of plant extracts, generally using ethyl alcohol, acetone, chloroform etc. as solvent, tool There is the features such as equipment is simple, and recovery rate is high.But the extract of the method preparation, it is more demanding to State of cosmetics, be not suitable for adding All dosage forms are added, the especially dissolubility in oil-type cosmetics is poor, so that pure finish makeup is added in plant extracts Precipitation is had after in product, seriously affects product quality, constrains its application in pure oil-type cosmetics.

5. means of supercritical extraction

Means of supercritical extraction is the new technology risen in recent years, supercritical fluid, generally supercritical CO when Extraction solvent², tool There is the advantages that nontoxic, recovery rate is high, and extract purity is high.But the device is complicated, input cost is high, and extraction cost is high, so that Industrial mass production is limited.And the extract that means of supercritical extraction obtains influences it in oil generally with the poor compatibility of grease Application in dosage form cosmetics.

There are many defects for above-mentioned existing method, meanwhile, it is limited by extraction efficiency, preparation cost is excessively high, organic solvent The problems such as discharge causes environmental pollution also increasingly highlights.Therefore, this field is badly in need of solving above-mentioned for cosmetics and care product The problem of plant extracts preparation of addition.

Summary of the invention

The primary purpose of the present invention is that propose it is a kind of have effects that repair skin barrier plant prescription and its preparation side Method, and obtained plant extracts.

The second object of the present invention is the plant extracts preparation side for proposing that a kind of recovery rate is high, extract property is stable Method.

The third object of the present invention is the cosmetics for proposing to be prepared by above-mentioned plant extracts.

Invention thinking of the invention are as follows: the composition that the present invention selects utilizes the principles of formulating prescriptions of " monarch minister, helps, makes ", by four Kind plant material carries out compatibility, and collaboration works between each raw material and cooperation new preparation method of the invention can play excellent repair The effect of multiple skin barrier, raising tolerance of skin.

To achieve the purpose of the present invention, the present invention adopts the following technical scheme:

It is a kind of to have effects that repair the exterior-applied plant extract of skin barrier, wherein the exterior-applied plant extract is under The raw material for stating weight is prepared through following methods:

(1) each raw material is weighed according to following weight parts proportion, mixed；

Safflower 1~10, gardenia 1~10, FLOS CHRYSANTHEMI ALBA from Haizhou of China 1~10, armeniaca mume 1~10；

(2) it extracts for the first time: being 1:10~100m/m mixed raw material and solvent one according to solid-liquid ratio, under the conditions of 40~90 DEG C Extract 0.5~2h；

Solvent for use one of the present invention is one of ethyl alcohol, chloroform and acetone or a variety of mixing.

Solid-liquid ratio and Extracting temperature have vital influence to extraction efficiency and extraction cost, for Extraction solvent one Extraction efficiency not only can be improved with its more matched solid-liquid ratio and extracting parameter in physicochemical property selection, can also enhance and lower step The concertedness that solvent two extracts.Solid-liquid ratio range interplantation raw material of the present invention contacted with solvent one it is more abundant, in plant material Active constituent is easier to be extracted, and extraction efficiency is higher while not will cause the waste of solvent and plant material, and extraction cost is more It is economical.The preferred solid-liquid ratio value range that extracts for the first time is 1:10~50m/m, and extraction effect is more preferable within the scope of this, and and solvent Two concertednesses are stronger.

0.5~2h is extracted under the conditions of Extracting temperature of the present invention and preferably 40~90 DEG C of the time.Extracting temperature and time are direct Extract property is influenced, inappropriate Extracting temperature and time may cause the oxidative deformation of plant material in extraction process, waves Loss of hair property ingredient and heat-sensitive ingredients property change etc., within the scope of this dissolubility of extract functional component in solvent and Mass exchange rate is best, and extract effect is excellent and stablizes.

The conditional parameter of above-mentioned steps (2) cooperates more suitable for following step (3), can generate with step (3) synergistic The effect of.

(3) it extracts for second: being that solvent two is added in 1:10~100m/m according to solid-liquid ratio, extracted under the conditions of 40~90 DEG C 0.5~2h；

Solvent for use two of the present invention is one of following raw materials or a variety of mixing, is respectively: white oil, kinematic viscosity (40 DEG C)≤30cSt recommends to use white oil 3#, 5#, 7#, 10#, 15#, 26#；Parleam, kinematic viscosity (40 DEG C)≤ 30cSt recommends to use Parleam Parleam 6, Parleam EX；Nexbase 2004, kinematic viscosity (40 DEG C)≤ 30cSt recommends to use Nexbase 2004 PAO2, PAO4, PAO6；Caprylic/capric triglyceride, isostearyl isostearate ester and Vegetable oil.Vegetable oil is recommended to use soybean oil, sunflower seed oil, sesame oil, macadimia nut oil, Sweet Almond Oil, olive oil, grape One of seed oil, oat oil, tea oil or a variety of mixing.

The cooperation of solvent two and solvent one is particularly important to the technology of the present invention effect, inventor experiments verify that, two solvents Between cannot dissolve each other completely, although preferable extraction efficiency can be guaranteed completely by dissolving each other, be added in cosmetics stability not It is good, easily there is a problem that precipitating is precipitated.Two solvents can not be completely immiscible, and two solvents are immiscible, cannot play collaboration The effect of synergy, extraction efficiency is very low and extract stability is poor.Therefore two partial miscibility technical effect of solvent one and solvent Most preferably, in order to keep the two solvents cooperation higher extraction cost of extraction efficiency more economical, temperature that inventor extracts second and when Between control in above-mentioned condition parameter area, can not only improve solvent one simultaneously and what two partial miscibility of solvent extracted jointly mentions Effect is taken, effectively extraction efficiency can also be avoided to tend to the problems such as being slowly increased extraction cost.According to two characteristic of solvent, temperature is extracted Degree is unsuitable excessively high, and control is best at 90 DEG C or less, and temperature is also unsuitable too low, will affect functional component lower than 40 DEG C in solvent two Dissolubility and solvent one and solvent two intermiscibility, and then influence extraction efficiency.

According to the description of the above method, the selection of solvent one and solvent two is particularly important, and the two cooperation needs synergy The extraction efficiency of plant material is improved, and in order to adapt to industrial production, extraction process need to be short, extract quality needs high to be to add Stability is good, and extraction cost also needs lower.Therefore, inventor is experiments verify that have found, if two pole of solvent of the present invention Property be greater than solvent one, extraction efficiency and extract stability are poor.Inventor it is pleasantly surprised have been found that solvent one than solvent two Polarity is stronger, solvent one and solvent two under certain condition can partial miscibility, this feature can enhance active constituent in solvent two Dissolubility so that certain scripts do not dissolve in grease, or in grease the substance of dissolubility difference can be good at being dissolved in it is molten In agent two.The two cooperation is extracted, and can be met all conditions needed for above-mentioned cosmetics plant material extracts, be greatly improved The extraction efficiency of active components of plants, obtained extract property are stablized, other raw material compatibility are splendid with cosmetics.

The present invention can choose one of all multi-solvents of above-mentioned record and carry out single solvent extraction, can also be according to reality The compounding that the plant material characteristic that border is extracted carries out multi-solvent is extracted, and compound proportion can be according to those skilled in the art between solvent Member's experience or actual needs arbitrary proportion compounding, limit without specific.Because of the characteristic of solvent two, stability of the water to solvent two Influence it is huge, so the preferred anhydrous system of solvent one, by taking ethyl alcohol as an example, preferred dehydrated alcohol.

The Extraction solvent that solvent two of the present invention selects polarity weak compared with solvent one, it is mild non-stimulated, with the function in plant material It is good to imitate COMPONENTS COMPATIBILITY.Solvent two can choose one of all multi-solvents of above-mentioned record and carry out single solvent extraction, can also It is extracted with carrying out the compounding of multi-solvent according to the plant material characteristic of actual extracting, compound proportion can be according to ability between solvent Field technique personnel experience or actual needs arbitrary proportion compounding, limit without specific.

It is 1:10~50m/m that second, which is extracted solid-liquid ratio preferred range value, in above-mentioned steps (3).

(4) solvent one is removed；Well known to a person skilled in the art the methods of removable solvent can be applicable to this, the present invention The preferred approach of recommendation is: being concentrated under reduced pressure into solvent one at 40~80 DEG C and completely removes, pressure relief ranges general control is in 0.01Mpa To negative 0.15Mpa.Solvent one may have certain irritation to skin, and removal solvent one can make properties of product milder, pacify Completely without toxic side effect.Solvent one can also be removed using modes such as film concentration, ultrafiltration, reverse osmosis, seepage slopes.

(5) refined filtration is extremely clarified；The purpose of this step is to make the more stable clarification of final extract, and refined filtration process uses The filter plate in 0.2~10 μm of aperture is filtered.

In order to be more advantageous to the progress of above-mentioned reduced pressure and refined filtration step, and preferably protection reduced pressure and refined filtration Equipment can also increase coarse filtration step between step (3) and step (4), and the condition of coarse filtration is 60~100 mesh coarse filtration, filter off Raw material slag.In order to keep the stabilization of filtering feed liquid, cooling step can also be increased before coarse filtration, feed liquid is cooled to 40 DEG C or 40 DEG C or less to carry out coarse filtration again best.

Plant material can also be pre-processed before first time extracts, and pretreated purpose is to make Extraction solvent More easily permeation cell wall further increases extraction efficiency.Pretreated step is not required, and recovery rate of the present invention is high main Depending on the cooperation of solvent one and solvent two and for processing step and parameter used in solvent one or two, pretreatment can be Further shorten extraction time on the basis of present invention recovery rate achieved, but for being not easy to pretreated plant material Pre-treatment step can not used.Inventor recommend it is pretreated steps are as follows states, well known to other skilled in the art The step of pretreatment purpose can be achieved can also be applied to this.

(1) raw material coarse crushing: is crushed to 20~60 mesh；Pulverising step can using disintegrating apparatus well known in the art into Row, such as cutting machine, wall-breaking machine, pulverizer, pulverising step can be completed disposably, can also be step by step by slightly to carefully gradually complete At.

(2) high temperature high pressure process, high temperature described herein are generally at least the temperature equal to or higher than 100 DEG C, the present invention Control is advisable at 100~130 DEG C.High pressure refers to 0.1Mpa or more, and control effect within the scope of 0.1~0.2Mpa is best.When processing Between it is unsuitable too long, control is preferred within 30min.The main component of plant cell wall is cellulose and pectin, and the present invention uses High temperature and pressure pretreated feedstock is the hydrogen bond destroyed between polysaccharide molecule using vapor, keeps cell wall structure loose, be more advantageous to Solvent enters through cell wall during subsequent extracted, makes extraction efficiency more preferably.

(3) dry, dry purpose is steam extra after removing high temperature and pressure, the more conducively progress of later period extraction process With the stabilization of extract, 50~80 DEG C of dry 1~2h are preferred in the present invention.Dry hand well known to other skilled in the art Section also can be applied to this.

Above-mentioned plant extracts has effects that repair the application in the cosmetics of skin barrier in preparation.

It is a kind of to have effects that repair the cosmetics of skin barrier, wherein the cosmetics by above-mentioned plant extracts and Cosmetic field is subjected to auxiliary material and is made.

A kind of external-use skin care oil for having effects that repair skin barrier, wherein the skin care oil is matched by following weight parts Raw material be made:

Phytosterin ester 1~4, bisabolol 0.2~0.5, sunflower oil 5~10, Purple Perilla Seed Oil 5~10, above-mentioned plant Object extract 65~85, butyl hydroxytoluene 0.1~0.3.

A kind of preparation method of above-mentioned external-use skin care oil, wherein steps are as follows for the preparation method:

(1) each raw material is weighed according to above-mentioned proportion；

(2) phytosterin ester and butyl hydroxytoluene are added in the exterior-applied plant extract, are heated at 50~60 DEG C 20~40min of stirring and dissolving；

(3) bisabolol, sunflower oil and Purple Perilla Seed Oil are added after being cooled to 30~40 DEG C, stir evenly to get.

What the above method was prepared is oil-type cosmetics, conventional using plant extracts of the present invention and skin care field Other dosage forms, such as cream, toner, lotion, spray can also be prepared in method and auxiliary material.Plant extracts of the present invention External application can also play described effect after being simply pulverized and mixed, and preparation method is not limited to of the present invention.

Invention formulation is recommended to use method are as follows: imposes on human skin surface with smearing method, gently massage is until absorb.

Beneficial outcomes of the invention:

The present invention is using safflower, gardenia, FLOS CHRYSANTHEMI ALBA from Haizhou of China, armeniaca mume combination and compatibility and gives optimal compatibility dosage, It cooperates with and works between each component, cosmetics plant material is effectively extracted in conjunction with new opposed polarity solvent pairs proposed by the present invention Method, obtained plant extracts is substantially improved compared with the more excellent recovery rate of prior art extraction efficiency, so that final repair Skin barrier effect is more significant compared with the extract that the prior art is extracted.The present invention proposes that a kind of new opposed polarity is double molten The method that cosmetics plant material is effectively extracted in agent is right according to the selection of optimization cooperation and specific solvent to Extraction solvent Plant material extraction efficiency is significantly increased in the optimization of extraction step and extraction conditions parameter, the evaluation and test master of plant extract efficiency It to be evaluated by the anti-oxidant and anti-inflammatory efficacy of plant material, the plant extracts primary efficacy of cosmetics addition is also above-mentioned Two kinds, the extract extracted by the method for the invention can be seen that much excellent in terms of above-mentioned two effect by Efficacy experiments In the extract that the prior art is extracted.Extracting method of the present invention effectively shortens extraction time, and extraction efficiency is high, used Equipment is conventional and cheap, effectively reduces preparation cost, and the present invention is very suitable to large-scale industrial production.The present invention obtains Plant extracts ingredient is more stable, more preferable with the auxiliary material compatibility of the various dosage forms of cosmetics, is especially added to oil-type In cosmetic, effectively improves prior art extract and the defect for influencing product quality and effect such as be precipitated and occur precipitating, make Cosmetics are easier to storage transport, more preferably, and Use Limitation fruit is more preferably for product quality.The present invention effectively reduces in the prior art The dosage of organic solvent reduces the pollution to environment, more economical environmental protection.

Detailed description of the invention

Fig. 1 is that 1~24 extraction effect of sample passes through DPPH clearance rate evaluation figure；

Fig. 2 is that 25~30 extraction effect of sample passes through DPPH clearance rate evaluation figure；

Fig. 3 is that 31~36 extraction effect of sample passes through DPPH clearance rate evaluation figure；

Fig. 4 is prescription screening experiment DPPH clearance rate evaluation figure；

Fig. 5 is that adhesive tape causes damage test TEWL measurement result figure.

Specific embodiment

In order to make those skilled in the art are more detailed to understand extracting method of the present invention, inventor provides following tool Body embodiment, involved reagent are that well known in the art and commercially available purchase obtains, and the instrument being related to is set Standby is also the equipment that those skilled in the art is known and will appreciate that and uses.In order to guarantee the steady of solvent two and extract Fixed, each solvent that solvent one uses in present embodiment is anhydrous solvent.Following embodiment must not be interpreted as any meaning Limiting to the claimed invention in justice.

Tables 1 and 2 is seen using raw material and equipment purchase producer in the specific embodiment of the invention.

1 present invention of table uses raw material

2 present invention of table uses instrument

Embodiment 1

Safflower 2g, gardenia 4g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 4g, armeniaca mume 6g；

(2) it extracts for the first time: being that ethyl alcohol is added in 1:20m/m according to solid-liquid ratio, mix, extract 2h under the conditions of 55 DEG C；

(3) it extracts for second: being that sunflower seed oil is added in 1:20m/m according to solid-liquid ratio, 2h is extracted in stirring under the conditions of 55 DEG C；

(4) 40 DEG C are concentrated under reduced pressure into ethyl alcohol and completely remove；

(5) 10 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 2

Safflower 6g, gardenia 1g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 6g, armeniaca mume 4g；

(2) it extracts for the first time: being that ethyl alcohol is added in 1:10m/m according to solid-liquid ratio, mix, extract 1h under the conditions of 40 DEG C；

(3) it extracts for second: being that Parleam (20cSt) is added in 1:10m/m according to solid-liquid ratio, stirred under the conditions of 40 DEG C It mixes and extracts 1h；

(4) 50 DEG C are concentrated under reduced pressure into ethyl alcohol and completely remove；

(5) 1 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 3

Safflower 8g, gardenia 6g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 1g, armeniaca mume 1g；

(2) it extracts for the first time: being that dehydrated alcohol is added in 1:40m/m according to solid-liquid ratio, mix, extracted under the conditions of 90 DEG C 0.5h；

(3) it extracts for second: being that caprylic/capric triglyceride is added in 1:40m/m according to solid-liquid ratio, stirred under the conditions of 90 DEG C Extract 0.5h；

(4) 80 DEG C are concentrated under reduced pressure into ethyl alcohol and completely remove；

(5) 0.2 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 4

(1) each raw material is weighed according to following weight parts proportion；

Safflower 10g, gardenia 5g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 4g, armeniaca mume 1g；

(2) coarse crushing: each bulk pharmaceutical chemicals are crushed to 20 mesh and are mixed；

(3) high temperature high pressure process: 0.2MPa, handles 15min by 120 DEG C；

(4) dry: 50 DEG C of dry 1h；

(5) it extracts for the first time: being that chloroform is added in 1:60m/m according to solid-liquid ratio, mix, extract 1h under the conditions of 65 DEG C；

(6) it extracts for second: being that white oil (7cSt) is added in 1:60m/m according to solid-liquid ratio, 1h is extracted in stirring under the conditions of 65 DEG C；

(7) 40 DEG C are concentrated under reduced pressure into chloroform and completely remove；

(8) 0.2 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 5

Safflower 5g, gardenia 10g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 1g, armeniaca mume 10g；

(2) coarse crushing: each bulk pharmaceutical chemicals are crushed to 40 mesh and are mixed；

(3) high temperature high pressure process: 0.1MPa, handles 15min by 120 DEG C；

(4) dry: 60 DEG C of dry 2h；

(5) it extracts for the first time: being that chloroform is added in 1:50m/m according to solid-liquid ratio, mix, extract 0.5h under the conditions of 85 DEG C；

(6) it extracts for second: being that caprylic/capric triglyceride is added in 1:50m/m according to solid-liquid ratio, stirred under the conditions of 85 DEG C Extract 0.5h；

(7) 60 DEG C are concentrated under reduced pressure into chloroform and completely remove；

(8) 10 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 6

Safflower 2g, gardenia 1g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 10g, armeniaca mume 3g；

(2) coarse crushing: each bulk pharmaceutical chemicals are crushed to 60 mesh and are mixed；

(3) high temperature high pressure process: 0.1MPa, handles 30min by 100 DEG C；

(4) dry: 75 DEG C of dry 1.5h；

(5) it extracts for the first time: being that chloroform is added in 1:60m/m according to solid-liquid ratio, mix, extract 2h under the conditions of 90 DEG C；

(6) it extracts for second: being that Nexbase 2004 (30cSt) is added in 1:60m/m according to solid-liquid ratio, stirred under the conditions of 90 DEG C Extract 2h；

(7) 80 DEG C are concentrated under reduced pressure into chloroform and completely remove；

(8) 6 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 7

Safflower 5g, gardenia 3g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 1g, armeniaca mume 1g；

(2) coarse crushing: each bulk pharmaceutical chemicals are crushed to 30 mesh and are mixed；

(3) high temperature high pressure process: 0.2MPa, handles 10min by 100 DEG C；

(4) dry: 70 DEG C of dry 1h；

(5) it extracts for the first time: being that acetone is added in 1:70m/m according to solid-liquid ratio, mix, extract 1h under the conditions of 70 DEG C；

(6) it extracts for second: being that isostearyl isostearate ester is added in 1:70m/m according to solid-liquid ratio, stirred under the conditions of 70 DEG C It mixes and extracts 1h；

(7) 45 DEG C are concentrated under reduced pressure into acetone and completely remove；

(8) 2 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 8

Safflower 3g, gardenia 5g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 4g, armeniaca mume 3g；

(2) coarse crushing: each bulk pharmaceutical chemicals are crushed to 50 mesh and are mixed；

(3) high temperature high pressure process: 0.1MPa, handles 20min by 110 DEG C；

(4) dry: 60 DEG C of dry 1h；

(5) it extracts for the first time: being that acetone is added in 1:35m/m according to solid-liquid ratio, mix, extract 2h under the conditions of 65 DEG C；

(6) it extracts for second: being that soybean oil is added in 1:35m/m according to solid-liquid ratio, 2h is extracted in stirring under the conditions of 65 DEG C；

(7) 50 DEG C are concentrated under reduced pressure into acetone and completely remove；

(8) 4 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 9

Safflower 3g, gardenia 2g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 1g, armeniaca mume 3g；

(3) high temperature high pressure process: 0.1MPa, handles 30min by 130 DEG C；

(4) dry: 65 DEG C of dry 2h；

(5) it extracts for the first time: being that (chloroform alcohol is according to quality for 1:55m/m addition chloroform alcohol mixed liquor according to solid-liquid ratio Compounded than 1:1), it mixes, extracts 2h under the conditions of 65 DEG C；

(6) it extracts for second: being that sesame oil is added in 1:55m/m according to solid-liquid ratio, 2h is extracted in stirring under the conditions of 65 DEG C；

(7) 55 DEG C are concentrated under reduced pressure into solvent one and completely remove；

(8) 8 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 10

Safflower 1g, gardenia 6g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 5g, armeniaca mume 5g；

(2) coarse crushing: being broken to 40 mesh for each raw material, mixes；

(3) high temperature high pressure process: 0.2MPa, handles 30min by 110 DEG C；

(4) dry: 60 DEG C of dry 1.5h；

(5) it extracts for the first time: being that ethyl alcohol is added in 1:30m/m according to solid-liquid ratio, mix, extract 1h under the conditions of 80 DEG C；

(6) it extracts for second: being that caprylic/capric triglyceride is added in 1:10m/m according to solid-liquid ratio, stirred under the conditions of 80 DEG C Extract 2h；

(7) 40 DEG C are cooled to hereinafter, 60 mesh coarse filtration；

(8) 60 DEG C are concentrated under reduced pressure into solvent one and completely remove；

(9) 40 DEG C are cooled to hereinafter, 10 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 11

Safflower 6g, gardenia 3g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 5g, armeniaca mume 1g；

(2) coarse crushing: each raw material is crushed to 50 mesh and is mixed；

(3) high temperature high pressure process: 0.2MPa, handles 15min by 110 DEG C；

(4) dry: 75 DEG C of dry 1h；

(5) extract for the first time: according to solid-liquid ratio be 1:95m/m be added chloroform and acetone mixed solvent (therebetween according to Mass ratio 1:1 compounding), it mixes, extracts 1h under the conditions of 40 DEG C；

(6) it extracts for second: being that caprylic/capric triglyceride and Nexbase 2004 is added in 1:95m/m according to solid-liquid ratio (17cSt) compound (the two according to mass ratio 1:1 compound), 1h is extracted in stirring under the conditions of 40 DEG C；

(7) 40 DEG C are cooled to hereinafter, 80 mesh coarse filtration；

(8) 70 DEG C are concentrated under reduced pressure into solvent one and completely remove；

(9) 40 DEG C are cooled to hereinafter, 1 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 12

Safflower 8g, gardenia 1g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 1g, armeniaca mume 3g；

(2) each raw material coarse crushing: is crushed to 60 mesh；

(2) high temperature high pressure process: 0.2MPa, handles 10min by 130 DEG C；

(3) dry: 80 DEG C of dry 1.5h；

(4) extract for the first time: according to solid-liquid ratio be 1:34m/m be added ethyl alcohol and acetone mixed solvent (therebetween according to 1:1 compounding), it mixes, extracts 1h under the conditions of 80 DEG C；

(5) it second extracts: being that 1:35m/m is added olive oil and macadimia nut oil compound (the two is pressed according to solid-liquid ratio Compounded according to mass ratio 1:1), 1h is extracted in stirring under the conditions of 60 DEG C；

(6) 40 DEG C are cooled to hereinafter, 100 mesh coarse filtration；

(7) 80 DEG C are concentrated under reduced pressure into solvent one and completely remove；

(8) 40 DEG C are cooled to hereinafter, 6 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 13

Safflower 4g, gardenia 3g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 10g, armeniaca mume 1g；

(2) each raw material coarse crushing: is crushed to 30 mesh；

(3) high temperature high pressure process: 0.2MPa, handles 30min by 100 DEG C；

(4) dry: 60 DEG C of dry 1h；

(5) extract for the first time: according to solid-liquid ratio be 1:15m/m be added chloroform and alcohol mixed solvent (therebetween according to Mass ratio 1:1 compounding), it mixes, extracts 1.5h under the conditions of 70 DEG C；

(6) it extracts for second: being that white oil (16cSt) and Parleam (11cSt) is added in 1:15m/m according to solid-liquid ratio Mixed solvent (the two according to mass ratio 1:1 compound), 1.5h is extracted in stirring under the conditions of 70 DEG C；

(7) 40 DEG C are cooled to hereinafter, 90 mesh coarse filtration；

(8) 80 DEG C are concentrated under reduced pressure into solvent one and completely remove；

(9) 40 DEG C are cooled to hereinafter, 5 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 14

Safflower 1g, gardenia 10g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 2g, armeniaca mume 5g；

(2) each raw material coarse crushing: is crushed to 40 mesh；

(3) high temperature high pressure process: 0.2MPa, handles 10min by 110 DEG C；

(4) dry: 40 DEG C of dry 1h；

(5) it extracts for the first time: being that ethyl alcohol is added in 1:35m/m according to solid-liquid ratio, mix, extract 1h under the conditions of 90 DEG C；

(6) it second extracts: being that 1:35m/m is added grape seed oil and oat oil mixed solvent (the two is pressed according to solid-liquid ratio Compounded according to mass ratio 1:1), 0.5h is extracted in stirring under the conditions of 50 DEG C；

(7) 40 DEG C are cooled to hereinafter, 90 mesh coarse filtration；

Embodiment 15

Safflower 1g, gardenia 5g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 5g, armeniaca mume 10g；

(2) each raw material coarse crushing: is crushed to 40 mesh；

(3) high temperature high pressure process: 0.2MPa, handles 10min by 130 DEG C；

(4) dry: 70 DEG C of dry 1h；

(5) it extracts for the first time: being that chloroform is added in 1:65m/m according to solid-liquid ratio, mix, extract 1h under the conditions of 70 DEG C；

(6) it extracts for second: being that Sweet Almond Oil is added in 1:65m/m according to solid-liquid ratio, 1h is extracted in stirring under the conditions of 70 DEG C；

(7) 40 DEG C are cooled to hereinafter, 90 mesh coarse filtration；

(9) 40 DEG C are cooled to hereinafter, 0.5 μm of filter plate aperture, refined filtration to filtrate clarify to get.

Embodiment 16 has effects that repair the oil-type cosmetics of skin barrier

(1) each raw material is weighed according to following proportions；

Phytosterin ester 1g, bisabolol 0.3g, sunflower oil 6g, Purple Perilla Seed Oil 10g, embodiment 1 prepare plant extract Object 65g, butyl hydroxytoluene 0.2g.

(2) phytosterin ester and butyl hydroxytoluene are added in the exterior-applied plant extract, the heating stirring at 50 DEG C Dissolve 30min；

(3) bisabolol, sunflower oil and Purple Perilla Seed Oil are added after being cooled to 40 DEG C, stir evenly to get.

Embodiment 17 has effects that repair the oil-type cosmetics of skin barrier

(1) each raw material is weighed according to above-mentioned proportion；

Phytosterin ester 3g, bisabolol 0.2g, sunflower oil 5g, Purple Perilla Seed Oil 6g, embodiment 10 prepare plant extract Object 70g, butyl hydroxytoluene 0.1g.

(2) phytosterin ester and butyl hydroxytoluene are added in the exterior-applied plant extract, the heating stirring at 60 DEG C Dissolve 20min；

(3) bisabolol, sunflower oil and Purple Perilla Seed Oil are added after being cooled to 30 DEG C, stir evenly to get.

Embodiment 18 has effects that repair the oil-type cosmetics of skin barrier

(1) each raw material is weighed according to above-mentioned proportion；

Phytosterin ester 4g, bisabolol 0.5g, sunflower oil 10g, Purple Perilla Seed Oil 5g, embodiment 15 prepare plant extract Object 85g, butyl hydroxytoluene 0.3g.

(2) phytosterin ester and butyl hydroxytoluene are added in the exterior-applied plant extract, the heating stirring at 55 DEG C Dissolve 40min；

(3) bisabolol, sunflower oil and Purple Perilla Seed Oil are added after being cooled to 35 DEG C, stir evenly to get.

Efficacy experiments of the present invention

The cooperation of solvent one and solvent two of the present invention, the extraction process optimized in conjunction with the present invention and extracting parameter, can play Synergistic effect, so that recovery rate is higher, extract property is more excellent more stable, and extraction cost is lower, is suitble to industrialization Using.

One, the selection of solvent one and solvent two of the present invention

1, solvent one selects plant extract common, and with each active component good compatibility, recovery rate is high, representative Solvent；It is best that one polarity of solvent in view of testing confirmation should be greater than two extraction effect of solvent, therefore is ultimately determined to ethyl alcohol, third Ketone and chloroform.Inventor thinks that above-mentioned technical effect has reached the present invention claims therefore need not carry out the sieve of further solvent one again Choosing, in this way also for the workload reduced when solvent two selects.

2, the selection course summary of solvent two:

Solvent two selects polarity to be less than the solvent of solvent one, is preferred with grease type.

(1) vegetable oil: each plant oil nature is similar, therefore only selecting a kind of is representative, multiple with three kinds of solvents of solvent one respectively With extraction, there is preferable effect；

(2) white oil: selection limit range of viscosities in and range outside two kinds of white oils (numerical value generally near critical value, Such as 26 and 32), extracted respectively with three kinds of solvent complexes of solvent one, the white oil effect in range of viscosities is good, the effect outside range It is bad；

(3) Parleam, Nexbase 2004: both are all olefin polymers, are only selected a kind of for representative, repetition The work of white oil screening, i.e. selection limit in range of viscosities and outside range, (numerical value generally near critical value, such as 26 Hes 32) it tests respectively, obtains different extraction effects；

(4) it caprylic/capric triglyceride: is extracted with three kinds of solvent complexes of solvent one, there is preferable effect；

(5) it isostearyl isostearate ester: is extracted with three kinds of solvent complexes of solvent one, there is preferable effect；

(6) dimethyl silicone polymer (silicone oil): silicone oil is silicon chain, poor to the active constituent solute effect of carbochain, respectively with Solvent one compounds, and extraction effect is bad.

It is the experimental considerations of solvent screening part above, i.e. the sample 1~24 of solvent selected section.The original of sample 1~24 Material and preparation method are identical, and only Extraction solvent is different.

It is specific the preparation method is as follows:

Safflower 3g, gardenia 6g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 5g, armeniaca mume 5g；

(2) each raw material coarse crushing: is crushed to 40 mesh；

(4) dry: 60 DEG C of dry 1.5h；

(5) it extracts for the first time: being that solvent one is added in 1:30m/m according to solid-liquid ratio, mix, extract 1h under the conditions of 80 DEG C；

(6) it extracts for second: being that solvent two is added in 1:10m/m according to solid-liquid ratio, 2h is extracted in stirring under the conditions of 80 DEG C；

(7) 40 DEG C are cooled to hereinafter, 60 mesh coarse filtration obtain filtrate；

1~24 solvent for use of sample is shown in Table 3

3 sample solvent table of table

3. test result:

This part content is the screening to solvent two, and solvent one is fixed as ethyl alcohol, chloroform, acetone.

(1) DPPH removes free radical experiment: the complicated component of plant extracts, analysis for extract effective component and Quantitative comparison is difficult, therefore those skilled in the art evaluate the efficiency of effective component extraction by detecting to antioxidant activity, The extract that often the good technique of extraction efficiency is prepared has superior antioxidant activity effect.Antioxidant activity is general Using DPPH radicals scavenging experimental evaluation.DPPH (2,2- xenyl -1- picrylhydrazyl) is a kind of organic nitrogen being stabilized Free radical is widely used in antioxidation in vitro agent capability study.There is characteristic absorption peak in 515nm or so based on DPPH, it is anti-oxidant Agent, which provides hydrogen atom, weakens its color the one-electron reduction on DPPH, evaluates free radical according to the reduction amount of its light absorption value Removing degree.

Experimental result is shown in Fig. 1 for 1~24 antioxidant activity of sample.

(1) stability experiment is shown in Table 4.

The stability that 4 different solvents of table extract sample compares

Experimental result:

1. sample 1~3 is that vegetable oil (plant oil nature is similar, only by taking sunflower seed oil as an example) compounds with solvent one respectively It extracts, vegetable oil is compounded with ethyl alcohol, acetone, chloroform, there is good extraction effect.

2. sample 4~6 is that caprylic/capric triglyceride compounds extraction with ethyl alcohol, acetone, chloroform respectively, have good Extraction effect.

3. sample 7~9 is that isostearyl isostearate ester compounds extraction with ethyl alcohol, acetone, chloroform respectively, have preferable Extraction effect.

4. sample 10~12 be white oil (26cSt meets kinematic viscosity≤30cSt requirement for limiting of the present invention) respectively with Ethyl alcohol, acetone, chloroform compounding are extracted, and have preferable extraction effect.

5. sample 13~15 is white oil (32cSt does not meet kinematic viscosity≤30cSt requirement that the present invention limits) difference Extraction is compounded with ethyl alcohol, acetone, chloroform, extraction effect is all poor.

6. sample 10~15 is to compare kinematic viscosity≤30cSt white oil with the white oil of kinematic viscosity > 30cSt, By the difference of extraction effect, illustrate the reason of selecting kinematic viscosity≤30cSt white oil.

7. sample 16~18 is Nexbase 2004 (30cSt meets kinematic viscosity≤30cSt requirement that the present invention limits) Extraction is compounded with ethyl alcohol, acetone, chloroform respectively, there is preferable extraction effect.

8. sample 19~21 is that (46cSt does not meet kinematic viscosity≤30cSt that the present invention limits and wants Nexbase 2004 Ask) extraction is compounded with ethyl alcohol, acetone, chloroform respectively, extraction effect is all poor.

It is by kinematic viscosity≤30cSt Nexbase 2004, with kinematic viscosity > 9. sample 16~21 is similar with white oil 30cSt's compares, and by the difference of extraction effect, illustrates the reason of selecting kinematic viscosity≤30cSt Nexbase 2004.Separately Outside, Nexbase 2004 and Parleam are all polymer, therefore are only illustrated by taking Nexbase 2004 as an example.

10. sample 21~24 is that dimethyl silicone polymer (silicone oil, PMX200,6cSt) is multiple with ethyl alcohol, acetone, chloroform respectively It is poor to the active constituent solute effect of carbochain since silicone oil is silicon chain structure with extraction, therefore extraction effect is very poor, performance It is extremely low for DPPH clearance rate；Due to poor compatibility, cause its stability also bad, shows as sample muddiness or active constituent is precipitated (precipitating).

By above-mentioned experiment, the solvent two that the present invention preferably goes out includes vegetable oil (sample 1~3), caprylic/capric glycerol three Ester (sample 4~6), isostearyl isostearate ester (sample 7~9), the white oil (sample 10 of kinematic viscosity (40 DEG C)≤30cSt ~12), the Parleam of kinematic viscosity (40 DEG C)≤30cSt (is all olefin polymer with Nexbase 2004, only with hydrogenation Tested for poly decene), the Nexbase 2004 (sample 16~18) of kinematic viscosity (40 DEG C)≤30cSt.

The present invention as a comparison the solvent two including kinematic viscosity (40 DEG C) > 30cSt of counter-example white oil (sample 13~ 15), the Nexbase 2004 (sample 19~21) of kinematic viscosity (40 DEG C) > 30cSt, 6cSt dimethyl silicone polymer PMX200 (sample Product 21~24).

According to comparative experiments above it is found that being mentioned by carrying out compounding with solvent one (ethyl alcohol, acetone, chloroform) respectively It takes, vegetable oil, caprylic/capric triglyceride, isostearyl isostearate ester, white oil, the hydrogen of kinematic viscosity (40 DEG C)≤30cSt Change polyisobutene and Nexbase 2004, all has preferable extraction effect, and the product stability after extraction is good, be suitable as this The solvent two of invention cooperates with solvent one, realizes the extraction process in the present invention.And kinematic viscosity (40 DEG C) > 30cSt's is white Oil, Parleam and Nexbase 2004, since viscosity increases, the substance transmitting being unfavorable in extraction process causes to extract Effect is undesirable, is not suitable as solvent two of the invention.Silicone oil (dimethyl silicone polymer) is due in architectural difference, with plant Carbochain active constituent compatibility it is bad, and then cause extraction efficiency low, and the product stability after extracting is poor, is also not suitable for making It is used for solvent two of the invention.

Two, the determination of extracting parameter of the present invention

1. temperature parameter choice experiment: second step extraction be one solvent two of solvent collaboration extract, therefore this step extract to Close important, second step Extracting temperature directly influences dissolve each other degree and the extraction efficiency of two solvents.

Solvent one is by taking ethyl alcohol as an example in this experiment, and solvent two is by taking Miglyol 812N as an example.

Specific preparation process such as experiment one, the specific steps are as follows:

(2) coarse crushing: being crushed to 40 mesh for each raw material, mixes；

(4) dry: 60 DEG C of dry 1.5h；

(6) it extracting for second: being that caprylic/capric triglyceride is added in 1:10m/m according to solid-liquid ratio, Extracting temperature is shown in Table 5, 2h is extracted in stirring；

Table 5

25~30 extraction effect of sample is evaluated by DPPH clearance rate, and experimental method is shown in that DPPH radicals scavenging is tested.Knot Fruit sees Fig. 2.As it can be seen that in extract temperature between 40~90 DEG C extraction efficiency highest, lower than 40 DEG C or be higher than 90 DEG C the case where Lower extraction efficiency is too low, if can only improve recovery rate by extending extraction time using bad temperature, will affect and mentions Economic benefit of the taking technique in industrial application.Extracting temperature is that 80 DEG C of extraction efficiencies are best.

The stability experiment method of sample 25~30 is shown in that stability compares, and the results are shown in Table shown in 6.

The stability that 6 different temperatures of table extracts sample compares

This part content is the technological parameter screening extracted to second step, by taking temperature as an example, compares 30 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, under the conditions of 90 DEG C and 95 DEG C of six temperature, the DPPH and stability of product, 40~90 DEG C of extraction effects (DPPH) and Stability is all preferable, and 30 DEG C of extraction effects are poor, and 95 DEG C of extraction effects are poor, and since temperature is excessively high, the stability of product is also poor, Appearance changes colour and peculiar smell, therefore final Extracting temperature is recommended to use 40 DEG C~90 DEG C ranges, and optimum extraction temperature is 80 DEG C.

2. second of extraction solid-liquid ratio parameter selection experiments: extracting solid-liquid ratio and directly affect dissolving each other for solvent one and solvent two The extraction efficiency that degree and cooperation are extracted

(2) coarse crushing: being crushed to 40 mesh for each raw material, mixes；

(4) dry: 60 DEG C of dry 1.5h；

(6) it extracts for second: caprylic/capric triglyceride is added according to solid-liquid ratio shown in table 7, stirs and mentions under the conditions of 80 DEG C Take 2h；

Table 7

31~36 extraction effect of sample is evaluated by DPPH clearance rate, and experimental method is shown in that DPPH radicals scavenging is tested.Knot Fruit sees Fig. 3.As it can be seen that being the extraction efficiency of 1:10~100 height in solid-liquid ratio, and high in the extraction efficiency of 1:10~50.

Three, each bulk pharmaceutical chemicals of the present composition and compatibility selection optimization

The selection thinking of bulk pharmaceutical chemicals of the present invention: according to the thought of Chinese medicine " whole, dialectical, comprehensive ", according to " monarch, minister, assistant, Make " the principles of formulating prescriptions, safflower, gardenia, FLOS CHRYSANTHEMI ALBA from Haizhou of China, armeniaca mume are subjected to compatibility, monarch drug in a prescription blood circulation promoting and dispersing pathogen accumulation, ministerial drug heat-clearing is cool Blood, the two mutually make for synergistic；Adjutant is clearing heat and detoxicating, wind-dispelling heat-dissipating；Make medicine nourishing Yin and promoting production of body fluid.Full side by promoting blood circulation and cooling blood, Clearing heat and detoxicating, wind-dispelling heat-dissipating removes inflammatory factor, and nourishing Yin and promoting production of body fluid cares for shield skin, keeps the skin wet, thus alleviate rubefaction, The symptoms such as slight discomfort, and then skin barrier is repaired, improve tolerance of skin.It is significant to increase in conjunction with the improvement to preparation method The extraction efficiency of active constituent is added, to obtain a kind of efficient plant extracts.

The preparation method of this experiment each sample is identical, and bulk pharmaceutical chemicals gross mass is 10g, and the component and compatibility of each sample prescription are closed System is different, and see Table 8 for details.Steps are as follows for specific preparation method:

(1) each raw material is weighed according to 8 weight of table, mixed；

(2) coarse crushing: being crushed to 40 mesh for each raw material, mixes；

(4) dry: 60 DEG C of dry 1.5h；

(6) it extracts for second: being that Miglyol 812N is added in 1:10m/m according to solid-liquid ratio, extracted under the conditions of 80 DEG C 2h；

Table 8

1~11 prescription effect of sample causes damage test to be evaluated by DPPH clearance rate and adhesive tape.

The test of 1.DPPH free radical scavenging activity:

Test method is shown in above-mentioned DPPH free radical scavenging activity test.

Test result is shown in Fig. 4, the results showed that, the prescription and dosage DPPH clearance rate highest of sample 5 (prescription of the present invention), effect Fruit is best, and sample 1~4,6~11 prescription raw materials lack or match not within ratio range of the present invention, DPPH clearance rate compared with It is low, it is ineffective.

2. adhesive tape causes damage test:

Mouse skin damage (adhesive tape causes damage) model is established, plant extracts of the present invention is investigated and the recovery of damage epidermis is made With, characterize its repair effect.

Adhesive tape causes loss testing method: torn fast is continuously pasted for several times using adhesive tape, until small blood point occurs in mouse skin Stop stickily tear, smear each sample respectively, smear once daily, continuously smear 4d, smears 0d, 2d, 4d measurement through the severe edema due to hypofunction of the spleen respectively Disperse vector (TEWL).

Animal experiment is to add the external application that plant extracts mass percent of the present invention is 5.0% to repair barrier shield with sample Skin composite preparation, formula table are as shown in the table.

Table 9 repairs barrier skin care compositions pharmaceutical formulation

The sample is the sample 1~11 in table 8；Blank group is not smear any instance model group after skin causes damage；Just Chang Zuwei skin causes damage model group without using adhesive tape.

Skin causes damage repairing test result (as shown in table 10) to show the skin care system containing 5.0% sample 5 (prescription of the present invention) The percutaneous water loss amount of agent is far smaller than other groups, i.e., prescription (sample 5) and other prescriptions used in the present invention (sample 1~4, Sample 6~11) compared to having effects that quick and more excellent reparation skin barrier, preferably skin injury can be promoted to repair Multiple and healing.

The different group formula extraction adhesive tapes of table 10 cause damage test TEWL value

Four, the method for the present invention is compared with art methods extraction efficiency

The complicated component of plant extracts, the analysis and quantitative comparison for extract effective component are difficult, therefore ability Field technique personnel evaluate the efficiency of effective component extraction by the detection to antioxidant activity and anti-inflammatory activity, often extract effect The extract that the good technique of rate is prepared has superior effect.

Antioxidant activity generally uses DPPH radicals scavenging experimental evaluation.DPPH (2,2- xenyl -1- picrylhydrazyl) It is a kind of organic nitrogen free radical being stabilized, is widely used in antioxidation in vitro agent capability study.Based on DPPH on the left side 515nm There is characteristic absorption peak on the right side, and antioxidant, which provides hydrogen atom, weakens its color the one-electron reduction on DPPH, according to its light absorption value Reduction amount evaluate the removing degree of free radical.

Anti-inflammatory activity is generally using inhibition hyaluronidase experimental evaluation.Hyaluronidase is anaphylactoid participant, Some researches show that hyaluronidase and inflammation, allergy strong correlation, and hyaluronidase body outer suppressioning test is anti-frequently as measurement The method of activity.Antiallergic activity is using hyaluronic acid enzyme inhibition rate as index, the more big then anti-mistake of hyaluronic acid enzyme inhibition rate Quick activity is stronger.

The sample preparation of Efficacy experiments of the present invention is for example following

Sample 1 (prior art grease extracts twice): weighing safflower 3g, gardenia 6g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 5g, armeniaca mume 5g, It is crushed to 40 mesh, 0.2MPa, 110 DEG C of processing 30min, 60 DEG C of dry 1.5h；It is sweet that caprylic/capric is added in solid-liquid ratio 1:30 (m/m) 1h is extracted in three ester 100g of oil, 80 DEG C of stirrings；Solid-liquid ratio 1:10 (m/m), again be added caprylic/capric triglyceride 300g, 80 DEG C 2h is extracted in stirring；40 DEG C are cooled to hereinafter, 10 μm of filter plate aperture, refined filtration to clarification to get.

Sample 2 (prior art ethyl alcohol extracts twice): weighing safflower 3g, gardenia 6g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 5g, armeniaca mume 5g, It is crushed to 40 mesh, 0.2MPa, 110 DEG C of processing 30min, 60 DEG C of dry 1.5h；Dehydrated alcohol is added in solid-liquid ratio 1:30 (m/m) 1h is extracted in 100g, 80 DEG C of stirrings；Solid-liquid ratio 1:10 (m/m), is added dehydrated alcohol 300g again, and 2h is extracted in 80 DEG C of stirrings；It is cooling To 40 DEG C hereinafter, filtering, obtains filtrate；60 DEG C of reduced pressures；10 μm of filter plate aperture, refined filtration to clarification to get.

Sample 3 (one polarity of solvent is extracted twice in the case where being less than solvent two): safflower 3g, gardenia 6g, FLOS CHRYSANTHEMI ALBA from Haizhou of China 5g, armeniaca mume 5g are crushed to 40 mesh, 0.2MPa, 110 DEG C of processing 30min, 60 DEG C of dry 1.5h；Solid-liquid ratio 1:30 (m/m), adds Enter hexamethylene 300g, 1h is extracted in 80 DEG C of stirrings；Solid-liquid ratio 1:10 (m/m), is added butanediol 900g, and 2h is extracted in 80 DEG C of stirrings；It is cold But to 40 DEG C hereinafter, filtering, obtains filtrate；60 DEG C of reduced pressures, remove hexamethylene；10 μm of filter plate aperture, refined filtration are obtained to clarifying To extract.

Sample 4: embodiment 10.

1.DPPH radicals scavenging experiment

(1) experimental method: taking DPPH solution 1mL and sample liquid 1mL, and sufficiently oscillation is uniformly mixed, and stands 30min, uses enzyme Mark instrument measures its absorbance under 517nm wavelength.

DPPH free radical scavenging activity calculation formula:

DPPH free radical scavenging activity %=[(B+C)-A]/B*100

In formula: A is sample solution and the mixed OD value of DPPH solution, and B is that dehydrated alcohol and DPPH solution are mixed OD value, C are dehydrated alcohol and the mixed OD value of sample solution.

(1) experiment conclusion: as shown in table 11.

11 different process of table prepares the comparison of sample DPPH clearance rate

Sample ID	Tested concentration %	Clearance rate %
			Sample 1	5	31
Sample 2	5	45
			Sample 3	5	24
Sample 4 (embodiment 10)	5	87

Sample 1 is directly extracted using grease, since grease molecules amount is larger, not easily passs through cell wall and cell membrane, is extracted Intracellular activity ingredient, and viscosity is higher, the substance transmitting being unfavorable in extraction process, therefore DPPH clearance rate is low.

Sample 2 is extracted using ethyl alcohol, and ethyl alcohol is excellent solvent, while extracting fuel-displaced molten active constituent, a large amount of water Soluble polysaccharide also dissolves out therewith；When concentration, the stickums such as polysaccharide sweep along the part molten active constituent of oil to be precipitated, and form precipitating, make At the loss of active constituent, therefore DPPH clearance rate is lower.

Sample 3 uses two-step method duo-sol extraction, but polarity is weaker for solvent 1 (comparing with solvent 2), solvent 2 (with the ratio of solvent 1) Polarity is stronger, and solvent 1 and cell membrane interaction are weak, is unfavorable for two kinds of solvents and enters cell extraction active constituent, it is molten to destroy two Synergistic function between agent, causes recovery rate to reduce, therefore DPPH clearance rate is lower.

Embodiment 10 prepares sample DPPH clearance rate and is apparently higher than sample 1,2 and 3, and the effect of far superior to sample 1 and 2 The sum of.

Inventor has done same comparison with other embodiments, leads to the same conclusion.

2. inhibiting hyaluronidase experiment

(1) experimental method: take 0.1mL 0.25mmol/L calcium chloride solution and 37 DEG C of 0.5mL hyaluronic acid enzyme solution heat preservation Cultivate 20min；Sample liquid 0.5mL is added, continues 37 DEG C of heat insulating culture 20min；37 DEG C of 0.5mL sodium hyaluronate liquid heat preservations are added 30min, room temperature 5min；0.1mL 0.4mol/L sodium hydroxide solution and 0.5mL acetylacetone,2,4-pentanedione solution is added, sets boiling water bath Immediately with the cooling 5min of ice water after middle heating 15min；Ehrlich's reagent 1.0mL is added and is carried out with 3.0mL dehydrated alcohol dilute It releases, places 20min colour developing, measure its absorbance under 555nm wavelength with microplate reader.

Hyaluronic acid enzyme inhibition rate calculation formula:

Hyaluronic acid enzyme inhibition rate %=[(A-B)-(C-D)]/(A-D) * 100

In formula: for A by contrast solution absorbance (replacing sample solution with acetate buffer solution), B is control blank solution extinction It spends (replacing sample solution and enzyme solution with acetate buffer solution), C is sample solution absorbance value, and D is sample blank solution absorbance (replacing enzyme solution with hac buffer).

(2) experiment conclusion: as shown in the table.

12 different process of table prepares the comparison of sample clear matter acid enzyme inhibition rate

Sample ID	Tested concentration %	Inhibiting rate %
			Sample 1	5	13
Sample 2	5	44
			Sample 3	5	21
Sample 4 (embodiment 10)	5	64

Sample 1 is directly extracted using grease, since grease molecules amount is larger, not easily passs through cell wall and cell membrane, is extracted Intracellular activity ingredient, and viscosity is higher, the substance transmitting being unfavorable in extraction process, therefore hyaluronic acid enzyme inhibition rate is low.

Sample 2 is extracted using ethyl alcohol, and ethyl alcohol is excellent solvent, while extracting fuel-displaced molten active constituent, a large amount of water Soluble polysaccharide also dissolves out therewith；When concentration, the stickums such as polysaccharide sweep along the part molten active constituent of oil to be precipitated, and form precipitating, make At the loss of active constituent, therefore hyaluronic acid enzyme inhibition rate is lower.

Sample 3 uses two-step method duo-sol extraction, but polarity is weaker for solvent 1 (comparing with solvent 2), solvent 2 (with the ratio of solvent 1) Polarity is stronger, and solvent 1 and cell membrane interaction are weak, is unfavorable for two kinds of solvents and enters cell extraction active constituent, it is molten to destroy two Synergistic function between agent, causes recovery rate to reduce, therefore hyaluronic acid enzyme inhibition rate is low.

Embodiment 10 prepares sample clear matter acid enzyme inhibition rate and is apparently higher than sample 1,2 and 3, and far superior to sample 1 and 2 The sum of effect.

Five, the extract that the present invention obtains compared with prior art stability in oil-type cosmetics compares

1. comparing for clarity in oil-type cosmetics

(1) experimental method: taking sample liquid 3.0g and oil-type cosmetics often to use auxiliary material grease 27.0g, is heated to 50 DEG C of left sides The right side, stirring and dissolving 20min after standing cooling 1h, observe dissolution situation of the sample in grease.Sample is good with gel compatibility, Then dissolved sample clear；Sample and gel compatibility are poor, then dissolved sample becomes cloudy.Therefore, sample is in oil Dissolubility in rouge can be characterized with its dissolved muddy degree (turbidity).

Turbidity belongs to a kind of optical characteristics, is the scattering of the light due to caused by the molecule in liquid, and turbidity gets over Gao Ze Amount of scattered light is bigger.This experiment uses HI93414 high accuracy data type turbidimetric apparatus test sample turbidity.Surveyed numerical value is lower Prove that the lower clarity of turbidity is better, it was demonstrated that product stability is good.

(2) sample preparation technique: identical as DPPH radicals scavenging laboratory sample.

The comparison of 13 different process sample turbidity of table

(3) experiment conclusion: as shown above.

1, sample is extracted as grease, therefore turbidity is more excellent in oil-type cosmetic；Sample 2 is that alcohol is molten Property extract, it is poor with the compatibility of grease, therefore turbidity is high.The Extraction solvent of sample 3 has overturned solvent polarity of the invention, So that the solvent polarity of finished product is stronger, it is poor with gel compatibility, therefore turbidity is high.Sample 4 is cooperated using solvent one and solvent two It extracts, and optimizes extraction process, so that active constituent often uses the compatibility of auxiliary material grease good with cosmetics, therefore turbidity is lower, The even better than extract that extracts of grease.

2. stability experiment

(1) experimental method: taking sample liquid 10g and caprylic/capric triglyceride 190g, is heated to 50 DEG C or so, stirs molten Solve 20min, configured sample average be divided into five parts, be respectively placed in be protected from light (in room temperature magazine), refrigeration (4 DEG C of refrigerators), Under the conditions of illumination (28 DEG C of illumination boxs), hot (45 DEG C of baking ovens), freezing (- 15 DEG C of refrigerators) five, and respectively the 7th day, 14 It, 30 days observation stability.

(2) sample message: above-mentioned sample 1,2,3,4.

The comparison of 14 different process sample stability of table

(3) experiment conclusion: as shown above.

30 days visible its of stability experiment of sample 1 (grease extraction) have a small amount of precipitating, and have slight peculiar smell, illustrate sample Product are rotten.30 days visible its of stability experiment of sample 2 (ethyl alcohol extraction) have a large amount of precipitatings, illustrate that sample stability is deteriorated.Sample 3 (one polarity of solvent is less than the case where solvent two) 30 days, stability experiment was as it can be seen that its appearance illustrates that sample is steady with a large amount of precipitatings Qualitative variation.30 days stability experiments of sample 4 (embodiment 10) illustrate system of the present invention as it can be seen that appearance clear, smell is normal Standby extract stability is better than sample 1,2 and 3.

Six, the method for the present invention is compared with existing method technical costs

According to DPPH radicals scavenging experimental result it is found that when identical extraction conditions (solid-liquid ratio, Extracting temperature, when extracting Between), the extraction efficiency of (sample 4) of the invention directly extracts (sample 1) much higher than grease and ethyl alcohol extracts (sample 2).

15 present invention of table is compared with the cost of prior art industrial applications

By above table it is found that extraction efficiency of the present invention is far superior to sample 1 and sample 2.If it is desired to reaching and this hair Bright identical extraction efficiency needs to increase to twice of dosage, therefore the present invention, compared with existing extraction process, raw material dosage is less, Therefore the cost of preparation, storage and transport is lower.The present invention has save the cost compared with prior art, reduces material, energy The advantages of consumption.It is highly suitable for the industrialized production of current energy-saving and emission-reduction.

Seven, Efficacy experiments

1. adhesive tape causes damage test

Table 16 repairs barrier skin care compositions pharmaceutical formulation

Material name	Additive amount (%)
		Caprylic/capric triglyceride	50
Parleam	30
		White oil -16	15
Sample	5

The sample is above-mentioned sample 1 (oil extract), sample 2 (ethyl alcohol extraction), (one polarity of solvent is less than solvent to sample 3 Extracted twice in the case where two) and sample 4 (embodiment 10), embodiment 16, embodiment 17, embodiment 18；Blank group is skin Skin does not smear any instance model group after causing damage；Normal group is skin without using adhesive tape cause damage model group；Commercially available competing product be containing The skin care formulation of 5.0% Cer NP, formula table are as shown in the table.Embodiment 16,17 and 18 is oil-type product, Ke Yidan It solely uses, can also equally be used as additive with this experiment, specifically used method does not have an impact final effect.

The commercially available competing product group skin care formulation formula of table 17

Material name	Additive amount (%)
		Caprylic/capric triglyceride	50
Parleam	30
		White oil -16	15
Cer NP	5

Skin cause damage repairing test result (as shown in Figure 5) show contain 5.0% embodiment of the present invention (embodiment 10,

Embodiment 16, embodiment 17, embodiment 18) the percutaneous water loss amount of preparation is far smaller than other groups, therefore table Barrier skin care formulation is repaired in bright external application of the present invention has quick and more excellent reparation skin barrier compared with prior art Effect promotes skin injury reparation and healing.

2, human trial

By 4h normal individual trial, percutaneous water loss is measured, investigates the function of the Gu shield skin barrier of sample.

Percutaneous water loss test method: dissipating instrument using CK company water, at 25 ± 2 DEG C of temperature, the survey of humidity 50 ± 10% Under the conditions of examination, with the percutaneous moisture loss of skin (TEWL) for index, sample is tested.Human trial sample is caused with adhesive tape Damage test sample used, it is caprylic/capric triglyceride that blank group, which adds sample, and formula table is as shown in table 16.Measurement result is such as Shown in table 18.

Table 18 add 5.0% sample preparation human efficiency's test result --- arm dissipates data through the severe edema due to hypofunction of the spleen

It is confirmed by above-mentioned test, after the external-use skin care preparation that subject is prepared using extract of the embodiment of the present invention, hand It is in decreasing trend that arm is dissipated through the severe edema due to hypofunction of the spleen, shows that external-use skin care agent prepared by the present invention has the function of significantly repairing skin barrier.

(3) human body patch test

Referring to " cosmetics safety technical specification (2015 editions) ", chapter 7 Section 2, human skin enclosed type patch test side Method evaluates plant extracts safety of the present invention.

Recipient site is back, 33 people of volunteer, and patch continues for 24 hours, to remove 30min after tested material spot tester and divide for 24 hours It is not observed.

Human body patch test with sample is sample 1 (oil extract), sample 2 (ethyl alcohol extraction), (one polarity of solvent is small for sample 3 Extracted twice in the case where solvent two) and embodiment 10, embodiment 16, embodiment 17, embodiment 18, add sample size hundred Score is 20%, and formula table is as shown in the table.

Barrier skin care compositions pharmaceutical formulation is repaired used in 19 human body patch test of table

Material name	Additive amount (%)
		Caprylic/capric triglyceride	35
Parleam	30
		White oil -16	15
Sample	20

Human body patch test results are as shown in the table.Judgment criteria: suspicious reaction: only faint erythema.Weakly positive reaction (erythematous response): erythema, oedema, can have papule at infiltration.Strong positive reaction (erythematous response): erythema, oedema, can have mound at infiltration Rash；Reaction can exceed tested area.Extremely strong positive reaction (erythematous response): obvious erythema, severe infiltration, oedema, amalgamation bleb； Reaction exceeds tested area.

0.5 hour observation result after the removal of 20 spot tester of table

24 hours observation results after the removal of 21 spot tester of table

It is 33 people, 31 people of 0.5h efficiently individual quantity, for 24 hours 30 people of efficiently individual quantity that this self-test, which participates in number,.

0.5h is the results show that spot tester+dry filter paper occurs adverse reaction 5；Spot tester occurs adverse reaction 2；Sample Product 1 (oil extract), sample 2 (ethanol extract), sample 3 (one polarity of solvent is less than the extract in the case of solvent two) occur Adverse reaction 1；Sample 4 (embodiment 10), sample 5 (embodiment 16), sample 6 (embodiment 17), sample 7 (embodiment 18) do not have Occur adverse reaction.

For 24 hours the results show that spot tester+dry filter paper, spot tester, sample 1 (oil extract), sample 2 (ethanol extract), There is 1 adverse reaction in sample 3 (one polarity of solvent is less than the extract in the case of solvent two)；Sample 4 (embodiment 10), sample There is not adverse reaction in 5 (embodiments 16), sample 6 (embodiment 17), sample 7 (embodiment 18).

Comprehensive 0.5h and result for 24 hours and according to the requirement of 2007 " cosmetics health specifications ", are concluded that this hair Bright extract does not have adverse reaction to human skin, passes through.

Claims

1. a kind of have effects that repair the exterior-applied plant extract of skin barrier, which is characterized in that the exterior-applied plant extract It is prepared by the raw material that following weight parts match through following methods:

(2) it extracts for the first time: being 1:10~100m/m mixed raw material and solvent one according to solid-liquid ratio, extracted under the conditions of 40~90 DEG C 0.5~2h；

(3) it second extracts: being that solvent two is added in 1:10~100m/m according to solid-liquid ratio, extract 0.5 under the conditions of 40~90 DEG C~ 2h；

(4) solvent one is removed；

(5) refined filtration is to clarification to get extract；

The solvent one is one of ethyl alcohol, chloroform and acetone or a variety of mixing；

The solvent two is white oil, Parleam, Nexbase 2004, caprylic/capric triglyceride, the different tristearin of isostearic acid One of alcohol ester and vegetable oil or a variety of mixing.

2. having effects that repair the exterior-applied plant extract of skin barrier as described in claim 1, which is characterized in that the step Suddenly solid-liquid ratio is 1:10~50m/m in (2).

3. having effects that repair the exterior-applied plant extract of skin barrier as described in claim 1, which is characterized in that the step Suddenly solid-liquid ratio is 1:10~50m/m in (3).

4. having effects that repair the exterior-applied plant extract of skin barrier as described in claim 1, which is characterized in that the step Suddenly it is concentrated under reduced pressure into (4) using 40~80 DEG C and completely removes solvent one.

5. having effects that repair the exterior-applied plant extract of skin barrier as described in claim 1, which is characterized in that the step Suddenly (5) use the filter plate refined filtration in 0.2~10 μm of aperture.

6. having effects that repair the exterior-applied plant extract of skin barrier as described in claim 1, which is characterized in that the step Suddenly further include cooling step before (5) refined filtration, be cooled to 40 DEG C or 40 DEG C or less.

7. having effects that repair the exterior-applied plant extract of skin barrier, spy as described in any one of claim 1 to 6 Sign is, further includes 60~100 mesh coarse filtration between step (3) and step (4).

8. having effects that repair the exterior-applied plant extract of skin barrier as claimed in claim 7, which is characterized in that described thick Further include cooling step before filter, is cooled to 40 DEG C or 40 DEG C or less.

9. having effects that repair the exterior-applied plant extract of skin barrier, spy as described in any one of claim 1 to 6 Sign is that the raw material pre-processes before first time extracts, the pretreated step are as follows:

(1) raw material coarse crushing: is crushed to 20~60 mesh；

(2) high temperature high pressure process；

(3) dry.

10. having effects that repair the exterior-applied plant extract of skin barrier as claimed in claim 9, which is characterized in that described The condition of high temperature and pressure is: the raw material after coarse crushing 100~130 DEG C, handles 5~30min in 0.1~0.2MPa.

11. having effects that repair the exterior-applied plant extract of skin barrier as claimed in claim 9, which is characterized in that described Drying condition is 50~80 DEG C of dry 1~2h.

12. having effects that repair the exterior-applied plant extract of skin barrier as claimed in claim 7, which is characterized in that described Raw material pre-processes before first time extracts, the pretreated step are as follows:

(1) raw material coarse crushing: is crushed to 20~60 mesh；

(2) high temperature high pressure process；

(3) dry.

13. having effects that repair the exterior-applied plant extract of skin barrier as claimed in claim 12, which is characterized in that described High temperature high pressure process condition is: the raw material after coarse crushing handles 5~30min under the conditions of 0.1~0.2MPa, 100~130 DEG C.

14. having effects that repair the exterior-applied plant extract of skin barrier as claimed in claim 12, which is characterized in that described Drying condition is dry 1~2h at 50~80 DEG C.

15. exterior-applied plant extract described in any one of claim 1 to 6 has effects that repair the change of skin barrier in preparation Application in cosmetic.

16. exterior-applied plant extract described in claim 7 has effects that repair the application in the cosmetics of skin barrier in preparation.

17. a kind of have effects that repair the cosmetics of skin barrier, which is characterized in that the cosmetics are by claim 1 to 6 Exterior-applied plant extract and cosmetic field described in any one are subjected to auxiliary material and are made.

18. cosmetics as claimed in claim 17, which is characterized in that the cosmetics are oil-type cosmetics.

19. a kind of have effects that repair the cosmetics of skin barrier, which is characterized in that the cosmetics are as described in claim 7 Exterior-applied plant extract and cosmetic field are often made of auxiliary material.

20. a kind of have effects that repair the cosmetics of skin barrier, which is characterized in that the cosmetics are as described in claim 8 Exterior-applied plant extract and cosmetic field are often made of auxiliary material.

21. a kind of have effects that repair the cosmetics of skin barrier, which is characterized in that the cosmetics are as described in claim 9 Exterior-applied plant extract and cosmetic field are often made of auxiliary material.

22. a kind of have effects that repair the cosmetics of skin barrier, which is characterized in that the cosmetics are as described in claim 12 Exterior-applied plant extract and cosmetic field are often made of auxiliary material.

23. a kind of have effects that repair the cosmetics of skin barrier, which is characterized in that the cosmetics are matched by following weight parts Raw material be made:

Phytosterin ester 1~4, bisabolol 0.2~0.5, sunflower oil 5~10, Purple Perilla Seed Oil 5~10, claim 1 to 6 Any one of described in exterior-applied plant extract 65~85, butyl hydroxytoluene 0.1~0.3.

24. a kind of preparation method of cosmetics described in claim 23, which is characterized in that the step of preparation method is as follows:

(1) each raw material is weighed according to the proportion described in claim 23；

(2) phytosterin ester and butyl hydroxytoluene are added in the exterior-applied plant extract, the heating stirring at 50~60 DEG C Dissolve 20~40min；