阅读说明：本技术 一种欧蓍草提取物的提取方法及应用 (Extraction method and application of yarrow extract ) 是由 杨凯 辛英祥 孙学磊 于 2020-12-30 设计创作，主要内容包括：本申请涉及植物提取技术领域,具体公开了一种欧蓍草提取物的提取方法及应用。一种欧蓍草提取物的提取方法,包括以下步骤：将欧蓍草粉碎,对欧蓍草粉末进行酶解浸提；微滤,收集滤液,即得欧蓍草粗提液；将欧蓍草粗提液进行超滤,收集超滤滤液；将超滤滤液进行浓缩、脱盐,即得欧蓍草提取物；欧蓍草提取物包括有机酸和黄酮。本申请的提取方法从欧蓍草中提取多种有效成分,且提取分离率较高,最大程度保证欧蓍草有效成分不被破坏,使欧蓍草提取物用于化妆品中具有较好的提亮肤色、抗炎、抑制色素沉着等效果。(The application relates to the technical field of plant extraction, and particularly discloses an extraction method and application of a yarrow extract. A method for extracting Achillea millefolium extract comprises the following steps: pulverizing milfoil, and performing enzymolysis extraction on the powder; microfiltering, and collecting filtrate to obtain coarse extract of milfoil; ultrafiltering the coarse extract, and collecting the filtrate; concentrating and desalting the ultrafiltration filtrate to obtain Achillea millefolium extract; the extract of Achillea millefolium comprises organic acid and flavone. The extraction method of the application extracts a plurality of effective components from the milfoil, has high extraction and separation rate, ensures that the effective components of the milfoil are not damaged to the maximum extent, and ensures that the milfoil extract has good effects of brightening skin color, resisting inflammation, inhibiting pigmentation and the like when being used in cosmetics.)

1. A method for extracting an extract of yarrow, comprising the steps of:

s1, pulverizing milfoil, and performing enzymolysis and extraction on the milfoil powder;

s2, microfiltration, and collecting filtrate to obtain the coarse extract of milfoil;

s3, performing ultrafiltration on the coarse extract of the milfoil, and collecting ultrafiltration filtrate;

s4, concentrating and desalting the ultrafiltration filtrate to obtain Achillea millefolium extract;

the extract of Achillea millefolium comprises organic acid and total flavone.

2. The method for extracting Achillea millefolium extract according to claim 1, wherein the enzyme used in the enzymatic leaching in S1 is selected from one or more of cellulase, pectinase, papain and pepsin, and the ratio of the added amount of the enzyme to the dry weight of the Achillea millefolium powder is (2.1-5.5): 1000.

3. The method for extracting yarrow extract according to claim 2, wherein the solvent used in S1 is deionized water, and the ratio of the weight of the solvent to the dry weight of the yarrow powder is (5-20): 1.

4. The method for extracting Achillea millefolium L.extract according to claim 3, wherein the extraction temperature in S1 is set at 30-50 deg.C, and the extraction is repeated 1-3 times, and the extraction time for each time is 0.5-2 h.

5. The method of claim 4, wherein a chelating agent is further added during the enzymatic digestion of S1.

6. The method for extracting Achillea millefolium L.extract as claimed in claim 1, wherein in S2, the microfiltration membrane is ceramic membrane or polypropylene membrane.

7. The method of extracting yarrow extract according to claim 1, wherein the ultrafiltration membrane has a cut-off molecular weight of 1K to 10K in S3.

8. The method for extracting Achillea millefolium extract as claimed in claim 1, wherein the concentration in S4 is performed by nanofiltration, and the molecular weight cut-off of the nanofiltration membrane is 150-250; desalting by reverse osmosis.

9. Use of an extract of yarrow in a skin care product.

Technical Field

The application relates to the technical field of plant extraction, in particular to an extraction method and application of an extract of achillea millefolium.

Background

Achillea millefolium L, also known as yarrow, is a perennial herb of the genus Achillea of the family Compositae, which is pungent, bitter, cold in nature and frequently used as an anti-inflammatory, analgesic, antispasmodic agent.

More and more components in the milfoil are discovered in recent years, for example, the total organic acid of the milfoil has the effects of resisting bacteria, diminishing inflammation, relieving fever and easing pain and is published in journal, and for example, some documents report that flavonoid glycoside in the milfoil can reduce melanosome transportation and melanocyte dendritic growth so as to inhibit melanin transportation to keratinocytes, thereby achieving certain skin color brightening effect, and some cosmetic material companies also extract effective parts of the milfoil for improving skin glossiness and increasing epidermis thickness, so that the extract of the milfoil can be inferred to have certain effect of improving pigmentation.

The yarrow contains a plurality of effective components such as organic acid, flavonoid glycoside and the like, in the related technology, the extraction of the yarrow is usually carried out aiming at the extraction and separation of single components, however, the plurality of effective components in the yarrow play a certain role in the whole drug effect, and the synergistic effect exists among the effective components, so the extraction method of the yarrow extract is to be improved.

Disclosure of Invention

The application provides an extraction method and application of an extract of achillea millefolium, aiming at extracting various active ingredients from the achillea millefolium and simultaneously improving the content of the active ingredients in the extract of the achillea millefolium so that the extract of the achillea millefolium has better effects of resisting inflammation, inhibiting pigmentation and the like when being used in cosmetics.

In a first aspect, the present application provides a method for extracting an extract of milfoil, which adopts the following technical scheme:

a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing milfoil, and performing enzymolysis and extraction on the milfoil powder;

s2, microfiltration, and collecting filtrate to obtain the coarse extract of milfoil;

s3, performing ultrafiltration on the coarse extract of the milfoil, and collecting ultrafiltration filtrate;

s4, concentrating and desalting the ultrafiltration filtrate to obtain Achillea millefolium extract;

the extract of Achillea millefolium comprises organic acid and total flavone.

By adopting the technical scheme, the yarrow extract is obtained by multiple steps, the extraction separation rate can be improved, the effective components of the yarrow are not damaged to the maximum extent, and the membrane separation technology is utilized to purify and remove impurities from the crude extract of the yarrow to finally obtain the yarrow extract. The obtained extract exists in the form of aqueous solution, and is easy to use in formula, and simultaneously, because impurities such as polysaccharide, protein, inorganic salt, tannin, etc. are removed by filtration, the stability of formula system can be ensured. The yarrow extract extracted by the extraction method can be added into the skin care product to improve the effects of diminishing inflammation, repairing skin, brightening skin and the like of the skin care product.

Preferably, the enzyme used in the enzymatic digestion in S1 is selected from one or more of cellulase, pectinase, papain and pepsin, and the ratio of the added amount of the enzyme to the dry weight of the milfoil powder is (2.1-5.5): 1000.

By adopting the technical scheme, the yarrow extract is extracted by using a complex enzyme low-temperature extraction method, the extraction content is high, the operation is simple, and meanwhile, the extraction temperature is low, so that the condition that the effective components are damaged due to too high temperature is reduced.

Preferably, the solvent used in S1 is deionized water, and the ratio of the weight of the solvent to the dry weight of the yarrow powder is (5-20): 1.

By adopting the technical scheme, deionized water is used as the solvent, so that the cost is saved, and the solvent is convenient to remove in the subsequent steps.

Preferably, the extraction temperature in S1 is 30-50 deg.C, the extraction is repeated for 1-3 times, and the single extraction time is 0.5-2 h.

By adopting the technical scheme, the extraction separation rate can be effectively improved and the content of the effective components in the milfoil extract can be improved by extracting for times at the temperature in the range.

Preferably, in the S1, a certain amount of chelating agent is also added during the enzymatic leaching.

By adopting the technical scheme, the chelating agent is added to chelate Ca2+ combined with the organic acid, so that the organic acid exists in a free form, and the extraction and the separation are convenient.

Preferably, in the S2, the microfiltration membrane is a ceramic membrane or a polypropylene membrane.

By adopting the technical scheme, the achillea herb residue contained after the enzymolysis and the extraction is removed through microfiltration, so that the content of solid impurities in the achillea herb crude extract is reduced, the content of effective components in the achillea herb extract is favorably improved, and the situation that an ultrafiltration membrane is blocked due to the achillea herb residue contained in the achillea herb crude extract is reduced.

Preferably, in the S3, the molecular weight cut-off of the ultrafiltration membrane is 1K-10K during ultrafiltration.

By adopting the technical scheme, macromolecular substances such as protein, polysaccharide, pigment, tannin and compounds thereof are removed by ultrafiltration, so that small molecular substances such as flavone, organic acid, sesquiterpene and the like are reserved, and the content of active ingredients such as flavone and organic acid in the yarrow extracting solution is increased.

Preferably, the concentration in the S4 is carried out by nanofiltration, and the molecular weight cut-off of the nanofiltration membrane is 150-250; desalting by reverse osmosis.

By adopting the technical scheme, the extracting solution is concentrated by nanofiltration, the method has the advantages of saving energy consumption and reducing cost, the influence of inorganic salt on the stability of the system is reduced by reverse osmosis desalination after concentration, the method is simple, the cost is saved, and the method is suitable for large-scale production.

In a second aspect, the present application provides an application of an extract of yarrow, which adopts the following technical scheme:

use of an extract of yarrow in a skin care product.

By adopting the technical scheme, the yarrow extract is applied to the skin care product, so that the melanosome transportation and the melanocyte dendrite growth can be reduced, the epidermal differentiation is promoted, the skin thickness is increased, the epidermal renewal is accelerated, and the skin color is improved. Meanwhile, the skin care product has the effects of resisting inflammation, repairing skin and the like, can relieve skin inflammation such as allergic dermatitis, irritant or allergic eczema and the like, and can effectively improve damaged skin.

In summary, the present application has the following beneficial effects:

1. according to the extraction method of the yarrow extract, during the extraction process, the yarrow powder is subjected to primary extraction by using enzymolysis and extraction, plant cell walls are destroyed by enzyme, so that effective components are dissolved out to the maximum extent, and the structures of organic acids and flavonoid components are remained without being destroyed to the maximum extent by using extraction, so that the extraction separation rate of the effective components is improved;

2. the extraction method of the yarrow extract removes pigments, polysaccharides, proteins and other large molecular substances by using a membrane separation technology, so that the yarrow extract has lighter color and better stability, has simple process and is suitable for industrial production;

3. The yarrow extract extracted by the application is applied to skin care products, and has the effects of brightening the skin color, improving the skin, resisting inflammation and the like.

Drawings

FIG. 1 is a graph showing the results of the anti-inflammatory model of cells in the third performance test of the present application;

FIG. 2 is a graph of chick embryo allantoic membrane test results of 10% yarrow extract in the fourth performance test of the present application;

FIG. 3 is a graph of the results of clinical performance tests in performance test trial five of the present application;

FIG. 4 is a graph showing the results of the clinical performance tests in the fifth performance test of the present application.

Detailed Description

The present application will be described in further detail with reference to the following drawings and examples.

Yarrow in the examples of this application was taken from Yunnan, wild;

cellulase, pectinase, papain and pepsin are all collected from Shandong Nuanli Biotech Co., Ltd;

EDTA-2Na is obtained from Jinan Zhongjie chemical Co., Ltd;

ceramic membranes were collected from delagmeir;

the polypropylene filter membrane is collected from Hangzhou micron class science and technology company;

cellulose filter membranes were collected from sartorius, germany;

the reverse osmosis membrane is adopted from Shenzhen mingsheng Jiuzhou industries, Ltd;

anion exchange resin D280 was obtained from Kunning Bai chemical Co.Ltd;

The polyamide adsorption resin is obtained from Cangzhou Zhonghuazhong environmental protection science and technology limited company;

the acrylic acid crosslinked polymer is obtained from Guangzhou Bokuming Industrial science and technology Co;

sodium hyaluronate was collected from Shanxi Huashi Biotech limited;

p-hydroxyacetophenone was collected from Hubei Jiujiulong chemical Co., Ltd;

arginine is collected from Anhui Zhonghong bioengineering Co Ltd;

butanediol, 1, 3-propanediol, glycerol, and 1, 2-pentanediol were obtained from Shandong Asahi Chen chemical science and technology Co., Ltd;

ultrafiltration system (Labscale TFF) from millipore;

the reverse osmosis equipment is selected from Tianjin Populus technology;

the ultraviolet spectrophotometer is obtained from Beijing, Kyoco, Ruida technologies, Inc., and has a model number of UV 2401.

Examples

Example 1: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g cellulase, extracting with 5L deionized water at 30 deg.C in water bath for 0.5h, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 4L filtrate to obtain coarse extract of Achillea millefolium;

S3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cutoff of 1K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 3.5L of filtrate;

s4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 150 is used, the surface pressure is 0.5MPa, and the filtrate is 1L, and then, desalting is carried out by using a reverse osmosis membrane to obtain 0.5L of filtrate, thus obtaining the milfoil extract.

Example 2: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 3.8g of cellulase, extracting with 12.5L of deionized water at 40 deg.C in water bath for 1 hr, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 10L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cutoff of 1K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 8L of filtrate;

s4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 150 is used, the surface pressure is 0.5MPa, and 2L of the filtrate is desalted by a reverse osmosis membrane to obtain 1L of the filtrate, namely the yarrow extract.

Example 3: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 5.5g cellulase, extracting with 20L deionized water at 50 deg.C in water bath for 1 hr, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 16L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cutoff of 1K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 14L of filtrate;

s4, carrying out nanofiltration concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 150 is used, the surface pressure is 0.5MPa, 4L of the filtrate is desalted by a reverse osmosis membrane, and 2L of the filtrate is obtained, namely the yarrow extract is obtained.

Example 4: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g of pectinase, extracting with 5L of deionized water in water bath at 30 deg.C for 0.5h, and cooling to room temperature to obtain extractive solution;

S2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 4L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cutoff of 1K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 3.5L of filtrate;

s4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 150 is used, the surface pressure is 0.5MPa, and the filtrate is 1L, and then, desalting is carried out by using a reverse osmosis membrane to obtain 0.5L of filtrate, thus obtaining the milfoil extract.

Example 5: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 1.05g of papain and 1.05g of pepsin, extracting with 5L of deionized water in water bath at 30 deg.C for 0.5 hr, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 4L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cutoff of 1K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 3.5L of filtrate;

S4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 150 is used, the surface pressure is 0.5MPa, and the filtrate is 1L, and then, desalting is carried out by using a reverse osmosis membrane to obtain 0.5L of filtrate, thus obtaining the milfoil extract.

Example 6: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g of cellulase, extracting with 5L of deionized water at 30 deg.C in water bath for 2 times, each time for 0.5 hr, mixing filtrates, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 8L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cutoff of 1K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 7L of filtrate;

s4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 150 is used, the surface pressure is 0.5MPa, and 2L of the filtrate is desalted by a reverse osmosis membrane to obtain 1L of the filtrate, namely the yarrow extract.

Example 7: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g of cellulase, extracting with 5L of deionized water at 30 deg.C in water bath for 3 times, each time for 0.5 hr, mixing filtrates, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 12L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cut-off of 1K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 10.5L of filtrate;

s4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein 3L of the filtrate with the surface pressure of 0.5MPa is obtained by using a ceramic filter membrane with the molecular weight cutoff of 150 during nanofiltration, and then desalting by using a reverse osmosis membrane to obtain 1.5L of the filtrate, thus obtaining the yarrow extract.

Example 8: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g cellulase, extracting with 5L deionized water at 30 deg.C in water bath for 0.5h, and cooling to room temperature to obtain extractive solution;

S2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 4L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with molecular weight cutoff of 5K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 3.5L of filtrate;

s4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 200 is used, the surface pressure is 0.5MPa, and the filtrate is 1L, and then, desalting is carried out by using a reverse osmosis membrane to obtain 0.5L of filtrate, thus obtaining the milfoil extract.

Example 9: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g cellulase, extracting with 5L deionized water at 30 deg.C in water bath for 0.5h, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 4L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cut-off of 10K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 3.5L of filtrate;

S4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 250 is used, the surface pressure is 0.5MPa, and the filtrate is 1L, and then desalting is carried out by using a reverse osmosis membrane to obtain 0.5L of filtrate, namely the milfoil extract.

Example 10: a method for extracting Achillea millefolium extract comprises the following steps:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g of cellulase and 2.5g of EDTA-2Na, extracting with 5L of deionized water in water bath at 30 deg.C for 0.5 hr, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 4L filtrate to obtain coarse extract of Achillea millefolium;

s3, performing ultrafiltration on the crude extract of Achillea millefolium by using a cellulose filter membrane with a molecular weight cutoff of 1K on an ultrafiltration system under the condition that the surface pressure is 0.5MPa, and collecting 3.5L of filtrate;

s4, carrying out nanofiltration and concentration on the ultrafiltration filtrate, wherein during nanofiltration, a ceramic filter membrane with the molecular weight cutoff of 150 is used, the surface pressure is 0.5MPa, and the filtrate is 1L, and then, desalting is carried out by using a reverse osmosis membrane to obtain 0.5L of filtrate, thus obtaining the milfoil extract.

Comparative example

Comparative example 1: an extraction method comprising the steps of:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g cellulase, extracting with 5L deionized water at 30 deg.C in water bath for 0.5h, and cooling to room temperature to obtain extractive solution;

s2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 4L filtrate to obtain coarse extract of Achillea millefolium;

s3, concentrating the coarse extract of milfoil under reduced pressure, adding ammonia water to adjust pH to 9-10, adding into anion exchange resin D280 for adsorption, controlling the outflow speed of the liquid at the lower end of the chromatographic column to be 10mL/min, eluting with 2 times of column water, 4 times of column volume of 30% ethanol solution and 4 times of column volume of 60% ethanol solution, collecting 30% ethanol eluate and 60% ethanol eluate, adding citric acid to adjust pH to 5-6, and concentrating under reduced pressure to 1.5L to obtain the final product.

Comparative example 2: an extraction method comprising the steps of:

s1, pulverizing 1kg of milfoil to obtain 1kg of milfoil powder with particle size less than 80 μm, adding 2.1g cellulase, extracting with 5L deionized water at 30 deg.C in water bath for 0.5h, and cooling to room temperature to obtain extractive solution;

S2, microfiltration of the extract, sequentially filtering with 74 μm, 5 μm and 0.22 μm ceramic filter membrane under the surface pressure of 0.5MPa, and collecting 4L filtrate to obtain coarse extract of Achillea millefolium;

s3, concentrating the crude extract under reduced pressure, loading onto polyamide adsorbent resin for adsorption, controlling the outflow rate of liquid at the lower end of the chromatographic column to be 10mL/min, eluting with 4 times of column water and 4 times of 80% ethanol solution, collecting water eluate and 80% ethanol eluate, mixing, and concentrating under reduced pressure to 1.5L.

Application examples

The application of the yarrow extract extracted by the extraction method in the skin care product has the addition amount of 3-5%.

Performance test

Test one:

for the extraction methods of examples 1 to 10 and comparative examples 1 to 2, the total organic acid content in the extract was measured using a potentiometric titration method, and the total flavone content in the extract was measured using an ultraviolet spectrophotometer, and the test results are shown in the following table 1.

As can be seen from the test data in table 1: using the method of extracting yarrow extract of examples 1-10, the extracted yarrow extract had a high organic acid content and a high total flavone content, wherein the organic acid content was greater than 7.2% and the total flavone content was greater than 9.6%.

Combining example 1 and comparative example 1, and table 1, it can be seen that the extraction method in comparative example 1 does not give a large change in the content of organic acids in the obtained yarrow extract, but the total flavone content is significantly reduced, compared to the extraction method in example 1. It is shown that when the extraction method of comparative example 1 is used to extract the yarrow extract, a part of the flavonoids are structurally destroyed under alkaline conditions, resulting in a lower content of total flavonoids in the extract, and the extraction method of comparative example 1 does not extract flavonoids well, whereas the method of example 1 can extract organic acids and total flavonoids well and increase the content of organic acids and total flavonoids in the yarrow extract.

In combination with example 1 and comparative example 2, and table 1, it can be seen that the extraction method in comparative example 1 significantly reduces the contents of organic acids and total flavonoids in the obtained extract of yarrow as compared to the extraction method in example 1. It is explained that the extraction method of comparative example 2 cannot extract organic acids and total flavonoids from yarrow well, resulting in low contents of organic acids and total flavonoids in the yarrow extract, affecting the skin-lightening, anti-inflammatory, skin-repairing, etc. effects of the yarrow extract.

TABLE 1 test results of the content of active ingredients

And (2) test II:

the yarrow extract obtained by extraction in example 1 and comparative examples 1 and 2 was applied to the essence water, and the contents of the components in the essence water were as follows:

0.15% of acrylic crosslinked polymer;

7% of polyol;

0.05% of sodium hyaluronate;

EDTA-2Na 0.05％；

0.4 percent of p-hydroxyacetophenone;

achillea millefolium extract 4%;

0.15 percent of arginine;

the balance being deionized water.

Wherein the polyalcohol is prepared by mixing butanediol, 1, 3-propanediol, glycerol and 1, 2-pentanediol according to the weight ratio of 1:1.2:0.8: 1.1.

The essence water is prepared by the following preparation processes:

adding acrylic acid cross-linked polymer into deionized water, stirring, sequentially adding polyalcohol, EDTA-2Na, sodium hyaluronate and p-hydroxyacetophenone at 75 deg.C, stirring for 10min under heat preservation, cooling to 45 deg.C, adding Achillea millefolium extract, stirring for 10min, adding arginine, and stirring for 5min to obtain essence water.

And (3) performing a stability test on the prepared essence water, wherein 4 test samples are taken from each group of essence water, each test sample is 100mL, the test samples taken from the same group of essence water are respectively placed at 25 ℃, 45 ℃, 4 ℃ and illumination conditions for 30 days, the color, precipitation and viscosity changes of the test samples are observed, and the change is counted in the following table 2.

As can be seen from the test results in table 2, the yarrow extract obtained by the extraction method of the yarrow extract in example 1 of the present application is applied to the essence water, and the essence water system has better stability, lighter color, no component and more stable viscosity.

Table 2 stability test results

And (3) test III:

the achillea extract obtained in example 1 was subjected to a cellular anti-inflammatory model test:

5% CO at 37 deg.C₂Under the conditions, RAW 264.7 cells were cultured in DMEM-H complete medium (containing 10% FBS, 1% double antibody), and RAW 264.7 cells in logarithmic growth phase were subjected to cell suspension preparation and cell plating. 100 μ L of cell suspension at a density of 50000 cells/mL, i.e., 5000 cells/well, was added to the 96-well plate, and 100 μ L of PBS buffer was added to the blank. The cells were cultured for 24 hours until a semi-confluent monolayer was formed, during which time the cells recovered their viability, adhesion and exponential growth, after the culture was completed, 0.50%, 1.00%, 1.50%, 2.00%, 2.50%, 3.00% of the extract of Achillea millefolium (solvent deionized water) extracted in example 1 and 1. mu.g/mL of LPS were added, respectively, for 24 hours, and after completion of the treatment, the supernatant was collected and assayed for IL-6 by ELISA and for cell viability by NR.

As shown in fig. 1, the yarrow extract obtained in example 1 exhibited a dose-dependent inhibitory effect on LPS-induced IL-6 in the range of 0.50% to 3.00% on RAW 264.7 cells, indicating that the yarrow extract obtained in example 1 had an inhibitory effect on the release of inflammatory factors.

And (4) testing:

taking a 10-11d embryo chicken embryo, looking at the air chamber with an egg candler, determining the position of the air chamber, twisting and drilling a small hole at the upper end of the air chamber with a hand, peeling off the eggshell part on the upper layer of the air chamber with a medical ophthalmology bent-tip forceps, exposing the white shell membrane, dripping 0.4mL of 0.9% NaCl solution by using a suction pipe to moisten the shell membrane for 3min, and slowly pouring out the 0.9% NaCl solution. Taking out the shell membrane by tweezers, carefully removing the shell membrane to reduce the damage of the allantoic membrane caused by manual operation, placing a polytetrafluoroethylene resin ring on the intact chick embryo chorioallantoic membrane as a test area of a test sample, and taking a picture by using a stereoscope to obtain the 0S state. Transferring 40 μ L of sample to be tested with a pipette and dropping into a polytetrafluoroethylene resin ring, recording the time for adding the sample and covering the air chamber with a wet preservative film, transferring the chick embryo into a constant temperature and humidity chamber, culturing at 37.7 deg.C and 60% humidity for 300S, taking a picture with a stereoscope and observing the degree of blood vessel injury, as shown in fig. 2, when the concentration of the yarrow extract extracted in example 1 is 10%, the phenomena of bleeding, blood vessel thawing and blood coagulation do not occur in 300S.

Test samples: the extract of Achillea millefolium extracted in example 1 was extracted at concentrations of 3%, 5%, 7% and 10%, and the solvent was deionized water.

On chick embryo allantoic membranes, 0.9% NaCl appeared to be non-irritating. The non-irritant behavior is as follows: each toxic effect (bleeding, vessel thawing, clotting) occurred over a time period of greater than 300 s.

The test results are shown in Table 3 below.

As can be seen from the data in Table 3, the extract of Achillea millefolium is safe and non-irritating at concentrations of less than 10%.

TABLE 3 test results

And (5) testing:

and screening questionnaires and initial values of the questionnaires by volunteers, selecting 20 qualified volunteers as test subjects to participate in the test, and randomly dividing the test subjects into 2 groups of 10 persons each. Wherein 1 group used the extract of Achillea millefolium extracted in example 1 at a concentration of 3% in deionized water as a solvent to prepare experimental group; the other 1 group used deionized water as a control group. The film is used in the morning and evening, and a group of VISA pictures is taken before smearing on day 1, and a group of VISA pictures is taken after 28 consecutive days, and the taking results are shown in FIG. 3 and FIG. 4.

Referring to fig. 3, in the experimental group, the skin brightness of the volunteers who used the extract of yarrow at a concentration of 3% was significantly increased after 28 consecutive days; referring to fig. 4, in the control group, the skin brightness was not significantly improved after continuous application with deionized water for 28 days. It is shown that the extract of yarrow has a superior effect on skin lightening.

The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.