KR102026258B1 - The method for ph-controlled sericite extract and sericite extract by the same - Google Patents

Abstract

The present invention relates to a method for preparing sericite extract. More specifically, crushing sericite to prepare a sericite powder; Pressurizing and heating the sericite powder and water into a closed container; Eluting water vapor through a pipe connected from the sealed container, eluting by adjusting the pressure of the closed container, the temperature of the closed container, the diameter of the pipe and the pressure of the eluted vapor; And condensing the eluted water vapor to obtain a sericite extract.
In particular, the sericite extract prepared through the manufacturing method is used as a cosmetic base material because it has an antimicrobial activity against the causative bacteria causing human dermatitis while the pH is controlled to enhance the functionality of the cosmetic.

Description

Method for preparing sericite extract and sericite extract prepared by the above method {THE METHOD FOR PH-CONTROLLED SERICITE EXTRACT AND SERICITE EXTRACT BY THE SAME}

The present invention relates to a method for preparing sericite extract. More specifically, crushing sericite to prepare a sericite powder; Pressurizing and heating the sericite powder and water into a closed container; Eluting water vapor through a pipe connected from the sealed container, eluting by adjusting the pressure of the closed container, the temperature of the closed container, the diameter of the pipe and the pressure of the eluted vapor; And condensing the eluted water vapor to obtain a sericite extract.

In particular, the sericite extract prepared through the manufacturing method is used as a cosmetic base material because it has an antimicrobial activity against the causative bacteria causing human dermatitis while the pH is controlled to enhance the functionality of the cosmetic.

The ideal pH of human skin is 4.7 ~ 5.75, slightly acidic, and if the acidity of skin is close to acid, it is oily skin, and if it is close to alkaline, it is dry skin. The reason for this is that the skin is weakly acidic due to secretion of lower fatty acids, ascorbic acid, lactic acid and amino acids secreted by sebaceous glands and sweat glands.

The thin acid film on the surface of the skin is a natural protective film that protects the skin from external physical and chemical damage. In general, pathogens, such as bacteria, are alkaline, making it difficult to survive in the mildly acidic environment of the skin.

Changes in the pH of the skin are closely related to the condition of the skin, the protective film and the keratin. When the pH of the skin is out of the normal range, the balance is broken and skin diseases occur.

As the skin acidity approaches alkalinity, it is easily damaged by external stimuli and causes troubles. Various bacteria are easy to invade and the skin's immunity is reduced, making it sensitive.

In addition, the skin oil and moisture balance is collapsed, and sebum is secreted vigorously secretion sebum clogging the pores, causing trouble, or lack of moisture may cause dry acne that exfoliates keratin blocking pores. It is known that the pH of acne skin is 7.5 and that of atopic skin is increased to pH 8.0.

Generally, to adjust pH, chemicals called pH adjusters or buffers are added. The types of regulators used in cosmetics include sodium anoxide (disodium phosphate), citric acid (citric acid), stearic acid and di Ammonium citrate, disodium phosphate, sodium citrate, triethanolamine, potassium phosphate and the like.

However, long-term use of these ingredients can cause skin irritation, and triethanolamine, in particular, is known to have harmful effects on eye-related diseases when accumulated in the body for a long time.

Therefore, there is a need for a technology for preparing a composition capable of maintaining the skin pH balance using natural materials without a separate pH adjuster. In particular, since a composition using natural materials can replace purified water, which is generally used as a cosmetic base material, it is urgent in that it can enhance the functionality of cosmetics.

On the other hand, the present inventors have continuously conducted research related to the illite 10-1077824 (a cosmetic composition for improving atopy containing an illite extract and a method for preparing the same), No. 10-1301249 (advanced illite Eluent eluted during the metamorphic process, preparation method thereof and cosmetics for improving skin diseases including the same), No. 10-1575793 (preparation method of illite extract pH adjusted and illite extract prepared by the above method), Has the rights of 10-1696914 (pack composition containing illite and sodium silicate as an active ingredient and preparation method thereof) and 10-1597636 (pack composition containing illite extract and pack containing the composition) Doing. In particular, Korean Patent No. 10-1575793 discloses a method for producing an illite extract by controlling the pH by adjusting the diameter of a tube connected to a sealed container and the water vapor pressure eluted from the tube.

In addition, the present inventors have completed the present invention while promoting research on the utility of sericite. (Application No. 10-2017-0161142 is an invention on the antibacterial function of sericite.) Sericite is a variant of mica that is close to the composition of mica. K1.0 (H3O) 1.0Al4 (SiAl) 8O20 (OH) 4 It is indicated by low potassium and high moisture. This ratio is not in the order of the illite, but is located between the dolomite and the illite. In other words, since sericite has a different degree of hardness and inclusions from illite, it is necessary to extract it under different conditions from illite.

Overall, the present inventors intend to manufacture a composition that can maintain the skin pH balance using sericite without a separate pH adjuster, and the sericite extract is intended to be used as a cosmetic base material that can further enhance the functionality of cosmetics. The invention has been completed.

Republic of Korea Patent Publication No. 10-1575793 (2015.12.08)

The problem to be solved of the present invention is to provide a method for producing a pH-controlled sericite extract.

The problem to be solved by the present invention is to provide a manufacturing method capable of producing a sericite extract of the desired pH by adjusting the temperature of the sealed container, the pressure, the diameter of the pipe connected to the sealed container and the vapor pressure of the elution. .

The problem to be solved of the present invention is to provide a method for producing a sericite extract having antibacterial functionality while the pH is adjusted.

The present invention comprises the steps of preparing a sericite powder by grinding sericite; Pressurizing and heating the sericite powder and water into a closed container; Eluting water vapor through a pipe connected from the sealed container, eluting by adjusting the pressure of the closed container, the temperature of the closed container, the diameter of the pipe and the pressure of the eluted vapor; And condensing the eluted water vapor to obtain a sericite extract; to provide a method of producing a pH-controlled sericite extract, characterized in that it comprises a method to solve the technical problem.

The method for preparing a sericite extract according to the present invention has an effect of maintaining the pH balance of the skin by being used as a base material of cosmetics by providing a pH adjusted sericite extract.

The sericite extract prepared according to the present invention has the effect of preventing, improving or treating dermatitis caused by the pathogen by inhibiting the proliferation of the dermatitis-induced pathogen.

Sericite extract prepared according to the present invention has the effect of preventing, ameliorating or treating the symptoms of seborrheic dermatitis, hair loss due to seborrheic dermatitis, acne and dandruff.

The terms or words used in this specification and claims are not to be construed as limiting in their usual or dictionary meanings, and the inventors may appropriately define the concept of terms in order to best describe their invention. It should be interpreted as meaning and concept corresponding to the technical idea of the present invention based on the principle that the present invention.

Therefore, the experimental examples and reference examples described herein are only one of the most preferred embodiments of the present invention and do not represent all of the technical idea of the present invention, and various equivalents and modifications that may be substituted for them at the time of the present application. It should be understood that there may be examples.

Example  1. Preparation of Sericite Extract

1) Sericite Powder Manufacturing Step

Sericite ore is milled to produce sericite powder.

The sericite rock or rock may be crushed, and the crushing may be crushed by repeating the impact repulsion by installing a crusher on the inner wall of the crusher, or may be classified by installing an additional screen or grid under the crusher. Or turbo mill, super micron mill, port mill, tube mill, conical mill, jet mill, disc mill, pin mill, stamp mill, shredder, hammer mill, hammer crusher, cone crusher, jaw crusher, cutter mill, edge runner, roller It may also be milled using mills, raymond mills and turbomicron mills or jet mills.

Preferably, sericite may be ground to a powder of 100-500 mesh size and used for extraction.

2) pressurizing and heating step

Sericite powder is placed in an airtight container, water is added, and sericite extract is prepared by pressing and heating. In this case, distilled water or purified water may be used. In the case of using tap water or ground water, it is not preferable to use mineral water and various ions in addition to pure water molecules in the water, which may affect the pH of the sericite extract.

Preferably, distilled or purified water may be added 2 to 4 parts by weight based on 1 part by weight of sericite powder.

Inside the sealed container may be a pressure of 1 ~ 200 atm, it may be heated to a temperature of 100 ~ 400 ℃. Preferably, a pressure of 100 atm and a temperature of 250 ° C. are applied.

The heating time may be variously set according to design conditions, and may be heated for 1 to 5 hours. Preferably, the heating time is 3 hours.

3) vapor elution stage

The steam generated in the sealed container is eluted through the pressurizing and heating steps.

In this case, since the pH of the sericite extract is changed according to the time for which the steam stays in the container and the rate at which the steam is eluted, the setting of the vapor dissolution condition is most important in order to obtain a pH-controlled sericite extract.

Water vapor can be eluted through a tube connected to an airtight container, which can be a tube with a diameter of 5 to 50 mm. Water vapor is eluted through the connected tube and then a sericite extract is produced through the condensation step. Preferably, a tube with a diameter of 10 mm is used.

4) Steam elution pressure control and condensation step

Sericite extract is obtained by condensing water vapor eluted from a tube connected to an airtight container.

In addition to the time the water vapor stays in the vessel, the pressure of the eluted water vapor may also affect the pH of the sericite extract. Therefore, the pressure control valve is provided in the pipe from which steam is eluted so that the valve can be opened and closed according to the pressure to finely adjust the pH of the sericite extract. Preferably, the pressure at which water vapor elutes is adjusted from 20 atm to 15 atm.

The condensation of water vapor can be carried out in a conventional manner, preferably condensation of water vapor by water cooling with cooling water.

Experimental Example  1. pH measurement of sericite extract

Using the conditions of Example 1, extraction by adjusting the pressure of the airtight container 100 atm, the temperature of the sealed container at 250 ℃, the heating time 3-5 hours, the diameter of the tube 10mm and the elution pressure of the water vapor eluted to 20 ~ 15 The pH of the prepared sericite extract is measured as follows.

Heating time 3 hours 4 hours 5 hours pH 5.78 5.02 4.60

As a result of measuring different heating times of 3, 4 and 5 hours, it can be seen that the pH of the sericite extract is all in the weakly acidic range.

Experimental Example 2. Antibacterial Test of Sericite Extract

1. Preparation for experiment

1) Laboratory: Hoseo University Biomedical Research Institute

2) Experiment Outline

This experiment was carried out to investigate the antimicrobial effect of Sericite mineral extract (when heating time is 4 hours in Example 1) against human dermatitis causative bacteria Malassezia furfur , Staphylococcus aureus Five kinds of bacteria, Staphylococcus epidermidis , Streptococcus pyogens and Propionibacterium acnes, were tested for antimicrobial effect by broth microdilution method.

That is, the minimum amount of the stock solution that inhibits the growth of each bacterial solution (1 × 10 ⁶ cfu / mL) was calculated by confirming the rate of bacterial growth inhibition at each concentration after the step dilution with azeotropic 2 using the extract as a stock solution.

3) Storage condition: room temperature

4) Disclosure bacteria

Strain Strain number Sales organization Malassezia furfur 7743 KCTC Staphylococcus aureus 6538 ATCC Staphylococcus epidermidis 12228 ATCC Streptococcus pyogens 12344 ATCC Propionibacterium acnes 29399 ATCC

5) Culture medium and culture conditions

Strain name Culture Medium *
Culture condition Agar Broth (MIC)
Malassezia furfur
Sabouraud dextorose agar
SDB 30 ± 2 ℃, non CO ₂ , 24 ~ 48h Staphylococcus aureus
5% blood agar
MH 35 ± 2 ℃, non CO ₂ , 18 ~ 24h Staphylococcus epidermidis
5% blood agar
MH 35 ± 2 ℃, non CO ₂ , 18 ~ 24h Streptococcus pyogens
5% blood agar
BHI 35 ± 2 ℃, 5% CO ₂ , 18 ~ 24h
Propiobacterium acnes
5% blood agar NIH Thioglycollate broth
35 ± 2, anaerobic 42 ~ 48h

* SDB: Sabouraud dextrose broth, MH: Mullern-Hinton broth, BHI: Brain heart infusion broth

6) Medium preparation

Preparation of Sabouraud dextorose broth: 30 g of Sabouraud dextorose broth (DIFCO 238230) was dissolved in 1 L of distilled water and sterilized at 121 ° C. for 15 minutes.

[Preparation of Mueller Hinton broth]: 21 g of Mueller Hinton broth (DIFCO 275730) was dissolved in 1 L of distilled water and sterilized at 121 ° C. for 15 minutes.

Preparation of Brain Heart Infusion broth: 37 g of Brain Heart Infusion broth (DIFCO 237500) was dissolved in 1 L of distilled water and sterilized at 121 ° C. for 15 minutes.

[Preparation of NIH Thioglycollate broth]: 29 g of NIH Thioglycollate broth (DIFCO 225710) was dissolved in 1 L of distilled water and sterilized at 121 ° C. for 15 minutes.

2. Experimental method

1) Experimental standard

This experiment was conducted according to the Clinical and Laboratory Standards Institute Document, M31-A3 (Clinical and Laboratory Standards Institute, CLSI, 2008).

2) Experiment Method

2.1) Preparation of Test Substance

Dilution was carried out in 10 steps of test substances with the azeotropic ratio 2 at the highest concentration of the extract. As the diluent used for dilution, the same broth as the inoculum of each strain was used.

2.2) Preparation of bacterial solution

[Preparation of Malassezia furfur Fungus]

Malassezia furfur was plated in Sabouraud dextorose agar and incubated for 48-72 hours in a 30 ° C incubator. Four to six single colonies were inoculated in Sabouraud dextorose broth and incubated for 12-24 hours in a 30 ° C incubator.

The turbidity of the cultured bacteria was determined by MacFarland No. The bacterial count was adjusted to 0.5 to about 1.5 × 10 ⁸ cfu / mL, and then diluted 100 times with diluent to prepare about 1.5 × 10 ⁶ cfu / mL of the inoculated bacteria solution.

[Staphylococcus aureus, Staphylococcus epidermidis fungus preparation]

Staphylococcus aureus and Staphylococcus epidermidis were plated in 5% sheep blood agar and incubated for 12-24 hours in 37 ℃, 5% CO2 incubator. Incubated for ˜6 hours. The turbidity of the cultured bacteria was determined by MacFarland No. The bacterial count was adjusted to 0.5 to about 1.5 × 10 ⁸ cfu / mL, and then diluted 100 times with diluent to prepare about 1.5 × 10 ⁶ cfu / mL of the inoculated bacteria solution.

[Preparation of Staphylococcus pyogens Fungus]

Staphylococcus pyogens were plated in 5% sheep blood agar and incubated for 12-24 hours in a 37 ° C, 5% CO2 incubator, then 4-6 single colonies were inoculated into Brain Heart Infusion broth, and then in 37 ° C, 5% CO2 incubator. Incubated for 2-6 hours. The turbidity of the cultured bacteria was determined by MacFarland No. The bacterial count was adjusted to 0.5 to about 1.5 × 10 ⁸ cfu / mL, and then diluted 100 times with diluent to prepare about 1.5 × 10 ⁶ cfu / mL of the inoculated bacteria solution.

[Prepionibacterium acnes fungus preparation]

Propionibacterium acnes were plated in 5% sheep blood agar and incubated in anaerobic jars for 48-72 hours, then 4-6 single colonies were inoculated into NIH thioglycollate broth and incubated at 37 ° C for 12-24 hours.

The turbidity of the cultured bacteria was determined by MacFarland No. The bacterial count was adjusted to 0.5 to about 1.5 × 10 ⁸ cfu / mL, and then diluted 100 times with diluent to prepare about 1.5 × 10 ⁶ cfu / mL of the inoculated bacteria solution.

2.3) Reaction and cultivation of bacterial solution and test substance

A sterile 96-well microplate (F bottom, SPL) was prepared in advance and 8 replicate wells were used for the concentration groups for each test material. 0.05 mL of sterile broth was dispensed into the wells except the first well of the prepared microplate. After dispensing 0.1 mL of the test substance into the wells of the highest concentration group, 0.05 mL of the sample was taken, and diluted step by step with azeotropes 2 and broth dispensed into the wells of the next concentration group, thereby preparing a total of nine test substance concentration groups. Each well was inoculated with 0.05 mL of the culture solution adjusted to 1.5 x 10 ⁶ cfu / mL and incubated according to the culture conditions of the bacteria.

2.4) Determination of antimicrobial effect

After incubation for 18 to 24 hours, the growth of bacteria at the concentrations was visually observed.

3. Experimental Results

1) Antibacterial Effect of Serisite Extracts

Sericite extract is at least the required amount of inhibiting the growth of _{Malassezia furfur, Staphylococcus epidermidis (MIC 50} ) to a minimum required amount (MIC ₅₀₎ of each was 114.5mL and 58.5mL inhibit the growth of Staphylococcus aureus, Streptococcus pyogens, Propionibacterium acnes bacteria were 44.0 mL, 5.28 mL, and 8.0 mL.

Strain name Sericite Extract MIC ₅₀ ^(a) MIC ₉₀ ^(b) Malassezia furfur 114.5 mL ^(c) (1.69x) ^(d) 180.0mL (3.6x) Staphylococcus aureus 44.0 mL (0.88x) 186.4mL (2.0x) Staphylococcus epidermidis 58.5 mL (1.17x) 279.0 mL (3.1x) Streptococcus pyogens 5.28 mL (0.12x) 55.5 mL (1.10x) Propionibacterium acnes 8.0mL (0.16x) 154.0 mL (3.0x)

(a): M1C ₅₀ : Minimum concentration of antimicrobial agent that inhibits bacterial growth by 50%, (b): MIC ₉₀ : Minimum concentration of antimicrobial agent that inhibits bacterial growth by 90%, (c) 1x10 ⁶ cfu / mL , (D): Exhibit antimicrobial effect of extract required to inhibit 1x10 ⁶ cfu / mL of each species.

4. Review of experimental results

Results of the investigation of the antimicrobial activity of the dermatitis induced bacteria of sericite extract Malassezia furfur, Staphylococcus aureus, Staphylococcus epidermidis , Streptococcus pyogens, the amount of sericite extract required to inhibit the growth of 1x10 ⁶ cfu / mL bacteria against Propionibacterium acnes MIC _It was found to be 114.5, 44.0, 58.5, 5.28 and 8.0 mL at ₅₀ and 180.0, 186.4, 279.0, 55.5 and 154.0 mL at MIC ₉₀ .

In conclusion, sericite extract was found to have antimicrobial effects against the five strains, especially 44.0, 5.28 and 8.0mL to inhibit 1x10 ⁶ cfu / mL against Staphylococcus aureus, Streptococcus pyogens and Propionibacterium acnes . It can be seen that even a small amount of antibacterial effect.

Claims (6)

Grinding sericite to produce sericite powder;
Pressurizing and heating the sericite powder and water into a closed container;
Eluting water vapor through a pipe connected from the sealed container, eluting by adjusting the pressure of the closed container, the temperature of the closed container, the diameter of the pipe and the pressure of the eluted vapor; And
Condensing the eluted water vapor to obtain a sericite extract;
The pressure of the hermetic container is 1 ~ 200 atm, the temperature of the hermetic container is 100 ~ 400 ℃, the diameter of the tube is 5 ~ 50 mm, the vapor pressure of the elution is 20 ~ 15 atm, the heating time of the hermetic container 3 to 5 hours
The sericite extract has an antibacterial function against dermatitis pathogens,
The dermatitis pathogen is a Malassezia furfur Malassezia furfur method of producing a pH-controlled sericite extract.
delete delete delete delete Cosmetic composition comprising a sericite extract prepared according to claim 1 as an active ingredient.