KR102574601B1 - Preparation method of cosmetic composition comprising tea tree extracts and cosmetic composition prepared thereof - Google Patents

Abstract

The present invention includes the steps of washing the tea tree raw material, adding purified water as a primary solvent to the washed tea tree raw material, then irradiating the washed tea tree raw material with a microwave to obtain a primary extract, and adding lactic acid bacteria and secondary solvent to the primary extract. Preparing a mixture by adding a polyhydric alcohol-based compound, fermenting the mixture to obtain a secondary extract, low-temperature sterilizing and filtering the fermented secondary extract to obtain a tea tree extract, and the obtained tea tree Extract and purified water, glycerin, propanediol, 1,2-hexanediol, xanthan gum, butylene glycol, panthenol, trehalose, betaine, carbomer, allantoin, polyglyceryl-10 laurate, arginine, disodium. Method for producing a cosmetic composition containing tea tree extract, comprising the step of preparing a cosmetic composition by mixing one or more selected from the group consisting of DTA, dipotassium glycyrrhizate, and tocopheryl acetate, and cosmetics prepared therefrom A composition is provided.

Description

Method for producing a cosmetic composition containing tea tree extract and a cosmetic composition prepared therefrom

The present invention relates to a method for producing a cosmetic composition containing tea tree extract and a cosmetic composition prepared therefrom.

Tea tree, a natural product, is often distilled and used in the form of oil, and is known as a wound disinfectant, acne soothing agent, athlete's foot treatment, and respiratory disease treatment due to its antibacterial and antifungal properties.

Tea tree (Melaleuca alternifolia) is an evergreen tree belonging to the Myrtaceae family. Tea tree, which grows in swampy areas, is strong enough to grow well even if its stems are cut off. Tea tree was discovered along the coasts of Australia and New Zealand while searching for fresh tea. The water around the tea tree tree turned reddish brown, so people thought it was similar to black tea and started drinking it as tea, which is where the name tea tree comes from.

Extracts extracted from tea tree are collectively called essential oils, and conventional essential oils were mostly extracted through distillation or solvent extraction. The conventional extraction method achieved in this way has been a method of applying heat.

Typically, essential oils are made up of highly volatile substances, so there is a disadvantage in that the active ingredients are volatilized during the process of separating the active substances from the solvent (purified water or organic solvent) after extraction, reducing the extraction amount and effective ingredients. In addition, there was a problem in that residual waste and organic solvent remained during the separation process, and there was a disadvantage in that the oil flavor and active ingredients were destroyed.

Domestic Patent Publication No. 2018-0051821

The problem to be solved by the present invention is to provide a method for producing a cosmetic composition containing a tea tree extract secured with high extraction efficiency and a cosmetic composition containing the tea tree extract prepared by the production method.

In order to solve the above problem, the present invention includes the steps of washing the tea tree raw material, adding purified water as a primary solvent to the washed tea tree raw material, then irradiating the microwave to obtain a primary extract, and adding the primary extract to the primary extract. Preparing a mixture by adding a polyhydric alcohol-based compound as lactic acid bacteria and a secondary solvent, fermenting the mixture to obtain a secondary extract, and obtaining a tea tree extract by low-temperature sterilizing and filtering the fermented secondary extract. and the obtained tea tree extract and purified water, glycerin, propanediol, 1,2-hexanediol, xanthan gum, butylene glycol, panthenol, trehalose, betaine, carbomer, allantoin, polyglyceryl-10 laurate, A method for producing a cosmetic composition containing tea tree extract, comprising the step of preparing a cosmetic composition by mixing at least one selected from the group consisting of arginine, disodium EDTA, dipotassium glycyrrhizate, and tocopheryl acetate. and a cosmetic composition containing a tea tree extract prepared by the method.

By using the method for producing a cosmetic composition containing tea tree extract according to the present invention, it is possible to contain a high content of flavonoid derivative compounds obtained from tea tree raw materials, and p-, which is an oxide generated during the extraction process of tea tree raw materials, A cosmetic composition containing a minimum amount of cymene (p-Cymene) compounds can be manufactured.

BRIEF DESCRIPTION OF THE DRAWINGS Various embodiments of the present invention are described below with reference to the accompanying drawings. The present invention is not limited to specific embodiments, and should be understood to include various modifications, equivalents, and/or alternatives to the embodiments of the present invention. In connection with the description of the drawings, similar reference numbers may be used for similar components.

In this document, expressions such as “have,” “may have,” “includes,” or “may include” refer to the existence of the corresponding feature (e.g., a numerical value, function, operation, or component such as a part). , and does not rule out the existence of additional features.

In this document, expressions such as “A or B,” “at least one of A or/and B,” or “one or more of A or/and B” may include all possible combinations of the items listed together. . For example, “A or B”, “at least one of A and B”, or “at least one of A or B” (1) includes at least one A, (2) includes at least one B, or (3) it may refer to all cases including both at least one A and at least one B.

The expression "configured to" used in this document may be used depending on the situation, for example, "Suitable for," "Having the capacity to." It can be used interchangeably with ", "Designed to," "Adapted to," "Made to," or "Capable of." The term “configured (or set) to” does not necessarily mean “specifically designed to.”

Terms used in this document are merely used to describe specific embodiments and may not be intended to limit the scope of other embodiments. Singular expressions may include plural expressions, unless the context clearly indicates otherwise. Terms used herein, including technical or scientific terms, may have the same meaning as commonly understood by a person of ordinary skill in the technical field described in this document. Among the terms used in this document, terms defined in general dictionaries may be interpreted to have the same or similar meaning as the meaning they have in the context of related technology, and unless clearly defined in this document, they may be interpreted in an ideal or excessively formal sense. It is not interpreted. In some cases, even terms defined in this document cannot be interpreted to exclude embodiments of this document.

The embodiments disclosed in this document are presented for explanation and understanding of the disclosed technical content, and do not limit the scope of the present invention. Accordingly, the scope of this document should be interpreted as including all changes or various other embodiments based on the technical idea of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail. Prior to this, the terms or words used in this specification and claims should not be construed as limited to their usual or dictionary meanings, and the inventor should appropriately define the concept of terms in order to explain his or her invention in the best way. It must be interpreted as meaning and concept consistent with the technical idea of the present invention based on the principle of definability.

Therefore, the configurations of the embodiments described in this specification are only some of the most preferred embodiments of the present invention and do not represent the entire technical idea of the present invention, so various equivalents and modifications can be substituted for them at the time of filing the present application. You must understand that there may be.

Throughout the specification, when a part is said to “include” a certain element, this means that it may further include other elements rather than excluding other elements, unless specifically stated to the contrary.

Hereinafter, the present invention will be described in detail.

A method for producing a cosmetic composition containing a tea tree extract according to an embodiment of the present invention includes the steps of washing the tea tree raw material, adding purified water as a primary solvent to the washed tea tree raw material, and then irradiating it with a microwave. Obtaining a primary extract, preparing a mixture by adding lactic acid bacteria and a polyhydric alcohol-based compound as a secondary solvent to the primary extract, fermenting the mixture to obtain a secondary extract, the fermented secondary extract Obtaining a tea tree extract by low-temperature sterilization and filtration, and the obtained tea tree extract, purified water, glycerin, propanediol, 1,2-hexanediol, xanthan gum, butylene glycol, panthenol, trehalose, betaine, A step of preparing a cosmetic composition by mixing one or more selected from the group consisting of carbomer, allantoin, polyglyceryl-10 laurate, arginine, disodium EDTA, dipotassium glycyrrhizate, and tocopheryl acetate. Includes. Below, each step is described in detail.

The step of washing the tea tree raw material is performed to remove substances other than the tea tree raw material collected from nature and reduce biological and chemical hazards to the acceptable level required in the food field. For example, tea tree raw material This can be performed by washing under running water.

Additionally, in order to perform the subsequent extraction process more effectively, cutting and drying processes can be additionally performed.

The cutting process is performed to increase drying efficiency and extraction efficiency by increasing the surface area of the tea tree raw material during drying, and the washed tea tree raw material is cut into pieces of 2 to 3 cm in size.

The drying process is to lower the amount of moisture contained in the tea tree raw material to suppress microbial metabolism and improve storage. For example, the tea tree raw material can be dried using a dryer.

The step of adding purified water as a primary solvent to the washed tea tree raw material and then irradiating it with a microwave to obtain the primary extract minimizes the generation of p-Cymene compound, an oxide generated during the extraction process. This is to secure the target intermediate compounds, α-terpinene and γ-terpinene, in high yield.

Microwaves used in the above microwave irradiation are a form of energy with a low frequency among electromagnetic energy. Microwaves, also called centiwaves, are a type of electromagnetic wave whose wavelength is in centimeters (cm). The frequency range may be 300 to 300,000 MHz. In addition, microwaves propagate at the speed of light (300,000 km/s), and the microwave photon energy (0.037 kcal/mol) at this time is relatively low compared to the typical energy that can break intermolecular bonds (80 to 120 kcal/mol). Because it is very low, it does not affect the structure of the molecule and can induce the electronic spin of the molecule into an excited state. If the above-described characteristics of microwaves are used in the present invention, microbubbles can be formed around the molecules of the tea tree raw material due to the movement of the molecules, and the interfacial tension can be lowered, thereby maximizing extraction efficiency.

Microwave irradiation may be performed under pressure, for example, under a pressure of 1 to 100 atm. Microwave output is not particularly limited, and may be appropriately increased or decreased depending on the amount of reactants, and for example, 500 to 1000 W may be used. Preferably, the output of the microwave may be 850 to 1000 W. More preferably, the output of the microwave may be 900 to 1000 W.

Microwave irradiation can be performed at 100°C to 150°C. Additionally, microwave irradiation can be performed for 30 to 90 minutes.

During the microwave irradiation, tea tree raw materials may be used as is, or dried or freeze-dried products of tea tree raw materials may be used. In one embodiment, microwave irradiation may be performed on a solution containing tea tree raw material and purified water, for 30 to 90 minutes, at a temperature of 100 to 150° C., and at 1 atm to 100 atm.

During the microwave irradiation, purified water is supplied as a solvent, the entire inside and outside of the tea tree raw material is heated by the microwave, the heated water vapor is cooled and condensed, and the primary extract is formed through a steaming process at room temperature and pressure in which the tea tree is repeatedly circulated to the extraction container. .

In particular, according to one embodiment of the present invention, the energy of microwaves can be transferred directly to the tea tree raw material placed in purified water, so the solvent is heated like a conventional hot water extraction method and the energy of the heated solvent is transferred to the tea tree raw material. The indirect energy transfer path to can be further simplified. For this reason, the energy of the microwave can be transmitted directly into the tea tree raw material, thereby increasing extraction efficiency.

Microwaves have a wavelength of 1 mm to 1 m and belong to a spectroscopically relatively long wavelength range. When a relatively long wavelength is irradiated to the tea tree raw material, it is possible to penetrate into the interior of the tea tree raw material, thereby securing the extract more effectively. Specifically, inside the particles that make up tea tree, the electron spins of atoms are in the ground state at room temperature, but can be in an excited state by receiving energy absorbed from a long wavelength. Unlike the hot water extraction method that simply applies heat to the surface, when using a long wavelength, the desired extract can be obtained with higher efficiency due to the energy penetrating into the inside of the raw material, and the desired extract can be effectively obtained in a shorter time than the time required for the hot water extraction method. can be obtained, minimizing the time that tea tree raw materials are exposed to heat.

Extracts of interest from tea tree raw materials may include α-terpinene and γ-terpinene compounds, which may be oxidized by exposure to atmospheric oxygen, light, humidity, and high temperatures. In this case, α-terpinene, γ-terpinene compound can change to p-Cymene. The content of p-Cymene in the extract can increase up to 10 times depending on conditions. p-Cymene generated from the extract remains in the tea tree extract and may cause negative effects, such as skin troubles, when applied as a cosmetic composition.

In order to minimize the generation of p-Cymene, the ratio of tea tree raw materials and purified water must be precisely controlled in the step of obtaining the primary extract by irradiating microwaves. Specifically, the tea tree raw material and purified water may be applied at a weight ratio of 1:10 to 15. If the purified water is below the above range, the content of p-Cymene may actually increase due to excessive microwave irradiation, and if it is above the above range, the frequency of microwave irradiation on the tea tree raw material is low, thereby securing a low level of the desired extract. There is a problem.

The purified water may be purified water or ultrapure purified water commonly used in the art, and ultrapure purified water may be preferably used. General purified water is water commonly used in pharmaceuticals, cosmetics, etc., and has a dissolved solids content of 1.0 to 0.5 ppm, indicating purity, a filter size of 0.2 to 0.45 ㎛ used to remove particulates and microorganisms when producing purified water, and a pH of 0.2 to 0.45 ㎛. It varies from weak acid to weak alkaline. The ultrapure purified water has a very high purity with a dissolved solid content of 0.03ppm, and the size of the filter used in producing ultrapure purified water is 0.001㎛, which removes 99.99% of microorganisms. In particular, ultrapure purified water can prevent auto-oxidation reactions by removing metal ions.

The steps of preparing a mixture by adding lactic acid bacteria and a polyhydric alcohol-based compound as a secondary solvent to the primary extract and fermenting the mixture to obtain a secondary extract prevent oxidation of α-terpinene and γ-terpinene compounds, , It is introduced to obtain the desired extract with higher efficiency using an amphipathic solvent while simultaneously carrying out the fermentation process.

The polyhydric alcohol-based compound is an amphipathic substance and has affinity with both water-soluble and fat-soluble solvents. Since tea tree extracts basically have a fat-soluble structure such as terpene alcohol, monocyclic terpene, dicyclic terpene, and sesquiterpene, extraction efficiency may be reduced when water-soluble solvents such as hot water extraction are used.

After the extraction is performed in an excited state due to the microwave irradiation, the atoms inside the tea tree raw material are excited, and then the stabilization stage is entered into the secondary extraction stage. When the extraction efficiency is improved by applying a polyhydric alcohol-based compound solvent to the components with a relatively fat-soluble structure. can be maximized.

As a result of intensive research, in order to minimize the generation of p-Cymene, the present inventors obtained the primary extract by irradiating it with microwaves, and then used a polyhydric alcohol-based compound solvent to prevent oxidation of the obtained components and stably obtain the desired material. The applied extraction method was found to be efficient. By continuously performing the above-described first and second extraction processes, the content of p-Cymene contained in the finally obtained tea tree extract could be reduced to 0.0001 to 2% by weight out of the total 100% by weight of the tea tree extract.

In order to increase extraction efficiency and ensure skin application safety when the extract is later applied to the cosmetic composition, the polyhydric alcohol-based compound consists of dipropylene glycol, 1,3-butylene glycol, glycerin, 1,3-propanediol, and hexanediol. It may include one or more types selected from the group. In order to minimize the content of p-Cymene and achieve compatibility with lactic acid bacteria described later, dipropylene glycol can be preferably used.

Examples of the lactic acid bacteria include strains commonly used in the fermentation of natural extracts, such as Aspergillus sp., Mucor sp., and Lactobacillus sp., which can produce proteolytic enzymes. .) or Rhizopus sp., etc. can be used, and these can be used alone or as a mixture of two or more strains. For compatibility with the polyhydric alcohol-based compound, which is the above-mentioned secondary solvent, and optimal growth of the strain, it is preferable to use a Lactobacillus sp. strain. More preferably, the lactic acid bacteria may be Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP.

In the present invention, “Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP” is a novel lactic acid bacterium of Lactobacillus floctusus isolated and identified from Cosmos, and was registered at the Korea Research Institute of Bioscience and Biotechnology Biological Resources Center on March 25, 2022. It was deposited on date (accession number KCTC 14924BP).

According to one embodiment of the present invention, the lactic acid bacteria included in the mixture may be a lactic acid bacteria culture medium obtained by culturing lactic acid bacteria strains in NB broth at a temperature of 30°C to 40°C for 20 to 30 hours. The content of the lactic acid bacteria culture medium may be inoculated by weighing 3 to 15% by weight based on 100% by weight of the mixture.

As a result, the mixture may contain 30 to 50% by weight of the polyhydric alcohol-based compound, 3 to 15% by weight of the lactic acid bacteria culture medium, and the remainder of the primary extract.

In order to ensure efficiency for optimal extraction of terpene compounds α-terpinene and γ-terpinene from tea tree raw materials without interfering with the fermentation of lactic acid bacteria, the content of polyhydric alcohol compounds contained in the mixture must be precisely controlled. do. Specifically, based on 100% by weight of the mixture, the polyhydric alcohol-based compound may be included in an amount of 30 to 50% by weight. If the polyhydric alcohol-based compound is less than the above range, the extraction efficiency rapidly decreases, and if it is more than the above range, it is undesirable in terms of economic efficiency compared to the extraction efficiency, and in terms of poor survival of lactic acid bacteria due to too high alcohol concentration.

The fermentation is applied to extract the desired extract components from tea tree raw materials with maximum efficiency without heat treatment. In other words, changes in the components of the extracted material can be minimized compared to conventional high-pressure sterilization techniques. Specifically, in the fermentation step, the secondary mixture is created and then cultured for 30 to 60 hours at a temperature of 30°C to 40°C with good ventilation.

After completion of cultivation, flavonoid derivative compounds, which are low-molecular-weight components derived from α-terpinene and γ-terpinene compounds among the main fermentation components, can be obtained through a low-temperature sterilization step to remove cultured microorganisms and a microfilter purification step.

The step of concentrating the secondary extract is a step of evaporating the solvent of the secondary extract at reduced pressure and low temperature in a rotary low-temperature concentrator, collecting and concentrating the evaporated secondary extract in a cooling condenser. However, the step of filtration using a micro filter before concentration may be further included. The concentration step is evaporation and concentration at a temperature of 25 to 35°C, preferably 30°C. At this time, the internal vacuum degree of the rotary low-temperature concentrator is set to 39 to 43 mmHg.

Since the flavonoid derivative compound is a type of secondary metabolite of plants or fungi, it has a general structure of a 15-carbon skeleton consisting of two phenyl rings and a heterocyclic ring. This carbon structure can be abbreviated as C6-C3-C6, and plant pigments with this skeleton are collectively called flavonoids.

The obtained tea tree extract and purified water, glycerin, propanediol, 1,2-hexanediol, xanthan gum, butylene glycol, panthenol, trehalose, betaine, carbomer, allantoin, polyglyceryl-10 laurate, Al The step of preparing a cosmetic composition by mixing one or more selected from the group consisting of ginine, disodium EDTA, dipotassium glycyrrhizate, and tocopheryl acetate preserves and preserves the flavonoid derivative compound components secured from tea tree raw materials. It is intended to manufacture a cosmetic composition that additionally has the effect of supplying moisture to the skin, maintaining moisture, and soothing the skin. Preferably, the obtained tea tree extract, purified water, glycerin, propanediol, 1,2-hexanediol, white willow bark extract, centella asiatica extract, Houttuynia cordata extract, black bean extract, pea extract, sage extract, lavender extract, and rosemary extract. , lemongrass extract, xanthan gum, butylene glycol, Indian frankincense resin extract, panthenol, trehalose, betaine, carbomer, allantoin, polyglyceryl-10 laurate, arginine, disodium EDTA, dipotassium glycol. A cosmetic composition can be prepared by mixing one or more selected from the group consisting of seriesate, tocopheryl acetate, and tea tree oil (50ppm).

The content of the obtained tea tree extract may be 30 to 70% by weight based on 100% by weight of the cosmetic composition. Preferably, the content of the obtained tea tree extract may be 40 to 60% by weight based on 100% by weight of the cosmetic composition. If the content of the tea tree extract is less than 30% by weight, there is a problem that the antioxidant and moisturizing effect when applied to the skin is minimal, and if it exceeds 70% by weight, it reduces the formulation stability of the product without a clear effect due to an increase in content. Problems may arise.

Through the above manufacturing method, it is possible to secure a high content of flavonoid derivative compounds extracted from tea tree raw materials, and to manufacture a cosmetic composition containing tea tree extract by minimizing the generation of p-Cymene compounds, which are oxides generated during the extraction process. You can.

A cosmetic composition containing tea tree extract according to an embodiment of the present invention can be prepared as a cosmetic composition for application to the skin. The formulation of the composition of the present invention is not limited as long as it can be applied to the skin, for example, solution, suspension, emulsion, paste, gel, cream, lotion, powder, soap, surfactant-containing cleansing, oil. , it can be manufactured in at least one formulation selected from the group consisting of powder foundation, emulsion foundation, wax foundation, and spray. Specifically, it can be manufactured in the form of flexible lotion, nourishing lotion, mist, nourishing cream, moisturizing cream, massage cream, essence, eye cream, cleansing cream, cleansing foam, cleansing water, pack, mask pack, spray, or powder. However, it is not limited to this.

Components included in the composition of the present invention may include additive components commonly used in cosmetic compositions. For example, it may include at least one selected from the group consisting of stabilizers, solubilizers, vitamins, pigments, fragrances, and carriers, but is not limited thereto. The added ingredients may be adjusted depending on the formulation of the composition of the present invention.

Hereinafter, the present invention will be described in more detail through examples. These examples are only for illustrating the present invention in more detail, and it is understood by those skilled in the art that the scope of the present invention is not limited by these examples according to the gist of the present invention. It will be self-evident.

Examples and Comparative Examples

Example 1

Tea tree raw materials obtained from Jeju Island were washed in running water (S1).

After adding 100 g of purified water as a primary solvent to 10 g of the washed tea tree raw material, the primary extract was obtained by irradiating a microwave at a frequency of 1000w of a START D device from Milestone for 60 minutes (S2).

After transferring the obtained primary extract to a container, 30% by weight of dipropylene glycol and 8% by weight of Lactobacillus lactic acid bacteria culture medium were added as secondary solvents to prepare a mixture (S3). The weight percent was based on 100 weight percent of the total mixture. The lactic acid bacterium was Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP, and a culture solution was prepared by culturing in NB broth at 35°C for 24 hours.

Afterwards, in a place with excellent ventilation, fermentation was performed at 35°C for 36 hours to obtain a secondary extract (S4).

The obtained fermentation broth was sterilized at low temperature and filtered through a 0.2 micro-sized micro filter to obtain a tea tree extract (S5).

Examples 2 to 11

The composition and content added were adjusted as shown in Table 1 below, and the rest was carried out in the same manner as in Example 1 to obtain a tea tree extract.

note Tea tree raw material (S1, g) primary solvent
(S2, g) secondary solvent
(S3, weight%) Lactobacillus culture medium
(S3, weight%) Fermentation conditions
(S4, time) Example 1 10 100 30 8 36 Example 2 10 150 30 8 36 Example 3 10 50 30 8 36 Example 4 10 300 30 8 36 Example 5 10 100 40 8 36 Example 6 10 100 50 8 36 Example 7 10 100 20 8 36 Example 8 10 100 60 8 36 Example 9 10 100 30 8 36 Example 10 10 100 30 8 36 Example 11 10 100 30 8 36 Example 9: Change of secondary solvent to 1,3-butylene glycol
Example 10: Change the secondary solvent to glycerin
Example 11: Change the secondary solvent to 1,3-propanediol

Comparative Example 1

Tea tree raw materials obtained from Jeju Island were washed in running water.

Instead of the manufacturing method of Example 1, 10 g of the tea tree raw material was used as a reflux cooling extraction method, and the tea tree raw material and 100 g of purified water were mixed and heated to 100 to 150 ° C. to generate steam, and the evaporated steam was passed through the cooling tunnel. The primary extract was obtained using a process for 4 hours so that it could be extracted into a liquid phase.

After transferring the obtained extract to a container, 8% by weight of Lactobacillus lactic acid bacteria culture medium was added to prepare a mixture. The weight percent was based on the total 100 weight percent of the mixture. The lactic acid bacterium was Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP, and a culture solution was prepared by culturing in NB broth at 35°C for 24 hours. Afterwards, fermentation was carried out at 35°C for 36 hours in a place with excellent ventilation. The obtained fermentation broth was sterilized at low temperature and filtered through a 0.2 micro-sized micro filter to obtain a tea tree extract.

Comparative Example 2

Tea tree raw materials obtained from Jeju Island were washed in running water.

10 g of the tea tree raw material was extracted for 60 minutes using a conventional hot water extraction method to obtain a primary extract.

After transferring the obtained extract to a container, 8% by weight of Lactobacillus lactic acid bacteria culture medium was added to prepare a mixture. The weight percent was based on the total 100 weight percent of the mixture. The lactic acid bacterium was Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP, and a culture solution was prepared by culturing in NB broth at 35°C for 24 hours. Afterwards, fermentation was carried out at 35°C for 36 hours in a place with excellent ventilation. The obtained fermentation broth was sterilized at low temperature and filtered through a 0.2 micro-sized micro filter to obtain a tea tree extract.

Comparative Example 3

Tea tree raw materials obtained from Jeju Island were washed in running water.

10 g of the tea tree raw material was extracted for 120 minutes using a conventional hot water extraction method to obtain a primary extract.

After transferring the obtained extract to a container, 8% by weight of Lactobacillus lactic acid bacteria culture medium was added to prepare a mixture. The weight percent was based on the total 100 weight percent of the mixture. The lactic acid bacterium was Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP, and a culture solution was prepared by culturing in NB broth at 35°C for 24 hours. Afterwards, fermentation was carried out at 35°C for 36 hours in a place with excellent ventilation. The obtained fermentation broth was sterilized at low temperature, filtered through a 0.2 micro-sized micro filter, and the final extract was obtained.

Comparative Example 4

Tea tree raw materials obtained from Jeju Island were washed in running water.

After adding 100 g of purified water as a solvent to 10 g of the washed tea tree raw material, the primary extract was obtained by irradiating the mixture with a 1000w microwave using a START D device from Milestone for 60 minutes.

After transferring the obtained extract to a container, 8% by weight of Lactobacillus lactic acid bacteria culture medium was added to prepare a mixture. The weight percent was based on the total 100 weight percent of the mixture. The lactic acid bacterium was Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP, and a culture solution was prepared by culturing in NB broth at 35°C for 24 hours. Afterwards, fermentation was carried out at 35°C for 36 hours in a place with excellent ventilation. The obtained fermentation broth was sterilized at low temperature and filtered through a 0.2 micro-sized micro filter to obtain a tea tree extract.

Comparative Example 5

Tea tree raw materials obtained from Jeju Island were washed in running water.

After adding 70 g of dipropylene glycol as a solvent to 10 g of the washed tea tree raw material, extraction was performed at 35°C for 600 minutes to obtain a primary extract.

After transferring the obtained extract to a container, 8% by weight of Lactobacillus lactic acid bacteria culture medium was added to prepare a mixture. The weight percent was based on the total 100 weight percent of the mixture. The lactic acid bacterium was Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP, and a culture solution was prepared by culturing in NB broth at 35°C for 24 hours. Afterwards, fermentation was carried out at 35°C for 36 hours in a place with excellent ventilation. The obtained fermentation broth was sterilized at low temperature and filtered through a 0.2 micro-sized micro filter to obtain a tea tree extract.

Comparative Example 6

Tea tree raw materials obtained from Jeju Island were washed in running water.

After adding 100 g of purified water as a primary solvent to 10 g of the washed tea tree raw material, the primary extract was obtained by irradiating a microwave at a frequency of 1000w using a Milestone START D device for 60 minutes.

After transferring the obtained primary extract to a container, 30% by weight of dipropylene glycol was added as a secondary solvent to prepare a mixture. The weight percent was based on the total 100 weight percent of the mixture. The obtained fermentation broth was sterilized at low temperature, filtered through a 0.2 micro-sized micro filter, and the final extract was obtained.

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Manufacturing example

Manufacturing Example 1

Tea tree extract and purified water obtained through steps (S1) to (S5) of Example 1, glycerin, propanediol, 1,2-hexanediol, xanthan gum, butylene glycol, panthenol, trehalose, betaine, A cosmetic composition was prepared by mixing carbomer, allantoin, polyglyceryl-10 laurate, arginine, disodium EDTA, dipotassium glycyrrhizate, and tocopheryl acetate (S6).

The tea tree extract obtained according to Example 1 was included in 50% by weight based on 100% by weight of the cosmetic composition.

Preparation Examples 2 to 7

The composition and content added were adjusted as shown in Table 2 below, and the rest was carried out in the same manner as in Preparation Example 1 to prepare a cosmetic composition.

Content of each ingredient of cosmetic composition Ingredient name (% by weight) Sample name Manufacturing Example 1 Production example 2 Production example 3 Production example 4 Production example 5 Production example 6 Production example 7 Tea tree extract (% by weight) 50 40 60 30 70 10 80 Purified water To 100 To 100 To 100 To 100 To 100 To 100 To 100 glycerin 2.0 2.0 2.0 2.0 2.0 2.0 2.0 propanediol 0.5 0.5 0.5 0.5 0.5 0.5 0.5 1,2-hexanediol 1.5 1.5 1.5 1.5 1.5 1.5 1.5 xanthan gum 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Butylene glycol 0.3 0.3 0.3 0.3 0.3 0.3 0.3 panthenol 0.5 0.5 0.5 0.5 0.5 0.5 0.5 trehalose 0.1 0.1 0.1 0.1 0.1 0.1 0.1 betaine 0.2 0.2 0.2 0.2 0.2 0.2 0.2 carbomer 0.12 0.12 0.12 0.12 0.12 0.12 0.12 allantoin 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Polyglyceryl-10 Laurate 0.2 0.2 0.2 0.2 0.2 0.2 0.2 arginine 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Disodium EDTA 0.02 0.02 0.02 0.02 0.02 0.02 0.02 Dipotassium glycyrrhizate 0.05 0.05 0.05 0.05 0.05 0.05 0.05 Tocopheryl Acetate 0.03 0.03 0.03 0.03 0.03 0.03 0.03

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Experimental Example 1: Confirmation of ingredient content of tea tree extract of Examples and Comparative Examples

1) Check terpinen-4-ol content

After recovering all of the tea tree extracts in the above examples and comparative examples, the content of terpinen-4-ol contained in the entire extract was confirmed. Control group 1 expressed the net content of terpinen-4-ol contained in 10 g of tea tree raw material in grams. The results are shown in Table 3.

note terpinen-4-ol extracted amount (g)
(% of pure content in 10g tea tree raw materials) Example 1 0.01497g (33.18%) Example 2 0.01215g (26.93%) Example 3 0.01738g (38.52%) Example 4 0.00917g (20.32%) Example 5 0.01540g (34.13%) Example 6 0.01605g (35.57%) Example 7 0.01398g (30.98%) Example 8 0.01492g (33.07%) Example 9 0.01484g (32.89%) Example 10 0.01397g (30.96%) Example 11 0.01387g (30.74%) Comparative Example 1 0.00421g (9.33%) Comparative Example 2 0.00221g (4.90%) Comparative Example 3 0.00315g (6.98%) Comparative Example 4 0.01205g (26.71%) Comparative Example 5 0.02515g (55.74%) Control group 1 0.04512g

2) Check p-Cymene content

After all the tea tree extracts were recovered in the steps of the above Examples and Comparative Examples, the p-Cymene content contained in the entire extract was confirmed. Control group 1 expressed the net content of p-Cymene in 10g of tea tree raw material in grams. The results are shown in Table 4.

note p-Cymene content
(% of pure content in 10g tea tree raw material) Example 1 0.00081g (30.57%) Example 2 0.00094g (35.47%) Example 3 0.00138g (52.08%) Example 4 0.00071g (26.79%) Example 5 0.00102g (38.49%) Example 6 0.00105g (39.62%) Example 7 0.00099g (37.36%) Example 8 0.00111g (41.89%) Example 9 0.00093g (35.09%) Example 10 0.00090g (33.96%) Example 11 0.00091g (34.34%) Comparative Example 1 0.00558g (210.57%) Comparative Example 2 0.00515g (194.34%) Comparative Example 3 0.00758g (286.04%) Comparative Example 4 0.00424g (160.00%) Comparative Example 5 0.00222g (83.77%) Comparative Example 6 0.00266g (100.38%) Control group 1 0.00265g

3) Check α-terpinene and γ-terpinene content

After recovering all of the tea tree extract in the steps of the above examples and comparative examples, α-terpinene and γ-terpinene contained in the entire extract were confirmed. Control group 1 expressed the net content of α-terpinene and γ-terpinene contained in 10 g of tea tree raw material in grams. The results are shown in Table 5.

note α-terpinene content
(% of pure content in 10g tea tree raw material)
γ-terpinene content
(% of pure content in 10g tea tree raw material)
Example 1 0.00657g (31.29%) 0.00412g (37.45%) Example 2 0.00412g (19.62%) 0.00298g (27.09%) Example 3 0.00345g (16.43%) 0.00195g (17.73%) Example 4 0.00332g (15.81%) 0.00185g (16.82%) Example 5 0.00698g (33.24%) 0.00425g (38.64%) Example 6 0.00725g (34.52%) 0.00434g (39.45%) Example 7 0.00647g (30.81%) 0.00409g (37.18%) Example 8 0.00751g (35.76%) 0.00451g (41.00%) Example 9 0.00402g (19.14%) 0.00303g (27.55%) Example 10 0.00208g (9.90%) 0.00224g (20.36%) Example 11 0.00101g (4.81%) 0.00165g (15.00%) Comparative Example 1 0.00316g (15.05%) 0.00198g (18.00%) Comparative Example 2 0.00284g (13.52%) 0.00165g (15.00%) Comparative Example 3 0.00292g (13.90%) 0.00172g (15.64%) Comparative Example 4 0.00291g (13.86%) 0.00166g (15.09%) Comparative Example 5 0.01102g (52.48%) 0.00654g (59.45%) Comparative Example 6 0.00321g (15.29%) 0.00199 (18.09%) Control group 1 0.021g 0.011

4) Confirmation of flavonoid derivative compound content

Flavonoid derivative compounds were identified in the tea tree extracts from the above examples and comparative examples. The results are shown in Table 6.

note Flavonoid derivative content (% by weight)
(Compared to 100% by weight of total extract) Example 1 312 QE/g Example 2 283 QE/g Example 3 271 QE/g Example 4 268 QE/g Example 5 308QE/g Example 6 304QE/g Example 7 291 QE/g Example 8 288 QE/g Example 9 287 QE/g Example 10 284 QE/g Example 11 281 QE/g Comparative Example 1 198 QE/g Comparative Example 2 168 QE/g Comparative Example 3 200QE/g Comparative Example 4 121 QE/g Comparative Example 5 15QE/g Comparative Example 6 8QE/g

5) Check fermentation efficiency

Table 7 shows the results measured by OD600 (optical density at 600 nm) for the extracts from the above examples and comparative examples after fermentation and before low-temperature sterilization.

note 0D value Example 1 0.915 Example 2 0.901 Example 3 0.880 Example 4 0.811 Example 5 0.819 Example 6 0.623 Example 7 0.599 Example 8 0.550 Example 9 0.592 Example 10 0.576 Example 11 0.499 Comparative Example 1 0.802 Comparative Example 2 0.811 Comparative Example 3 0.786 Comparative Example 4 0.581 Comparative Example 5 - Comparative Example 6 -(No change, no lactic acid bacteria fermentation)

Experimental Example 2 Calming effect on skin irritants

The skin soothing effect was confirmed through human skin testing on 20 healthy adult men and women in their 20s to 50s with no skin disease or allergic symptoms and no history of hypersensitivity reactions.

A skin patch test was performed on the cosmetic compositions of Preparation Examples 1 to 7 (Table 2) and 5% lactic acid, a skin irritant, as a control sample. Before proceeding with the sedation test, the inner part of the test subject's forearm was thoroughly wiped with 70% ethanol, dried completely, and 30 ㎍ of 9 types of cosmetics were applied to each area. After 24 hours had elapsed based on the patch application time, the patch was removed, and approximately 30 minutes later, the patch area was observed using a magnifying glass (MicroView) to confirm the presence or absence of erythema and edema. The evaluation was conducted based on the standards in Table 8 below, and the average skin reactivity was calculated according to the equation below. The results are shown in Table 9.

sign score skin irritation Evaluation standard - 0 non-irritating No response ± 0.5 No stimulation Mild erythema that is faint or barely detectable + 1.0 light stimulation Erythema with clear boundaries but mild erythema ++ 2.0 medium irritation Marked erythema +++ 3.0 strong stimulation Severe erythema and blisters

Math equation:

Average skin reactivity =

Sample name score reactivity 0 0.5 1.0 2.0 3.0 Manufacturing Example 1 20 - - - - 0 Production example 2 19 One - - - 0.008 Production example 3 19 One - - - 0.008 Production example 4 17 One 2 - - 0.042 Production example 5 18 2 - - - 0.016 Production example 6 17 One 3 - - 0.058 Production example 7 14 5 One - - 0.058 Control sample (lactic acid) 3 12 3 2 - 0.216

Experimental Example 3 Skin moisturizing effect

The cosmetic compositions according to Preparation Examples 1 to 7 were applied to 20 male and female test subjects (25 to 50 years old) on both sides of the face and the front half of the face twice a day for 4 weeks. Before application, 2 The improvement in skin moisture after one week and four weeks was measured using a skin moisture meter Corneometer CM 820 (Courage + Khazaka, Germany). The unit is expressed in an arbitrary unit (AU) given by the device, and the higher the measurement value, the higher the moisture content on the skin surface. The results of the experiment on improving skin moisturization are shown in Table 10.

Sample name Skin moisturizing effect (AU) Before application 2 weeks later 4 weeks later Manufacturing Example 1 48 62 67 Production example 2 49 61 65 Production example 3 48 64 70 Production example 4 47 58 62 Production example 5 48 64 69 Production example 6 48 55 59 Production example 7 49 59 63

Experimental Example 4 Evaluation of formulation of cosmetic composition and degree of visual acuity and foreign body sensation

1) The degree of aging was determined by visually observing changes over time, i.e., formulation agglomeration, discoloration, and precipitation, under room temperature conditions immediately after manufacturing the cosmetic compositions according to Preparation Examples 1 to 7 until 2 weeks later, and the results were It is summarized in Table 11.

2) Foreign body sensation evaluation was performed by pushing the cosmetic compositions according to Preparation Examples 1 to 7 on a glass plate (width*length*thickness=19cm*19cm*0.3cm) immediately after manufacturing to check the foreign body sensation (homogeneous dispersion) of the formulation over time, and the results were obtained. is written in Table 11.

Sample name Stability over time Foreign body sensation evaluation (homogeneous dispersion) Manufacturing Example 1 ○ ++++ Production example 2 ○ ++++ Production example 3 ○ ++++ Production example 4 ○ ++++ Production example 5 × ++- Production example 6 ○ ++++ Production example 7 × -+-

<Standards for evaluation of safety level>

×: Unstability (at least one of formulation agglomeration, discoloration, and precipitation occurs)

○: Stable (no lumping, discoloration, or precipitation)

<Evaluation criteria for foreign body sensation over time>

+++: The state of application on the glass plate is clean, but there are rare rough parts, and a feeling of foreign body over time is rarely observed.

++++: The overall state of application on the glass plate is clean, and no foreign body sensation is observed over time.

++-: The state of application on the glass plate is smooth, but some rough parts are observed, and a feeling of foreign body over time is rarely observed.

-+-: The overall state of coating on the glass plate is rough, and some foreign body sensation is observed over time.

---: The overall state of coating on the glass plate is rough, and a feeling of foreign matter is observed overall over time.

Claims (8)

Washing tea tree raw materials;
Adding purified water as a primary solvent to the washed tea tree raw material and then irradiating it with a microwave to obtain a primary extract;
Preparing a mixture by adding lactic acid bacteria and a polyhydric alcohol-based compound as a secondary solvent to the primary extract;
fermenting the mixture to obtain a secondary extract;
Obtaining a tea tree extract by low-temperature sterilizing and filtering the fermented secondary extract; and
The obtained tea tree extract and purified water, glycerin, propanediol, 1,2-hexanediol, xanthan gum, butylene glycol, panthenol, trehalose, betaine, carbomer, allantoin, polyglyceryl-10 laurate, Al Comprising the step of preparing a cosmetic composition by mixing at least one selected from the group consisting of ginine, disodium EDTA, dipotassium glycyrrhizate, and tocopheryl acetate,
A method of producing a cosmetic composition containing a tea tree extract, wherein the lactic acid bacteria are Lactobacillus fructosus Mediheal 01 (Lactobacillus fructosus Mediheal 01) KCTC 14924BP.
In claim 1,
A method for producing a cosmetic composition containing a tea tree extract, wherein the weight ratio of the washed tea tree raw material and the primary solvent is 1:10 to 15.
In claim 1,
A method for producing a cosmetic composition containing a tea tree extract, wherein the content of p-Cymene contained in the tea tree extract is 0.0001 to 2% by weight out of the total 100% by weight of the tea tree extract.
In claim 1,
A method for producing a cosmetic composition containing a tea tree extract, wherein the content of the secondary solvent is 30 to 50% by weight based on 100% by weight of the mixture.
In claim 1,
A cosmetic containing a tea tree extract, wherein the polyhydric alcohol-based compound includes at least one selected from the group consisting of dipropylene glycol, 1,3-butylene glycol, glycerin, 1,3-propanediol, and hexanediol. Method for producing composition.
delete In claim 1,
A method for producing a cosmetic composition containing a tea tree extract, wherein the content of the obtained tea tree extract is 30 to 70% by weight based on 100% by weight of the cosmetic composition.
A cosmetic composition prepared by any one of the production methods of claims 1 to 5 and 7.