CN109498521A

CN109498521A - It is a kind of to have effects that the plant extracts of antiallergy and its application

Info

Publication number: CN109498521A
Application number: CN201811576842.6A
Authority: CN
Inventors: 张鹏; 陶志鹏
Original assignee: Guangzhou Suyan Skin Management Technology Co Ltd
Current assignee: Guangzhou Suyan Skin Management Technology Co Ltd
Priority date: 2018-12-23
Filing date: 2018-12-23
Publication date: 2019-03-22

Abstract

Have effects that the plant extracts of antiallergy and its application the present invention relates to a kind of.A kind of butterfly bush extracting flavonoids method, including drying, crushing, ethyl alcohol extract, filtering, cross macroporous absorbent resin chromatographic column, elution, vacuum freeze drying.Obtained chromocor extract has strong antihistaminicum, it is applied in Anti-allergic cosmetic, it can be used for all kinds of sensitive inflammation, there is good curative effect to allergic dermatitis, contact dermatitis, bite by mosquitos, deramatitis medicamentosa, eczema, prickly heat etc., it is mildly non-stimulated to skin, can be clearing heat and detoxicating, Shu Min is antipruritic.

Description

It is a kind of to have effects that the plant extracts of antiallergy and its application

Technical field

The present invention relates to cosmetic fields, have effects that the plant extracts of antiallergy and its application more particularly to a kind of.

Background technique

Flavones is widely present in the certain plants and berry of nature, and about more than 4,000 kinds of sum, molecular structure is not to the utmost It is identical, such as rutin sophorin, hesperidin, quercimentin, green tea polyphenols, pattern glucosides, pattern thuja acid all belong to flavones.

The effect of flavones be it is various, some flavones are strong antioxidant, can effectively remove intracorporal oxygen radical, such as Anthocyanidin can inhibit the full stage of oil peroxide to overflow, this ability for preventing oxidation be ten times of vitamin E with On, this antioxidation can prevent the degeneration of cell, aging, can also prevent the generation of cancer.Some flavones can improve Blood circulation can reduce cholesterol, and the flavones in Xiang Tianguo also contains a kind of PAF anticoagulant factor, these effects substantially reduce The disease incidence of cardiovascular and cerebrovascular disease, can also improve the symptom of cardiovascular and cerebrovascular disease.The referred to as chromocor compound of pattern thuja acid It is proved to reduce by 26% blood glucose and 39% ternary aliphatic propyl propionate in animal experiments, the effect of this reduction blood glucose is It is very magical, but more importantly its effect to collagen is stablized, therefore it is to retinopathy caused by diabetes and capillary Blood vessel embrittlement has good effect.Some flavones can inhibit the exudation of inflammatory biological enzyme, can promote wound healing and analgesic, Quercimentin is due to can be used for all kinds of allergies with strong antihistaminicum.

Loganiaceae Genus Buddleja L butterfly bushBuddleiadavidiiFranch., be distributed in more height above sea level 800~ In the hillside of 2200m, limes marginis shrubbery, it is distributed in provinces and regions such as China Shaanxi, Jiangsu, Zhejiang, Jiangxi, Hubei.It is its acrid flavour, micro- Hardship, temperature are toxic.Butterfly bush leaf is containing a variety of flavonoids such as buddleo-glucosides.With expelling wind and clearing away cold, promoting blood circulation and stopping pain, removing toxic substances desinsection The effect of.Clinically often it is used for that relieving rheumatism and cold, invigorating blood circulation and stopping pains, pain in rheumatoid joints, traumatic injury, fracture；Foot is controlled in external application Moss.

In the strong solvent of the general soluble easily in water, ethyl alcohol of flavonoid glycoside, methanol isopolarity；But it is insoluble in or insoluble in benzene, chloroform In equal organic solvents.Traditional extracting flavonoids method is mostly used ethyl alcohol and extracts, and decolourizes through macroreticular resin, then the dry preparation of elution and ?.The functional groups such as phenolic hydroxyl group, methoxyl group, methyl, isopentene group are often connected in flavone compound structure.In addition, it is also normal Glycosides is combined into sugar.Natural flavonoid compound exists mostly in the form of glycoside, and due to the type of sugar, quantity, coupled position And connecting mode difference can form various flavonoid glycoside.The carbohydrate for forming flavonoid glycoside includes monosaccharide and disaccharide, trisaccharide and acyl Change sugar.The more long then water solubility of flavone compound sugar chain is bigger.Flavone compound shows acid because having phenolic hydroxyl group in molecule more Property.Therefore, conventional alcohol extracting method, can be different because of phenolic hydroxyl group number, position when extracting flavone compound, can not extract to obtain Certain chromocor compounds.

It is, therefore, desirable to provide a kind of new scheme solves the above problems.

Summary of the invention

Primary and foremost purpose of the invention is to provide a kind of butterfly bush extracting flavonoids method, the liquor-saturated fish of great Ye provided by the invention It is butterfly bush leaf that raw material is extracted in straw colour ketone extracting method.

A kind of butterfly bush extracting flavonoids method, comprising the following steps:

(1) butterfly bush is taken to be dried, crushed into powder, be sieved to obtain butterfly bush powder；

(2) ethanol water is added into butterfly bush powder, adjusts pH value, then carries out heating extraction, obtain extracting solution；

(3) it is filtered after extracting solution is cooled to room temperature, obtains filtrate, citric acid adjusts filtrate pH value；

(4) macroporous adsorption resin chromatography column on filtrate, first with the water elution of 2-3 times of column volume；Then with 3-5 times of 30~60% second Alcohol (V/V) elution；

(5) 30~60% ethyl alcohol (V/V) eluent is collected, vacuum freeze drying obtains the drying butterfly bush of water content 1-4% Chromocor extract.

In wherein some embodiments, dry described in step (1) to set in baking oven 60 DEG C, drying to constant weight；The sieving To cross 10-40 mesh.

In wherein some embodiments, addition ethanol water described in step (2) is butterfly bush powder weight 2-5 times, wherein the volume fraction of ethyl alcohol in the solution is 60-80%, and the pH value that adjusts be that addition ammonium hydroxide makes PH in solution Value is 8.0-8.5；It is described to be extracted as extracting 40~60min at 80-90 DEG C.

In wherein some embodiments, the filtering of 200 mesh is filtered into described in step (3)；The citric acid adjusts filtrate PH It is worth to 6-6.5.

In wherein some embodiments, macroporous absorbent resin described in step (4) is D101 type, AB-8 type, HPD100 One of type, HPD200 type.

The chromocor extract obtained another object of the present invention is to provide the butterfly bush extracting flavonoids method exists The application in cosmetics is prepared, the dosage of the chromocor extract is calculated by mass percentage, and additive amount accounts for the total matter of cosmetics The 0.1-0.5wt% of amount.

A kind of toner containing butterfly bush chromocor extract of the present invention, by the group of following mass percentage It is grouped as:

PEG/PPG-17/6 copolymer 0.1-1%,

Butanediol 1-5%,

Preceding temple seaweed (APHANOTHECESACRUM) the polysaccharide 0.1-1% of water,

Glycerol 1-5%,

Beta glucan 1-5%,

Isoprene 1-3%,

1,2- hexylene glycol 0.1-1%,

Phosphoglycerol inositol choline salt 0.1-0.5%,

Hydroxy phenylpropionyl amine benzoic acid 0.1-0.5%,

Acrylic acid (ester) class/C10-30 alkylol acrylamide acid esters cross-linked polymer 0.1-0.5%,

- 9 0.1-0.5% of C12-13 Pareth,

Arginine 0.1-0.5%,

EDETATE SODIUM 0.01-0.05%,

Sodium Hyaluronate 0.01-0.05%,

Carbohydrate isomer 0.1-1%,

Butterfly bush chromocor extract 0.1-0.5% of the present invention,

Water surplus.

The present invention has the advantage that and the utility model has the advantages that

1. extracting flavonoids method of the present invention than existing alcohol extracting Flavonoids Method, has the advantage that ammonium hydroxide is added in auxiliary, can To improve the dissolution of flavone compound, the yield of extract is also promoted, and the ammonium hydroxide being added easily removes, to products molecule Structure and properties of product do not influence.

2. the chromocor extract that butterfly bush extracting flavonoids method of the present invention obtains is applied to antiallergy makeup In product, there is strong antihistaminicum, can be used for all kinds of sensitive inflammation, to allergic dermatitis, contact dermatitis, bite by mosquitos, Deramatitis medicamentosa, eczema, prickly heat etc. have good curative effect, mildly non-stimulated to skin, can be clearing heat and detoxicating, and Shu Min is antipruritic.

Specific embodiment

To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention will be made into one below Step ground detailed description, embodiments of the present invention are not limited thereto, for not specifically specified technological parameter or condition, can refer to Routine techniques carries out.

The cosmetic standard Chinese name of butterfly bush chromocor extract of the present invention can be with are as follows: butterfly bush (BUDDLEJA DAVIDII) extract.

Embodiment 1

A kind of butterfly bush chromocor extract chooses butterfly bush leaf as raw material, extracts to obtain by following steps:

(1) taking butterfly bush to set in baking oven 60 DEG C, drying to constant weight, is ground into powder, crosses 10 meshes and obtains butterfly bush powder End；

(2) 5 times of butterfly bush powder weight of ethanol water is added to butterfly bush powder

In end, at 80 DEG C, 60min is extracted, extracting solution is obtained；The wherein volume of ethyl alcohol in the solution

Score is 60%, ammonium hydroxide is added, the pH value in solution is made to be 8.5；

(3) after extracting solution is cooled to room temperature, the filtering of 200 mesh obtains filtrate, and it is 6 that filtrate citric acid, which adjusts pH value,；

(4) macroporous adsorption resin chromatography column on filtrate, first with the water elution of 2 times of column volumes；Then with 5 times of 30% ethyl alcohol (V/V) Elution；Wherein the macroporous absorbent resin is D101 type；

(5) 30% ethyl alcohol (V/V) eluent is collected, the drying butterfly bush flavones that vacuum freeze drying obtains water content 1% mentions Object is taken, the chromocor extract obtained through this embodiment, yield 7.1%.

Embodiment 2

(1) taking butterfly bush to set in baking oven 60 DEG C, drying to constant weight, is ground into powder, crosses 40 meshes and obtains butterfly bush powder End；

(2) ethanol water for being added 2 times of butterfly bush powder weight, at 90 DEG C, is extracted into butterfly bush powder 40min obtains extracting solution；Wherein the volume fraction of ethyl alcohol in the solution is 80%, and ammonium hydroxide is added and makes the pH value in solution to be 8.0；

(3) after extracting solution is cooled to room temperature, the filtering of 200 mesh obtains filtrate, and it is 6.5 that filtrate citric acid, which adjusts pH value,；

(4) macroporous adsorption resin chromatography column on filtrate, first with the water elution of 3 times of column volumes；Then with 3 times of 60% ethyl alcohol (V/V) Elution；The wherein macroporous absorbent resin AB-8 type；

(5) 60% ethyl alcohol (V/V) eluent is collected, the drying butterfly bush flavones that vacuum freeze drying obtains water content 4% mentions Object is taken, the chromocor extract obtained through this embodiment, yield 7.9%.

Embodiment 3

A kind of butterfly bush chromocor extract is chosen butterfly bush leaf as raw material, is passed through

Following steps are extracted to obtain:

(1) taking butterfly bush to set in baking oven 60 DEG C, drying to constant weight, is ground into powder, crosses 20 meshes and obtains butterfly bush powder End；

(2) ethanol water for being added 3 times of butterfly bush powder weight, at 85 DEG C, is extracted into butterfly bush powder 50min obtains extracting solution；Wherein the volume fraction of ethyl alcohol in the solution is 70%, and ammonium hydroxide is added and makes the pH value in solution to be 8.2；

(3) after extracting solution is cooled to room temperature, the filtering of 200 mesh obtains filtrate, and it is 6.3 that filtrate citric acid, which adjusts pH value,；

(4) macroporous adsorption resin chromatography column on filtrate, first with the water elution of 3 times of column volumes；Then with 4 times of 45% ethyl alcohol (V/V) Elution；Wherein the macroporous absorbent resin is HPD200 type；

(5) 45% ethyl alcohol (V/V) eluent is collected, the drying butterfly bush flavones that vacuum freeze drying obtains water content 2% mentions Object is taken, the chromocor extract obtained through this embodiment, yield 8.2%.

Comparative example 1

(2) ethanol solution for being added 3 times of butterfly bush powder weight, at 85 DEG C, is extracted into butterfly bush powder 50min obtains extracting solution；Wherein the volume fraction of ethyl alcohol in the solution is 70%；

(4) macroporous adsorption resin chromatography column on filtrate, first with the water elution of 3 times of column volumes；So

It is eluted afterwards with 4 times of 45% ethyl alcohol (V/V)；Wherein the macroporous absorbent resin is HPD200 type；

(5) 45% ethyl alcohol (V/V) eluent is collected, the drying butterfly bush flavones that vacuum freeze drying obtains water content 2% mentions Object is taken, the chromocor extract obtained through the method, yield 5.4%.

Comparative example 2

A kind of butterfly bush chromocor extract chooses butterfly bush herb as raw material, extracts to obtain by following steps:

Butterfly bush sets in baking oven 60 DEG C, and drying to constant weight, is ground into powder, crosses 20 meshes, and butterfly bush powder is with 95% Alcohol reflux 4 times, combined extract, after recycling design medicinal extract, medicinal extract is suspended in water, petroleum ether, acetic acid second are successively used Ester extraction, respectively obtains petroleum ether extract (part A), acetic acid ethyl ester extract (part B).Remainder is dissolved through water, mistake Filter, filtrate obtain ethanol elution object (C portion) through HPD200 type large pore resin absorption column, with 95% ethanol elution.With silicagel column color Rough segmentation B, C portion are composed, is alternately purified through polyamide column chromatography and silica gel column chromatography, directly vacuum freeze drying obtains after water redissolves The drying butterfly bush flavones of water content 2%, the flavones obtained through the method, yield 5.6%.

Test 1 general flavone purity detecting

1. the preparation of reference substance solution

Precision weighs control substance of Rutin 5mg, sets in 25mL brown volumetric flask, is diluted to scale after being dissolved with a small amount of methanol solution, Obtain the rutin contrast solution that concentration is 0.2mg/mL.

2. the preparation of standard curve

Precision measures control substance of Rutin solution 0mL, 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, is respectively placed in 25mL volumetric flask, respectively Add water to 6 .0mL, add 5% sodium nitrite solution 1mL, mix, place 6min after plus 1% sodium hydroxide test solution 10mL, finally plus Water shakes up to scale, places 15min.Absorbance value, using absorbance value as ordinate, reference substance concentration are measured at 510nm (mg/mL) it is abscissa, draws standard curve, and find out normal equation.

3. sample measures

It is accurate respectively to measure chromocor extract obtained by 1.0mL embodiment 1-3 and comparative example 1-2

100 times of dilutions (should suitably dilute if the flavonoid concentration height in sample and take 1.0mL for chromogenic assay again), set In 25mL volumetric flask, absorbance is measured in accordance with the law from " adding water to 6.0mL " according to the method under " preparation of standard curve " item Value is calculated from the concentration (mg/mL) for reading general flavone in test solution on standard curve by calculation formula up in sample General flavone purity, the results are shown in Table 1, calculation formula:

X=C × V2/V1

X is general flavone content in sample, unit mg/mL

C is from the concentration for checking in general flavone in test solution on standard curve, unit mg/mL；

V1 is that sample measures volume, unit mL；

V2 is sample constant volume, unit mL.

General flavone purity in the different embodiments of table 1

Experiment conclusion: for the general flavone purity of embodiment 1-3 compared with comparative example 1-2, purity is higher.

Test 2 butterfly bush chromocor extract antioxidant activity abilities

The antioxidant activity ability of chromocor extract is made using DPPH method measurement embodiment 1-3 and comparative example 1-2.Prepare a system VC solution is arranged, takes the VC solution of 1mL various concentration respectively, 5mLDPPH reagent is added, reacts 30min at room temperature, then exists The absorbance slip that DPPH solution is measured under 500nm, draws the homologous thread of VC concentration and DPPH elimination factor, and absorbance subtracts VC has been corresponded to the removal rate of DPPH less.Extracting flavonoids are made to the embodiment 1-3 and comparative example 1-2 of same dilution various concentration Object measures its DPPH elimination factor, and the corresponding VC content of flavones is made by eliminating rate conversion embodiment 1-3 and comparative example 1-2.Number It is repeated three times according to every group of experiment of processing, experimental data is expressed as average value.Experimental result is as shown in table 2:

2 DPPH removal rate record sheet of table

Experiment conclusion: chromocor extract made from embodiment 1-3 and comparative example 1-2 has good DPPH removal rate, illustrates have There is good senile-resistant efficacy.Wherein the DPPH removal rate of the obtained chromocor extract of embodiment 1-3 is relatively more preferable.

Embodiment 4

The toner 1-3 and control group 1-2 formed as shown in table 3 is prepared, is grouped as by the group of following mass percentage:

3 toner formula table of table

Test 3 crowds test on probation

Crowd's inclusion criteria: clinical manifestation allergic dermatitis, contact dermatitis, bite by mosquitos, deramatitis medicamentosa, eczema, Prickly heat etc., especially using after cosmetics, there is a series of symptom, it is repeatedly refractory (only for sensitive group with face, hand, Crowd based on foot；Exclude severe allergy, systemic anaphylaxis and other patients with medical sign disease).

According to above crowd's inclusion criteria, trial volunteer 250 are selected.Male 88, female 162；Age is 16~45 In year, 5 groups are divided into, every group of 50 people.

Methods of clinical observation and criterion of therapeutical effect

1, sample application method:

After daily face cleaning, sample obtained by toner 1-3 and control group 1-2, once in the morning and once at night, each dosage are applied in sensitive part For 0.1g/10cm², statistical data after 1 week.

2, curative effect determinate standard (1) is cured: clinical symptoms disappear, skin restores to normal condition, there is clean and smooth table Face, without cuticula.(2) effectively: clinical symptom relief, pruritis mitigate, and skin makes moderate progress；(3) invalid: clinical condition Shape, pruritis do not improve.

3, result

See Table 4 for details for the use observation situation of toner 1-3 and control group 1-2.

4 test recording table of table

2, interpretation of result

(1) using after sample 1 week of toner 1-3 to all kinds of inflammation, itch effective percentage up to 90% or more (47).With compare Group 1-2 comparison it is found that butterfly bush chromocor extract made from preparation method of the present invention has a better antiallergy, relieving itching with Remove Inflammatory effects；Especially allergic dermatitis, contact dermatitis, bite by mosquitos, deramatitis medicamentosa, eczema, prickly heat etc. are caused All kinds of symptoms have good effect, it is mildly non-stimulated to skin, can be clearing heat and detoxicating, Shu Min is antipruritic.

The discovery of subject's trial state is counted, the subject with severe allergic dermatitis uses toner 1-3 sample 1 week Afterwards, it has been observed that skin restores to normal condition, and there is clean and smooth surface to illustrate of the present inventionization without cuticula Adornment water has senile-resistant efficacy.Also, through detecting, the immunoglobulin E and histamine in subject's blood of toner 1-3 are used Horizontal significantly reduce 57.80% and 59.41% respectively.There is constant thickness and surface light using the subject of toner 1-3 Sliding epidermis, and there is the knot hoof tissue being upwardly formed in more constant side, show that allergic inflammation patient restores normal.

Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.

Claims

1. a kind of butterfly bush chromocor extract chooses butterfly bush leaf as raw material, which is characterized in that pass through following step Rapid extract obtains:

2. butterfly bush chromocor extract according to claim 1, which is characterized in that drying described in step (1) is Setting in baking oven 60 DEG C, drying to constant weight；The sieving was 10-40 mesh.

3. butterfly bush chromocor extract according to claim 1, which is characterized in that

Addition ethanol water described in step (2) is 2-5 times of butterfly bush powder weight, and wherein ethyl alcohol is in the solution Volume fraction is 60-80%, ammonium hydroxide is added, the pH value in solution is made to be 8.0-8.5；It is described to be extracted as extracting 40 at 80-90 DEG C ~60min.

4. butterfly bush chromocor extract according to claim 1, which is characterized in that step is filtered into described in (3) The filtering of 200 mesh；The citric acid adjusts filtrate pH value to 6-6.5.

5. butterfly bush chromocor extract according to claim 1, which is characterized in that macropore described in step (4) Absorption resin is one of D101 type, AB-8 type, HPD100 type, HPD200 type.

6. butterfly bush chromocor extract according to claim 1-5 is preparing the application in cosmetics, It is characterized in that, the dosage of butterfly bush chromocor extract is calculated by mass percentage, and additive amount accounts for cosmetics gross mass 0.1-0.5wt%.

7. application according to claim 6, which is characterized in that the cosmetics are toner.

8. a kind of toner containing butterfly bush chromocor extract as described in any one in claim 1-5, feature exist In being grouped as by the group of following mass percentage: