KR20170111528A

KR20170111528A - Manufacturing method of sasa querlpaertensis nakai extract using high temperature-alkali extraction technique and cosmetic compostion comprising the extract

Info

Publication number: KR20170111528A
Application number: KR1020160037135A
Authority: KR
Inventors: 구창섭; 서수경; 장동일; 김대현
Original assignee: 주식회사 콧데
Priority date: 2016-03-28
Filing date: 2016-03-28
Publication date: 2017-10-12
Also published as: KR102017572B1

Abstract

The present invention relates to a cosmetic composition containing as an active ingredient an extract of Cheju bamboo sake extract using a high temperature-alkaline extraction technique (HTAE Technique) and a extract of Cheju bamboo sword prepared by a high temperature-alkali extraction technique . The extract of Jeju Sasa prepared by the high temperature-alkali extraction method developed in the present invention contains p-coumaric acid at a concentration of 10% or more at a high concentration as compared with the extract prepared by other extraction methods, And a large amount of efficacy components, which can maximize the effects of the active ingredients.

Description

[0001] The present invention relates to a method for preparing a high-temperature-alkali extraction extract of Jeju berry, and a cosmetic composition containing the extract,

The present invention not only contains p-coumaric acid at a high concentration of 10% or more, but also includes various kinds and a large amount of efficacy components compared with extracts prepared by using other extraction methods, (High Temperature-Alkali Extraction Technique (HTAE Technique)) capable of maximizing the temperature of the skin, and a cosmetic composition containing as an active ingredient an extract of Jeju Sasa prepared by a high temperature-alkali extraction technique will be.

Jeju Sori is one of the most abundant plant species in the Jeju Island forest. Jeju Sasa (rice field) has been used for edible bamboo leaves, and dried leaves have been used for the production of leaf tea for the treatment of diabetes and gastritis. Among the compounds constituting the plant, p-coumaric acid has already been identified.

Korean Patent Application No. 2005-59961 discloses a bamboo sake berry leaf having an anti-oxidizing activity, an anti-inflammatory activity, a tyrosinase inhibiting activity and a melanin production inhibitory activity as an extract obtained from a preparation Sasa leaf The extracts are described.

Korean Patent Application No. 2007-134908 describes a method for purifying para-coumaric acid from a bamboo sake, and a method for purifying p-coumaric acid from a bamboo sake berry in a functional cosmetic and pharmaceutical composition using the para-coumarinic acid .

In this prior art document, a method of extracting an active ingredient from a bamboo sake berry is extracted with hot water extraction method and 30% to 80% ethanol, followed by filtration and concentration. The concentrate is then extracted with methylene chloride, chloroform chloroform and n-hexane, and then the fraction is added to ethyl acetate, methyl acetate, n-butanol, isopropanol, and the like And extracting the active ingredient.

However, since the extraction yield and the content of the active ingredient are very low, it is difficult to realize the desired efficacy with the practical application amount, and thus a need for a new extraction method has arisen.

1. Korean Patent Application No. 2005-59961 2. Korean Patent Application No. 2007-134908

Accordingly, the present invention has been researched in order to find an extraction method which can not only contain p-coumaric acid (p-coumaric acid) at a high concentration of 10% or more, but also contain various kinds and a large amount of effective ingredients As a result, Jeju Bacillus subtilis extract prepared by high temperature-alkali extraction method contained not only high concentration of p-coumaric acid (p-coumaric acid) more than 10% but also various kinds and a large amount of effective ingredient, Activity, anti-inflammatory activity and whitening effect are maximized, and the present invention has been completed.

Accordingly, it is an object of the present invention to provide a method of extracting Jeju bamboo sake extracts containing high purity of p-coumaric acid at a high concentration of 10% or more using various high-temperature and alkali extraction techniques, And a cosmetic composition containing the extract as an active ingredient.

According to an aspect of the present invention, there is provided a method for preparing an extract of Jeju bamboo sake, which comprises the step of extracting alkali at a high temperature of 80 to 130 ° C.

In the preparation method of the present invention, it is preferable that the alkali is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium hydrogencarbonate and sodium carbonate.

In the method for producing the extract of Sasa extract according to the present invention,

The Jeju sake berry and the alkali may be mixed in a weight ratio of 1: 0.01 to 1: 100.

The preparation method of the present invention may further include a step of neutralizing, filtering, concentrating and extracting the extracted hot alkali extracted extract.

According to another aspect of the present invention, there is also provided a method for preparing an extract of Jeju sake bran extract, comprising the step of extracting hot alkali at a high temperature of 80 to 130 ° C, Thereby providing a cosmetic composition.

In the cosmetic composition according to the present invention, the Jeju bamboo sake extract is contained in an amount of 0.001 to 20% by weight based on the total weight of the composition, and exhibits excellent antioxidative, anti-inflammatory and whitening effects.

The extract of Jeju Sasa prepared by the high temperature-alkali extraction method according to the present invention contains p-coumaric acid at a concentration as high as 10% or more as compared with the extract prepared by other extraction methods, It contains a large amount of efficacy components, which can maximize the effects of the active ingredients.

The extract of Jeju Sori provided by the present invention can be used as a cosmetic composition for antioxidant, anti-inflammation and whitening because it inhibits DPPH radical scavenging activity, NO production inhibitory activity and melanin synthesis and is also excellent in whitening effect.

The present invention provides a method for producing a Jeju bamboo sake extract comprising a high temperature alkaline extraction step of treating a bamboo sake bamboo bowl with an alkali at a high temperature of 80 to 130 ° C.

In addition, the present invention provides a cosmetic composition comprising as an active ingredient an extract of Jeju Bacillus subtilis prepared by the high temperature-alkali extraction technique.

Hereinafter, the present invention will be described in detail with reference to Examples and Test Examples.

The present invention relates to a process for preparing a lignin polyphenol component and a high content of p-coumaric acid and ferulic acid (hereinafter referred to as " ferulic acid) can be extracted. In addition, since a large amount of the active ingredients can be extracted, the effect of the active ingredients can be maximized.

The method for preparing the extract of the present invention comprises a high temperature alkali extraction step of treating the bamboo sake bran with alkali at a high temperature of 80 to 130 ° C. Further, it may further include a step of neutralizing, filtering, concentrating and extracting the solvent with the extracted hot alkali extract.

The process for preparing the extract of the present invention using the high temperature-alkali extraction method of the present invention will be described step by step.

1) a hot alkali extracting step of treating the bamboo sake bobbins with alkali at a high temperature of 80 to 130 캜;

Deg.] C at 80 to 130 [deg.] C. The active ingredients are not sufficiently extracted at a temperature lower than 80 캜 and alkali hydrolysis is carried out at a temperature within the above range since the increase in the extraction of the active ingredient is insignificant compared with the high temperature at a temperature higher than 130 캜. The most preferable temperature is 110 to 125 ° C, and the efficiency is most excellent when the extraction amount of the active ingredient and the amount of destruction in the extraction process are considered at this temperature.

The alkali which can be used in the present invention is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium bicarbonate, and sodium carbonate.

It is preferable that the above-mentioned sake bran and alkali are mixed in a weight ratio of 1: 0.01 to 1: 100. If the ratio is less than 1: 0.01, the amount of the alkali is too small to extract the active component properly. If the ratio is more than 1: 100, the amount of the extracted component is insufficient relative to the amount of alkali to be added, which is rather inefficient.

2) neutralizing the alkaline degraded solution;

In step 1), the alkali hydrolyzed solution may be neutralized to prevent the deterioration of the active ingredient. As the acid usable in the present invention, there may be used hydrochloric acid, sulfuric acid, acetic acid and the like which are conventionally known in the art. For example, hydrochloric acid is added to adjust the pH to 2.0 to 7.0, A crude alkaline hydrolyzate extract solution of the present invention can be obtained.

3) filtering the neutralized solution;

The crude solution of the extract of the extract of the extract of the extract of the present invention is removed by filtration to remove impurities in the extract of the extract of the extract of the present invention. As a filtration method usable in the present invention, any method common in the art can be used. For example, a crude filtrate of alkaline hydrolysis extract of a bamboo sake berry having impurities removed can be obtained by passing through a fine filter paper.

4) concentrating the filtered solution;

The stock solution of Jeju bamboo sake extract filtered in step 3) is concentrated to reduce the amount of the solvent used in step 5). Vacuum concentration methods conventionally used in the art can be used at this time.

5) solvent extraction of the concentrated solution;

The extract is extracted with an appropriate solvent to enhance the content of the active ingredient from the extract of the extract of the extract of the present invention. At this time, any solvent commonly used in the art can be used, but it is preferably extracted using ethanol, acetonitrile, ether, methanol, butanol, ethyl acetate or isopropanol, or a mixed solvent thereof.

Another object of the present invention is to provide a cosmetic composition containing a bamboo sake extract prepared by the above hot-alkali extraction method.

The cosmetic composition containing the extract of Jeju Bacillus subtilis prepared by the high temperature-alkali extraction method of the present invention inhibits DPPH radical elimination effect, NO production inhibitory activity and melanin synthesis and is also excellent in whitening effect, so that the composition for cosmetic composition for antioxidant, anti- Can be used.

The extract of the present invention is contained in an amount of 0.001 to 20% by weight, more preferably 0.1 to 20% by weight, based on the total weight of the composition. If the content is less than 0.001% by weight, the effect is insignificant. If the content is more than 20% by weight, the increase in the effect is not so large as compared with the content, which is rather inefficient.

The cosmetic composition of the present invention can be used for cosmetics such as softening longevity, astringent lotion, nutritional lotion, nutritional cream, massage cream, essence, eye cream, eye essence, cleansing cream, cleansing foam, cleansing water, pack, powder, body lotion, shampoo, A toothpaste, a mouthwash, and the like, but the present invention is not limited thereto.

Hereinafter, the present invention will be described in more detail with reference to examples and test examples, but the present invention is not limited to these examples.

[ Example 1] Preparation of Jeju Sori Extract Using High Temperature-Alkali Extraction Technique

2 liters of a 2% sodium hydroxide solution was added to 100 g of a bamboo sake bamboo basket at a temperature of 121 캜 and reacted for 5 hours to obtain a hydrolyzed crude bamboo sake extract solution. Subsequently, hydrochloric acid was added to the stock solution to adjust the pH to 2.0, followed by filtration with a filter paper to remove the residue, and the filtrate was concentrated under reduced pressure. The concentrate was extracted three times with 1 liter of acetonitrile, and then the filtrate was concentrated and dried to prepare a Jeju sake extract.

[ Comparative Example 1] Preparation of Jeju Sori Extract Using High Temperature Extraction Technique

100 g of the bamboo sake balsam was extracted with 2 liters of purified water at a temperature of 121 캜, and then filtered with a filter paper to concentrate and dry to prepare a bamboo sake berry extract.

[ Comparative Example 2] Preparation of Jeju Sauce Extract Using Alkali Solution

2 liters of a 2% alkali solution was added to 100 g of a bamboo sake brewer at a temperature of 25 캜, mixed and reacted. Then, hydrochloric acid was added to the resulting solution to adjust the pH to 2.0, followed by filtration with a filter paper to remove the residue. Respectively. The concentrate was extracted three times with 1 liter of acetonitrile, and then the filtrate was concentrated and dried to prepare a Jeju sake extract.

[ Comparative Example 3] Preparation of Jeju Sori Extract Using Ethanol Extraction

100 g of the bamboo sake bran was extracted with 2 liters of ethanol at a temperature of 25 캜, and the resulting solution was filtered through a filter paper and then concentrated to dry to prepare a bamboo sake extract.

[ Comparative Example 4] Preparation of Jeju Sori Extract Using Enzyme Decomposition Technique

100 g of the bamboo sake bran was treated with glycosidase at a temperature of 25 캜, extracted with 2 L of purified water, and then filtered with a filter paper to concentrate and dry to prepare a bamboo sake berry extract.

[ Test Example 1] Comparison of the content of the extract of Jeju Sasa extract by the high temperature-alkali extraction technique of the present invention and the conventional extraction method

The content of P-quadmarin in the Jeju bacillus subtilis extracts of Example 1 and Comparative Examples 1 to 4 was analyzed by the following HPLC method. The results are shown in Table 1 below.

1) HPLC conditions

- Column: Atlantis dC18 (4.6 x 250 mm) reverse phase column (Waters)

(HPLC, SP930D; detector, UV730D; vacuum degasser & mixer, Acme 9000)

- Analysis temperature: 30 ℃

- Detection wavelength: 280 nm

- Flow rate: 1 ml / min

Elution solvent: 2% acetic acid: acetonitrile = 80: 20 (v / v)

ingredient Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 p-coumaric acid 12.09% 0.04% 0.04% 0.03% 0.02% Ferulic acid 4.70% - - - - Lignin polyphenols 83.21% - - - -

As can be seen from Table 1 above, when comparing the total polyphenol contents of the extract of Jeju Sasa extract obtained by the conventional extraction methods (Comparative Examples 1 to 4) and the extract of Jeju Sage extract prepared by the high temperature-alkali extraction method, P-coumarinic acid and total polyphenol contents of Jeju Sori extracts were about 300 ~ 600 and 2,500 ~ 5,000 times higher than the conventional extraction method, respectively. In addition, the extraction method of ferulic acid and lignin- And extracted by the extraction method according to the present invention.

Therefore, the extract of Jeju Sasa extract obtained by using the high temperature-alkali extraction method of the present invention could contain a larger amount of potency components than those using other extraction methods.

[ Test Example 2] DPPH ( Diphenylpicryl Hyrazyl ) Radical Removal effect

In order to measure the antioxidative effect of Jeju Sori extracts using the high temperature-alkali extraction method, the removal effects of DPPH radicals from the extract of Jeju Sage Extract using the high temperature-alkali extraction method of the present invention and the extracts of Comparative Examples were compared with those of the conventional method.

The removal of the DPPH radicals is a typical method of measuring the antioxidant activity. It is known that the change of absorbance caused by the reduction of the free radical 1,1-diphenyl-2-picryl hydrazyl (Diphenylpicryl Hyrazyl, DPPH) It is a method to evaluate the antioxidant ability. The degree of decrease in the absorbance of DPPH compared with that of the control group was measured, and the concentration (IC50) showing an absorbance of 50% or less of the absorbance of the control group was evaluated as the effective antioxidant concentration. The lower the IC50, the higher the radical scavenging effect and the better the antioxidant capacity.

Specifically, 190 μl of a 100 μM (in ethanol) DPPH solution and 10 μl of each of Example 1 and Comparative Examples 1 to 4 were added to prepare a reaction solution. The reaction solution was reacted at 37 ° C. for 30 minutes, Were measured. The results are shown in Table 2 below.

division IC ₅₀ ([mu] g / ml) Example 1 150 Comparative Example 1 500 Comparative Example 2 480 Comparative Example 3 510 Comparative Example 4 500

As can be seen from the above Table 2, it can be confirmed that Example 1 using the high temperature-alkali extraction technique of the present invention is 3.3 times more excellent in antioxidative ability than Comparative Examples 1 to 4.

[ Test Example 3] Measurement of nitric oxide (NO) production inhibitory activity

Cell culture was performed using a 1% antibiotic (Gibco, USA) and 10% fetal bovine serum (FBS; Gibco, Grand Island, USA) in a murine macrophage cell line RAW 264.7 cells purchased from Korean Cell Line Bank ) In Dulbecco's modified Eagle's medium (DMEM) medium at 37 ° C in a 5% CO ₂ incubator and subcultured once every two days.

RAW 264.7 cells were cultured in DMEM medium supplemented with 10% FBS at a concentration of 2.0 × 10 ⁵ cells / ml in a 24-well plate for 18 hours to evaluate the inhibitory activity of nitric oxide (NO) production. LPS was mixed at a concentration of 1 ㎍ / ㎖ in the prepared samples, and the cells were treated at the same time and cultured in a 5% CO ₂ incubator at 37 ° C for 24 hours. 100 μl of cell culture supernatant and 100 μl of Griess reagent were mixed and reacted on a 96-well plate for 10 minutes. Absorbance was measured at 540 nm. The amount of produced NO Griess reagent [1% (w / v) sulfanilamide, 0.1% (w / v) naphylethylenediamine in 2.5% (v / v) phosphoric acid] by using the NO ₂ present in the cell culture ^- in the form of And sodium nitrite (NaNO ₂ ) was used as a standard.

division IC ₅₀ ([mu] g / ml) Example 1 125 Comparative Example 1 1,003 Comparative Example 2 980 Comparative Example 3 1,005 Comparative Example 4 1,012

As can be seen from the above Table 3, it was confirmed that Example 1 using the high temperature-alkali extraction technique of the present invention was excellent in anti-inflammatory activity about 8 times as compared with Comparative Examples 1 to 4.

[ Test Example 4] Measurement of inhibitory activity of melanin biosynthesis

B16F10 cell line was purchased from Korean Cell Line Bank and 1% antibiotic (Gibco, USA) and 10% fetal bovine serum (FBS; Gibco, Grand Island, USA) The cells were cultured in Dulbecco's modified Eagle's medium (DMEM) medium at 37 ° C in a 5% CO2 incubator and subcultured once every 2 days.

In order to evaluate melanin biosynthesis inhibition activity, B16F10 cells cultured in DMEM medium were inoculated into a 24-well plate at 2.0 × 10 ⁴ cells / well. After incubation at 37 ℃ in 5% CO ₂ incubator for 24 hours, samples were prepared by concentration. To stimulate samples and cells at each concentration, α-MSH, a stimulant, was added at 200 nM. After incubation at 37 ° C in a 5% CO ₂ incubator for 48 hours, the culture was removed and each well was washed with phosphate buffer (pH 7.4). 1N NaOH was added to each well in an amount of 100 μl, and the cell was removed and transferred to a 1.5 ml tube. After reacting at 80 ° C for 1 hour, the absorbance was measured at 405 nm on a spectrophotometer. Inhibition of melanin biosynthesis was expressed by the absorbance reduction rate of the sample solution with and without the sample solution.

division Concentration (/ / ml) Melanin inhibition rate (%) Example 1 250 80 Comparative Example 1 250 12 Comparative Example 2 250 10 Comparative Example 3 250 15 Comparative Example 4 250 8

As can be seen from Table 4, Example 1 of the present invention using the high temperature-alkaline extraction method of the present invention showed about 80% inhibition of melanin formation, whereas Comparative Examples 1 and 4 showed a low melanin production of about 8-15% Respectively.

Claims

And a high-temperature alkaline extracting step of treating the bamboo sake bobbins with an alkali at a high temperature of 80 to 130 ° C.

The method according to claim 1, wherein the alkali is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium hydrogencarbonate, and sodium carbonate.

The method according to claim 1,
Wherein the bamboo sake balsam and the alkali are mixed at a weight ratio of 1: 0.01 to 1: 100.

The method according to claim 1,
Further comprising the step of neutralizing, filtering, concentrating, and solvent extracting the extracted hot-alkaline extract.

5. A cosmetic composition comprising as an active ingredient an extract of the extract of the present invention obtained by the production method of any one of claims 1 to 4.

[Claim 6] The cosmetic composition according to claim 5, wherein the extract of Jeju Soseki is contained in an amount of 0.001 to 20 wt% based on the total weight of the composition.

The cosmetic composition according to claim 5, wherein the cosmetic composition exhibits an antioxidative activity, an anti-inflammatory activity, and a whitening effect.