KR100787634B1 - Cosmetic composition having antiseptic activity - Google Patents

Abstract

The present invention contains 0.05 ~ 2.0% by weight of the Gaza extract and 0.05 ~ 2.0% by weight of the gallja extract, and at least one extract selected from the group consisting of cinnamon extract 0.01 ~ 0.5% by weight, sewage oil extract 0.05 ~ 2.0% by weight It is a cosmetic composition which has antiseptic activity to contain.

The cosmetic composition of the present invention is a cosmetic composition in which natural antibacterial raw materials are mixed in an appropriate ratio, and exhibits excellent antimicrobial activity. The antimicrobial spectrum is broad, and thus, the antiseptic property of cosmetics is excellent, and the effects on physicochemical stability and cosmetic formulations It is very small and there is no chance of skin irritation because no chemical preservatives are added.

Preservatives, antibacterial, let's go, blast, cinnamon, sewage.

Description

Cosmetic composition having antiseptic activity {COSMETIC COMPOSITION HAVING ANTISEPTIC ACTIVITY}

1 is a graph showing the results of the antiseptic activity test results of the emulsion containing the Gaza extract of Example 5 according to the present invention and the emulsion containing the gall extract of Example 6,

2 is a graph showing the antiseptic activity test results of the milk containing the cinnamon extract of Example 7 and the milk containing the sewage oil extract of Example 8,

3 is a graph showing the results of the antiseptic activity test of the milk containing the Gaza extract and gallnut extract of Example 9 and the milk containing the cinnamon extract and sewage extract of Example 10,

Figure 4 is a graph showing the antiseptic activity test results of the milk containing the Gaza extract and cinnamon extract of Example 11 and the milk extract, the gall extract, cinnamon extract, and sewage extract of Example 12,

Figure 5 is a graph showing the results of the antiseptic activity test of the milk containing the Gaza extract, gallja extract and cinnamon extract of Example 13 and the milk extract, the gall extract and sewage extract of Example 14,

6 is a graph showing the results of confirming the antiseptic activity of Comparative Example 1 and Comparative Example 2.

The present invention relates to a cosmetic composition having antibacterial and antiseptic activity and having low skin irritation potential. The cosmetic composition of the present invention is characterized by having an excellent antimicrobial activity and antiseptic activity by adding a natural antibacterial raw material in an appropriate ratio, without adding a chemical preservative.

More specifically, it contains very good antibacterial activity by containing the extracts of Gaza, Gallja extract, cinnamon and sesame oil, and have a broad antimicrobial spectrum, which provides excellent antiseptic properties for cosmetics, and also affects physicochemical stability and cosmetic formulation. It relates to a very low preservative-free cosmetic composition with no chemical preservatives added, which is unlikely to cause skin irritation.

Existing cosmetic compositions can be easily contaminated with microorganisms during manufacturing, distribution, or consumer use when they are manufactured or distributed without the addition of chemical preservatives (designated ingredients), which can cause skin safety problems. . Labeled ingredients are those ingredients that must be labeled by the Korea Food and Drug Administration when using them due to the danger to the human body and have legally designated allowable contents.Tar pigment, antiseptic, fungicide, antihistamine, sunscreen, gold leaf, hair Only phosphate is a product of total phosphate.

Among these, preservatives are drugs that prevent the decay of substances, and it is antiseptic to prevent the decay of flora and fauna by the action of microorganisms, and a drug added for preservation for the purpose of preservation is a preservative. In order to maintain the quality of food, medicine, and cosmetics for a long time, preservatives that prevent decay by microorganisms are essential. Especially in the case of cosmetics, the shelf life is relatively long, and in the process of use and storage method, there is a high possibility of contact with microorganisms, various carbon sources and nitrogen sources, and high moisture content essential for microbial growth. There are more and more needs and problems with preservative treatment.

If an appropriate preservative system is not established in cosmetics, microorganisms multiply during manufacturing and consumer use, causing metabolic metabolism, causing odors and odors, or changes in product properties due to discoloration and product pH changes. It also causes harmful effects on the human body, such as causing irritation to the human body due to metabolites and microorganisms generated during the metabolic process. Especially pathogenic microorganisms cause disease.

Thus, preservatives in cosmetics are not simply additives added to prevent spoilage of the product, but irreversibly or accidentally, from the time the cosmetics are manufactured at the factory until the end of their use by the consumer with the product. Therefore, it can be referred to as a generic name of additives added for the purpose of inhibiting the growth of microorganisms contained in the product or contaminated, to prevent the deterioration, odor, deterioration, etc. of cosmetics caused by the growth of microorganisms.

Proper addition of preservatives to cosmetics not only prevents microbial contamination of the product due to microbial contamination in the raw materials and manufacturing processes, but also prevents microbial contamination during consumer use and storage, and maintains product properties and stability in the product. In addition, health risks to consumers can be minimized.

The types of preservatives used in cosmetics are very diverse, and as the production of cosmetics increases, preservatives are more diverse and the amount of their preservatives is increasing. On the other hand, preservatives can affect the public health, so in Korea, the type and formulation limit are designated as a labeling ingredient by the Ministry of Food and Drug Safety Notice, and they are required to be labeled on the product. Article 9 and 13 (6), KFDA Notice 2000-27)

Most of the preservatives having such antiseptic effect are artificial chemically synthesized materials which are easy to manufacture, low cost and easy to mass production. Among the preservatives, representative cosmetic preservatives include methyl paraben, ethyl paraben, propyl paraben, butyl paraben, butyl paraben and quaternium-15, which are paraoxybenzoic acid esters. , Imidazolidinyl Urea Diazolidinyl Urea, Phenoxyethanol, Benzalkonium Chloride, Chloconic Acid Chlorohexidine gluconic acid and Triclosan Chemical preservatives, such as these, are mentioned.

However, these chemical preservatives impair the growth of microorganisms to impart stability to cosmetics, but at the same time may cause irritation to the user's skin. Typical examples include formalin free preservatives, including diazolidinyl urea and formalin free preservatives, including imida zolidinyl urea, which have recently been reviewed for safety around the world, and their use is on the decline. Its use is limited to cleaning products and some wash off products. It is also a preservative that is banned or strictly controlled in some countries including Japan.

Such formalin-free preservatives are known to slowly release the formalin group contained in the structure over time, and this released formalin is known to not only cause skin irritation but also cause cancer.

In addition, even parabens preservatives, which are the safest as conventional chemical preservatives and are widely used in cosmetics and medicines, are allergic to skin (Andrea Counti et al., Contact Dermatitis, 1997, 37, 35-36.) And their potential as environmental hormones (Edwin). Et al., Toxicology and Applied Pharmacology, 1998, 153, 12-19.) And resistant bacteria. In addition, the use of permissible criteria is distrusted and new problems are emerging, such as acute, chronic toxicity and mutagenesis due to persistent body accumulation (Xinhua, Food Science and Industry, 1990, 23 (4) 68-72).

As described above, the side effects of such chemical preservatives lower the user's confidence in the product and ultimately act as a consumer dissatisfaction with cosmetics and beauty products.

Therefore, active research is being conducted to reduce the amount of preservatives in cosmetics, or to use unused preservative-free systems. In addition, hypoallergenicity and toxicity on the skin can be solved to solve side effects of conventional chemical preservatives and to ensure the safety of products. There is a need for natural preservatives that do not have excessive resistance.

To date, studies on natural antimicrobial agents have reported antimicrobial activities such as alkaloids, flavonoids, phytoalexin, antimicrobial peptides and organic acids and fatty acids. It is estimated to be due to the effect by chelate. (EI-shenawy, MA et al., J. Food Protec., 1989, 52 (11), 771-778) (Bizri, JN et al., J. Food Science, 1994, 59 (1), 130-135)

However, some of these natural antimicrobial ingredients, such as spices and herbal medicines, are too dark in color and have strong raw material odor, so they are limited or unsuitable for cosmetics that require the appearance of beautiful products. It is a situation that the characteristics as a cosmetic raw material, such as lowering the, and affecting the formulation stability, such as affecting the emulsification system. In addition, the characteristics of antimicrobial raw materials have a narrower antimicrobial spectrum than chemical preservatives, and the antimicrobial active ingredients contained in plant extracts often have very low physicochemical stability against heat, light and oxygen, compared to chemical preservatives. The antimicrobial active ingredient is decomposed, and in actual use of the consumer, there is a problem in that it cannot provide sufficient antiseptic activity, and most of them are not commercialized due to the limitation as a natural substance.

Commercially available natural antimicrobial agents have been developed such as henokiitiol, cypress extract, magnonol, and grapefruit seed extract (DF-100). However, most of them are economical and antibacterial spectrum, and limited use range. Due to the problem of the more advanced natural antibacterial situation is required.

Although antimicrobial peptides have been studied as an alternative for the combined effect (Giacometti A et al., J. Antimicrob. Chemother 2000, 46 (5), 807-811), because they are peptides due to their physicochemical properties, they are relatively weak to heat, especially in nature. Because it is very vulnerable to a widely existing protease, there is a limit to use universally. Moreover, due to the lack of selectivity for bacteria, fungi and animal cells due to their mechanism of action, they are limited in their use as pharmaceuticals. It is relatively expensive (Lee JH et al., Protein.Expr.Purif, 1998 Feb; 12 (1), 53-60).

In Patent No. 10-0481637, tetraacetylphytosphingosine, pentylene glycol (Hydrolite-5), polyglyceryl-2 laurate / glyceryl caprate / polyglyceryl-10 laurate, grapefruit seed extract, Cordyceps sinensis extract An antiseptic cosmetic composition is disclosed that is added according to each prescription. However, except for grapefruit seed extract and Cordyceps sinensis extract, an antiseptic cosmetic composition using chemical synthetic raw materials may cause skin irritation, such as tetraacetyl phytosphingosine, etc. In the case of having a very low solubility characteristics, there is a problem such as the application to various cosmetic formulations are required.

Patent application No. 10-2001-0006372 discloses a technique for a natural antimicrobial agent comprising a chitooligosaccharide complex and a gold extract. However, the natural antimicrobial agent has the same stability as the existing natural antimicrobial agent, and the antimicrobial activity is smaller than that of Gram-negative bacteria, and the antimicrobial activity is relatively weak against fungi, and the microorganisms containing chitosan in the cell wall have a slight antimicrobial activity. As it has a spectrum, it is not only limited in scope of use, but also has difficulty in commercialization due to formulation problems (Riccardo M et al., Antimicrobial Society and Chemotheraphy, 1990, 34, 2019-2023).

In addition, Patent Application No. 10-2004-0080717 discloses a cosmetic composition containing chitosan and grapefruit seed extract having antiseptic and antibacterial activity, but in the case of grapefruit seed extract and chitosan, Pseudomonas aero group It shows weak antimicrobial activity against Gram-negative bacteria such as labor and management, and the application of cosmetics is limited due to the strong positive charge of chitosan.

Therefore, in order to solve the side effects of the conventional chemical preservatives and to overcome the problems as a cosmetic raw material such as the existing natural antimicrobial agent, the present inventors studied not only the antimicrobial activity, but also the characteristics as a cosmetic raw material for various natural plants. When used in combination with five gall extract, cinnamon extract, and sesame oil extract, it exhibits excellent antimicrobial activity against gram-negative bacteria and gram-positive bacteria, fungi and fungi including fungi, and has a broad antibacterial spectrum and excellent antiseptic ability on cosmetics. In addition, it has also been developed a good natural preservative-free cosmetic composition has a very low impact on the physicochemical stability and cosmetic formulations, and very low skin irritation potential compared to conventional chemical preservatives.

The present invention is to solve the problems of the prior art as described above, excellent antimicrobial and antiseptic ability in natural products, physicochemical stability and selection of extracts having a very low impact on cosmetic formulations, excellent antibacterial and antiseptics without containing preservatives It is an object to provide a natural cosmetic composition having an activity.

In addition, the present invention shows a very good antibacterial activity against fungi including gram-negative bacteria and gram-positive bacteria, fungi and yeasts by combining the natural product of Gaza extract and quinine extract, cinnamon extract, sesame oil extract and excellent antiseptic ability on cosmetics The present invention aims to provide an antimicrobial antiseptic active cosmetic having a very low effect on physicochemical stability and cosmetic formulation and low skin irritation.

In order to achieve the above object, the present invention relates to a cosmetic composition having antibacterial and antiseptic activity, containing 0.05-2.0 wt% of Gaza extract, 0.05-2.0% wt. It is a cosmetic composition having antimicrobial and antiseptic activity, further comprising at least one extract selected from the group consisting of 0.05 to 2.0% by weight of the extract.

The cosmetic composition contains a Gaza extract and a gallja extract, cinnamon extract, sewage oil extract in an appropriate ratio, exhibits excellent antimicrobial activity, wide antibacterial spectrum, excellent antiseptic ability to cosmetics, and also physicochemical stability and cosmetic formulation It is characterized by a cosmetic composition having a very low impact on the skin, and having no chemical preservative added, which is unlikely to cause skin irritation.

Gaza of the present invention is a fruit of the four seasons (Terminalia chebula Retz.) Or woolly (Terminalia chebula Retz. Var. Tomentella Kurt.), The flowering period is from June to August, the fruiting period is from August to October In autumn, mature fruits are collected and dried in the sun. Fruit shape of dried Gaza is long ovate or ovate, 2.5cm to 3.0cm long, 1.5cm to 2.5cm in diameter. The outer surface is yellowish brown to brown, with five prominent longitudinal wrinkles and irregular wrinkles in between, and the base of the diseased off. The vagina is hard and the cut side is dark brown, and the flesh is 2mm to 5mm thick. Inner rind is yellowish brown with a thickness of about 5mm, its quality is very hard, there is brown suture, and there is one seed with a diameter of about 5mm in the center. Gaza has a slightly peculiar smell and tastes bitter and sour.

Rhus japonica L. is a worm family caused by aphids (Aphis chinensis J. Bell) on the leaves of the Rhus japonica L. (R. Japonica Anacardiaceae), which is distributed throughout the country. The process of developing worms is as follows. The winged worm, which drills a hole in the worm house in late September, lays larvae on its intermediate host, Minumver sicatum (M. trichomane). The larvae suck on the juices of the parasites and grow to make worms with white lead and spend the winter. It is a pupa in the following spring and emerges from the pupa in late April to become a winged worm. The worms lay wingless worms on the branches of the red tree after mating and die. Wingless worms migrate to young leaves, where worms grow. At this time, the size of the original five times because the name is said to be fivefold. Before the early fall bugs are picked up, the worms are picked up, steamed, killed and dried. In the form of gall, the outer surface is gray brown with light hairs, 3-7cm long, 2-5cm wide and 2mm thick, and hard and easily broken. The inside is usually empty or grayish white with dead bugs and secretions, sometimes with a disgusting smell. Gathered gall dry or boil or steam in the sun. Its main component is 50 ~ 70% of pyrogalloltannin, and it contains gallic acid. The drug is used for astringents, branches, hemostatic diarrhea, sputum, diabetes, bleeding, anemia.

The cinnamon (Cassiae cortex or Cinnamomi cortex) of the present invention is dried by removing the cork layer by peeling the stems and branches of the cinnamon tree (Cinnamomum cassiablume), an evergreen tree that is native to China and India, and belonging to the family Lauraceae. Cinnamic aldehyde, Cinnamylacetate, Cinnamic acid, etc., which are essential oils, are the main components, and other organic acids, tannins, starches, resins, mucus, sucrose (Mannitol), minerals, etc. It is said to be a raw material of cinnamon oil which contains a small amount and has strong fragrance.

Fructus of the present invention is an unripe fruit of a deciduous tree or a small tree (Evodia officinalis Dode or E. rutaecarpa Bentham), which is a deciduous shrub or subfamily tree belonging to the Rhusaceae. Tinnitus includes lactation, sewage, ochu, weak lactation, and left power. This fruit, used as medicinal herb oil, is spherical-spherical, the outer side is dark brown-grey brown, and many of the oils are concave and small dots appear, among which there are residues of shipper, but some are separated. Fruit disease dense with gray-green hairs. The rind is usually open and the ovate is divided into 5 lobes, each containing a globose seed of obovate-spherical brown-dark brown or blue color. It has an unusual aroma, tastes spicy, and aftertaste is persistent. Sewage tree grows about 3 ~ 10m high, and dense long soft hairs of light tan color are found throughout the tree. The leaves are opposite each other. The odd leaves are 16 ~ 32mm long. Small leaves are 5-9 in number, oval or oval, 6-15cm long. Leaf edges have dull teeth with or without teeth, and springs on the back. In early summer, a short cone inflorescence emerges from the tip of the branch and small white flowers bloom. Hermaphroditisa is a five-mercury flower. Female petals are relatively large and have soft hairs on the inside. Osuyu is native to China. It is mainly produced in China's provinces such as Guizhou, Guangxi, Hunan, Yunnan, Zhejiang, and Xixi. It is known to be grown in Gyeongju in Korea.

As used in the present invention, the Gaza, Gallja, cinnamon and sesame oil extracts are obtained by leaching or transferring leaching from Gaza or Caucasus, Ginseng, Cinnamon, and Fructus, or concentrates obtained by partially or fully concentrating the leachate, or again concentrated. It includes the extraction extract prepared by drying water and the chemical itself which exhibits the main effect contained in the extract.

The Gaza extract of the present invention is from the group consisting of water, ethanol, methanol, butanol, propanol, butylene glycol, propylene glycol, chloroform, ethyl acetate, dichloromethane, hexane, petroleum ether and diethyl ether It is extracted with one or more solvents selected.

Extraction method is to immerse the dried powder of Gaza or Gaja meat in a solvent for 5 to 72 hours at 15 to 50 ℃ or extracted for 5 to 72 hours in an extractor equipped with a cooling capacitor, and then concentrated under reduced pressure below 50 ℃ and concentrated under reduced pressure. It is prepared by lyophilization. In addition, after performing the extraction process may include a step of low temperature aging for 1 to 10 days at 4 to 15 ℃. In the method for preparing the Gaza extract, the extraction solvent may be used 100 to 1500 parts by weight based on 100 weight of Gaza or Caja meat dry weight.

The gall bladder, cinnamon and sesame oil extracts of ginseng, cinnamon and sesame oil each contain water, ethanol, methanol, butanol, propanol, butylene glycol, propylene glycol, chloroform, ethyl acetate, dichloromethane, hexane, petroleum ether, and distillate. It is extracted with one or more solvents selected from the group consisting of ethyl ether.

Extraction method is to immerse the dried powder of each gall, cinnamon, sewage oil for 5 to 72 hours at 15 to 50 ℃ in a solvent or 5 to 72 hours to extract in an extractor equipped with a cooling capacitor, concentrated under reduced pressure at 50 ℃ or less and Lyophilize the concentrate. In addition, the extraction process may further include a step of low temperature aging for 1 to 10 days at 4 to 15 ℃. In the manufacturing method of the gall, cinnamon, sewage oil extract, the extraction solvent may be used 100 to 1500 parts by weight based on the weight of the dry powder 100.

In addition, the cosmetic composition according to the present invention may contain, in addition to the above-mentioned extract, other components that can give a synergistic effect to the main effect, preferably within the range of not impairing the main effect of the present invention. The Ga, gall, cinnamon and sesame oil extract may be present in the composition in an amount of 0.1 to 10% by weight based on the total weight of the composition.

If the plant extract is present in the form of a solution containing the extract, those skilled in the art will be able to adjust the amount of this solution in the composition according to the invention within the concentration range.

The compositions of the present invention may be in the form of an aqueous, aqueous-alcoholic or oily solution, oil-in-water or water-in-oil or multiple emulsions, aqueous or oily gels, liquid, pasty or solid anhydrous products, oil dispersions in aqueous phase using globules. And more preferably in the form of lipid vesicles in ionic and / or nonionic form.

The composition may be somewhat fluid and may have the appearance of a white or colored cream, ointment, milk lotion, serum, essence, paste or mousse. It may optionally be applied to the skin in the form of an aerosol or may be in the form of a solid, such as a stick. It may be used as a skin care product and / or makeup product.

In a known manner, the compositions according to the invention are also useful in the cosmetic field as conventional auxiliaries such as hydrophilic or lipophilic gelling agents, hydrophilic or lipophilic active agents, preservatives, antioxidants, solvents, fragrances, fillers, blockers, pigments, odorants and dyes. It may contain. The amounts of these various adjuvants are amounts conventionally used in the art, such as from 0.01% to 20% by weight relative to the total weight of the composition. Depending on their nature, such adjuvants may be incorporated into the fatty phase, aqueous phase, lipid vesicles and / or nanoparticles. In any case the adjuvant and its proportions should be selected so as not to adversely affect the desirable properties of the cosmetic composition according to the invention. will be.

The composition of the present invention may further comprise an excipient. The excipients are typically used in cosmetics, and are representative of water, physiological saline, glycerol and the like.

The cosmetic composition of the present invention is prepared in the form of color cosmetics such as foundation lotion and foundation, lipstick, mascara or makeup base such as flexible lotion, milk lotion, nourishing cream, massage cream, essence, cleansing foam, cleansing water, pack or body oil can do. When the cosmetic of the present invention is used as a detergent, it may be prepared as a face wash and a bath.

Hereinafter, the present invention will be described in detail with reference to the following examples and experimental examples, which are only presented to aid the understanding of the present invention, but the present invention is not limited thereto.

Example 1 Preparation of Gaza Extract

The thinly dried and dried Gaza was refluxed three times for 5 hours with 70% (V / V) ethanol aqueous solution, and the mixture was cooled and then filtered through Whatman # 5 filter paper. The filtered extract was concentrated under reduced pressure at 50 ° C. or lower and dried using a lyophilizer to obtain 38 g of Gaza extract.

Example 2: Preparation of Mellitus Extract

The dried and dried malt was refluxed three times for 5 hours with a 70% (V / V) ethanol aqueous solution, and then cooled and filtered through Whatman # 5 filter paper. The filtered extract was concentrated under reduced pressure at 50 ° C. or lower, and dried using a lyophilizer to obtain 40.4 g of quinine extract.

Example 3: Preparation of Cinnamon Extract

The dried cinnamon was refluxed three times for 5 hours with an aqueous 70% (V / V) ethanol solution, cooled, and filtered through Whatman # 5 filter paper. The filtered extract was concentrated under reduced pressure at 50 ° C. or lower and dried using a lyophilizer to obtain 6.34 g of cinnamon extract.

Example 4: Preparation of Sewage Extract

The filthy filthy oil was chopped and refluxed three times with an aqueous 70% (V / V) ethanol solution three times for 5 hours, cooled, and filtered through Whatman # 5 filter paper. The filtered extract was concentrated under reduced pressure at 50 ° C. or lower, and dried using a lyophilizer to obtain 18.14 g of sewage extract.

Experimental Example 1: Antimicrobial Activity

In order to measure the antimicrobial activity of the extracts were measured the minimum inhibitory concentration using a solid culture dilution method (Agar Serial Dilution Method). The strains used were Gram-positive bacteria (Bacillus subtilis ATCC 6633), Staphylococcus aureus ATCC 6538P, Gram-negative bacteria (Escherichia coli ATCC 8739), Pseudomonas aeruginosa ATCC 9027, and yeast (Candida ida). albicans ATCC 10231), as a filamentous fungus, Aspergillus niger ATCC 22343.

Bacteria were tryptic soy broth (Tryptic soy broth) was used to inoculate the culture medium and pre-cultured for 24 hours in a 37 ℃ shaking incubator. Potatodextrose broth was used for cultivation of the yeast, and the culture was inoculated with the bacteria and precultured at 25 ° C. incubator for 2 days. Potato dextrose agar was used for the cultivation of filamentous fungi, and inoculated with the bacteria in the culture medium, which was precultured at 25 ° C. for 7 days.

More specific antimicrobial test was first inoculated bacteria in tryptic soy broth for bacteria, pre-incubation at 37 ℃ for 24 hours, in the case of yeast, bacteria in Potato dextrose broth 2 days pre-incubation at 25 ℃, filamentous bacteria inoculated bacteria in Potato dextrose agar (Potato dextrose agar) and incubated for 7 days in a 25 ℃ incubator, then formed on the surface of the medium using a sterile swab Spores of filamentous fungi were collected and diluted in sterile saline.

On the other hand, add 2 ml of each extract diluted in proper concentration to 5% Dimethylsulfoxide (DMSO) saline solution for each extract and test strain in sterilized Petri dish, and 2ml of 5% Dimethylsulfoxide saline solution for control group, After sterilization in a plate, 18 ml each of tryptic soy agar medium and potato dextrose agar medium, cooled to 48 ° C, mixed well, and left to solidify.

Then, each pre-cultured test bacteria are plated on each petri dish with a final concentration of about 1 × 10 ⁶ CFU for bacteria, and each petri dish with a uniform concentration of about 1 × 10 ⁵ CFU for yeast. In the case of filamentous fungi, each petri dish is smeared with a bacterial concentration of about 1x10 ⁴ CFU. Each petri dish was incubated for 24 hours at 37 ° C, yeast for 3 days in a 25 ° C incubator, and filamentous bacteria for 7 days in a 25 ° C incubator, followed by colony formation in each compartment. The minimum antimicrobial concentration of is called the minimum inhibitory concentration (MIC).

division Inhibitory concentration (% by weight) B. subtilis S. aureus E. coli P. aeruginosa C. albicans A. niger Gaza Extract 0.1 0.05 0.025 0.04 1.0 or higher 0.2 Gall bladder extract 0.025 0.0125 0.2 0.4 0.5 or more 0.5 Cinnamon Extract 1.0 1.0 or higher 1.0 or higher 1.0 or higher 0.025 0.04 Sewage Extract 1.25 2.0 or higher 2.0 or higher 2.0 or higher 0.4 0.1

As shown in Table 1, the extract of Gaza showed excellent antimicrobial activity even at concentrations of 0.05 wt% or less against Gram-negative bacteria E. coli and Pseudomonas aeruginosa, but relatively weak antimicrobial activity against Gram-positive Bacillus subtilis. In addition, Candida yeast showed very weak antimicrobial activity and relatively weak antimicrobial activity against Black Bacillus.

In the case of five-german extract, the antimicrobial activity of Gram-negative bacteria such as Bacillus subtilis and Staphylococcus was excellent at a concentration of 0.025% by weight or less, but showed relatively weak antimicrobial activity against Gram-negative bacteria Escherichia coli and Pseudomonas aeruginosa. It also showed very weak antimicrobial activity against Candida yeast and Black Bacillus.

Cinnamon extract showed weak antimicrobial activity against both Gram-negative bacteria and Gram-positive bacteria, but showed effective antimicrobial activity at concentrations below 0.04% by weight against fungi, yeast and filamentous fungi. In the case of sewage, although the antimicrobial activity was weak against bacteria, it was confirmed that the antimicrobial activity against filamentous fungi was excellent.

Experimental Example 2: Latex Preparation

Emulsions containing cosmetics containing the extract and conventional chemical preservatives were prepared. Cosmetics used in the experiment is in the form of an emulsion, the composition is shown in Table 2. First, the a) phase recorded in Table 2 is heated and stored at 70 ° C. Phase B) is added to this and then emulsified uniformly with a homomixer after pre-emulsification. After cooling, the plant extract of d) or a chemical preservative was added thereto, and stirred uniformly to prepare an emulsion (Examples 5 to 14, Comparative Example 1, and Comparative Example 2).

division ingredient weight% end Purified water 70.0% Disodium ID 0.01% Panthenol 0.2% Betaine 3.0% Butylene Glycol 4.0% glycerin 3.0% I Butylated hydroxytoluene 0.02% Stearic acid 0.5% Cetearyl Alcohol 0.5% Glyceryl Cerate 0.3% Polysorbate 60 0.6% Methylglucosesquistearate 1.3% Polyethylene glycol monostearate 1.0% Butyrodperm PARKII 2.0% Tocopheryl Acetate 0.1% Mineral oil 10.0% Dimethicone 0.3% Acrylate / sodium acrylamide copolymer 0.9% Cyclomethicone 1.0% All Triethanolamine 0.1% Purified water 1.0% la Antibacterial natural products or preservatives 0.5% Purified water Remaining amount

Examples 5 to 10 Preparation of Latex Containing Antimicrobial Active Extracts

According to the composition of Table 3, the emulsion of Examples 5 to 10 was prepared by the method of Experimental Example 2 containing the extract.

ingredient Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 Gaza Extract 0.5% - - - 0.25% - Gallnut extract - 0.5% - - 0.25% - Cinnamon Extract - - 0.5% - - 0.25% Sewage Extract - - - 0.5% - 0.25% Methyl Paraben - - - - - - Profile paraben - - - - - - Imidazolidinylurea - - - - - -

Example  11-14: Preparation of Latex Containing Antimicrobial Active Extracts

According to the composition of Table 4, the emulsion of Examples 11 to 14 was prepared by the method of <Experimental Example 2> containing the extract.

ingredient Example 11 Example 12 Example 13 Example 14 Comparative Example 1 Comparative Example 2 Gaza Extract 0.25% 0.2% 0.2% 0.2% - - Gallnut extract - 0.1% 0.2% 0.1% - - Cinnamon Extract 0.25% 0.1% 0.1% - - - Sewage Extract - 0.1% - 0.2% - - Methyl Paraben - - - - 0.2% - Profile paraben - - - - 0.1% - Imidazolidinylurea - - - - 0.2% - Purified water - - - - - 0.5%

Comparative Examples 1 and 2

According to the composition of Table 4, the emulsion of Comparative Example 1 containing a chemical preservative and Comparative Example 2 containing no chemical preservative and the extract was prepared by the method of <Experimental Example 2.

Experimental Example 2: Emulsification Stability Evaluation Experiment

In order to confirm the effect of the extract as a cosmetic raw material and the effect on the cosmetic formulation, the emulsion stability of the emulsion prepared in Examples 5 to 14, Comparative Example 1, Comparative Example 2 was stored and observed for 6 months at high temperature (45 ℃) The results are shown in Table 5 and Table 6.

division Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 Viscosity 2600 cps 1800 cps 1480 cps 2250 cps 1900 cps 1650 cps Emulsification stability No phase separation Weak Phase Separation Phase separation No phase separation No phase separation Weak Phase Separation

division Example 11 Example 12 Example 13 Example 14 Comparative Example 1 Comparative Example 2 Viscosity 1800 cps 2400 cps 2200 cps 2500 cps 2480 cps 2550 cps Emulsification stability Weak Phase Separation No phase separation No phase separation No phase separation No phase separation No phase separation

As can be seen from the results of Table 5 and Table 6, the emulsion of Example 6 using the galleng extract alone and Example 7, using the cinnamon extract alone Example 10 added 0.25% each of the cinnamon and sesame oil extract was chemical Compared with Comparative Example 1 without the addition of preservatives and Comparative Example 2 without the addition of chemical preservatives and extracts, a marked drop in viscosity and phase separation were observed, indicating a significantly lower emulsion stability. In addition, the emulsions of Example 9, which was added 0.25% each of the Gaza extract and the Fructus extract, and Experimental Example 11, which was added 0.25% of the cinnamon extract, also showed relatively low emulsion stability.

Therefore, as in the emulsions of Examples 6 to 8, Examples 9 and 11 above, when a high content of an extract alone, ie, gall bladder extract and cinnamon extract, is added, it has an adverse effect on the emulsion stability of the cosmetic. Confirmed. However, as in the latex of Examples 12 to 14, the cosmetics in which appropriately mixed five gall extract, Gaza extract, cinnamon extract, sesame oil extract and the like showed excellent emulsion stability.

Experimental Example 3: Confirming the preservative activity of the emulsion

In order to confirm the antiseptic activity of the cosmetic composition containing the extract, the antiseptic activity confirmation test of the emulsion prepared in Examples 5 to 14, Comparative Example 1, Comparative Example 2 was performed. The antiseptic activity test is a method of confirming death after inoculation of microorganisms into cosmetics (Challenge test, Inoculum test) .The cosmetics have an appropriate antiseptic system, which prevents microbial contamination during consumer use and storage. It is a test to ensure that the health hazards to consumers can be minimized by maintaining the appearance and giving the product safety and stability. The test method was a test method of the Microbiology Guidelines of the Cosmetic, Toiletry, and Fragrance Association (CTFA).

The strains used were Gram-positive bacteria (Bacillus subtilis ATCC 6633), Staphylococcus aureus ATCC 6538P, Gram-negative bacteria (Escherichia coli ATCC 8739), Pseudomonas aeruginosa ATCC 9027, and yeast (Candida ida). albicans ATCC 10231), as a filamentous fungus, Aspergillus niger ATCC 22343.

Bacteria were tryptic soy broth (Tryptic soy broth) was used to inoculate the culture medium and pre-cultured for 24 hours in a 37 ℃ shaking incubator. Potatodextrose broth was used for cultivation of the yeast, and the culture was inoculated with the bacteria and precultured at 25 ° C. incubator for 2 days. Potato dextrose agar was used for the cultivation of filamentous fungi, and inoculated with the bacteria in the culture medium, which was precultured at 25 ° C. for 7 days.

More specific antiseptic activity test is first prepared by inoculating bacteria in tryptic soy broth for bacteria, pre-incubation at 37 ℃ for 24 hours, in case of yeast, Potato dextrose broth Inoculate the bacteria to pre-incubate for 2 days in a 25 ℃ shaker incubator, filamentous inoculation bacteria in Potato dextrose agar (Potato dextrose agar) and incubated for 7 days in a 25 ℃ incubator, using a sterile swab, Spores of filamentous fungi formed on the surface of the medium were collected and diluted in sterile saline.

On the other hand, test bacteria prepared by preculture in 20 to 50 g of the test cosmetics contained in a sterile container are inoculated with a germ concentration of about 1 × 10 ⁶ CFU in the case of bacteria, and about 1 × 10 ⁵ CFU in the case of yeast. Inoculate each sample at a bacterial concentration of about 1 × 10 ⁴ CFU. Immediately after inoculation, each sample was taken, and a total aerobic bioburden test was performed, and bacteria were incubated at 37 ° C. for 24 hours, yeast was incubated for 3 days in a 25 ° C. incubator, and filamentous fungi were incubated for 3 days in a 25 ° C. incubator. Check the initial bacterial count of the test bacteria inoculated into each sample. Afterwards, each inoculated sample is stored at room temperature, and after 1, 2, 3, 7, 14, and 28 days, the total aerobic bioburden test confirms the number of bacteria and the degree of death of the test bacteria. The antiseptic activity of the cosmetic was measured. The results are shown in FIGS. 1 to 6.

As can be seen from the results of Figure 1, the milk solution containing 0.5% of the Gaza extract of Example 5 was confirmed to have an appropriate antiseptic activity by killing all of the Gram-negative bacteria E. coli and Pseudomonas aeruginosa after 7 days, Gram-positive bacteria such as Bacillus subtilis and Staphylococcus were detected after 7 days, and showed relatively weak antiseptic activity. In addition, the fungi Candida yeast and black fungi were detected after 14 days of inoculation, the test bacteria were detected, and have very weak antiseptic activity, thereby confirming that the possibility of microbial contamination by the fungi is very high. )

The latex containing 0.5% of the blastocyst extract of Example 6, Gram-positive bacteria and Staphylococcus were almost all test bacteria were killed after 3 days of inoculation, it was confirmed that they have very good antiseptic activity, but Gram For bacteria E. coli, Pseudomonas aeruginosa and fungi, Candida yeast and B. aeruginosa, test bacteria were detected after 14 days of inoculation, and have very weak antiseptic activity. Thus, there is a high possibility of microbial contamination by Gram-negative bacteria and fungi. It was confirmed to be high (FIG. 1).

As can be seen from the results of Figure 2, the milk liquid containing 0.5% cinnamon extract of Example 7 is a fungus Candida yeast and black yeast bacteria all test bacteria are killed 3 days after the inoculation, and has very excellent antiseptic activity However, both Gram-negative bacteria and Gram-positive bacteria were detected and most of the test bacteria were not killed after 14 days of inoculation, and thus, they had very weak antiseptic activity against bacteria. Thus, the possibility of microbial contamination by bacteria was very high. It was confirmed that (Fig. 2).

The milky milk containing 0.5% sewage extract of Example 8 was found to have very good antiseptic activity after 7 days of inoculation against fungi candida yeast and black yeast fungi, but had very good antiseptic activity. Test bacteria were detected even after 14 days of inoculation of both positive bacteria and had very weak antiseptic activity against bacteria, thereby confirming a high possibility of microbial contamination by bacteria (FIG. 2).

As can be seen from the results of Figure 3, the milky milk containing 0.25% of the Gaza extract and the fivefold extract of Example 9, Gram-negative bacteria E. coli, Pseudomonas aeruginosa, Gram-positive bacteria such as Bacillus subtilis and Staphylococcus three days after inoculation The test bacteria were killed and it was confirmed that they had very good antibacterial activity against bacteria. However, for the fungi Candida yeast and Black fungus, most of the test bacteria were detected after 14 days of inoculation, and have very weak antiseptic activity, thereby confirming the possibility of microbial contamination by fungi. 3)

The milky milk containing 0.25% of the cinnamon extract and the sesame oil extract of Example 10 was found to have very good antiseptic activity after almost 3 days of inoculation of the fungi Candida yeast and B. aeruginosa. Gram-negative bacteria E. coli, Pseudomonas aeruginosa, Gram-positive bacteria, Bacillus subtilis and Staphylococcus were detected in a large number of test bacteria even after 14 days of inoculation, and have very weak antiseptic activity. It was confirmed to be very high (FIG. 3).

As can be seen from the results of Figure 4, the milk solution containing 0.25% of the Gaza extract and 0.25% cinnamon extract of Example 11 killed all test bacteria after 7 days in the case of bacteria, after 7 days also for fungi Most of the test bacteria were killed, and it was confirmed to have an appropriate antiseptic activity. However, as shown in Table 6, the effect on the emulsion stability is relatively large, it was confirmed that it is not an appropriate preservative-free cosmetic composition (Fig. 4).

In the case of milky milk containing 0.2% of Gaza extract of Example 12, 0.1% of Gallja extract, 0.1% of cinnamon extract and 0.1% of sesame oil extract, both Gram-positive bacteria and Gram-negative bacteria were killed after 7 days of inoculation. After 7 days, most of the test bacteria were killed, and it was confirmed that they had very excellent antiseptic activity compared with Comparative Example 1 to which 0.5% of the chemical preservative was added. In addition, as shown in Table 6, the effect on the emulsion stability was also very small, had excellent cosmetic raw material properties, it was confirmed that it is a suitable antiseptic-free cosmetic composition with a very good antimicrobial activity and a broad antibacterial spectrum (Fig. 4).

As can be seen from the results of Figure 5, even in the case of milk containing the extract of the Gaza extract 0.2%, gallja extract 0.2%, cinnamon extract of Example 13, both Gram-positive bacteria, Gram-negative bacteria, most after 3 days of inoculation After 7 days, most of the test bacteria were killed, and it was confirmed that the fungus had very excellent antiseptic activity compared with Comparative Example 1 to which 0.5% of the chemical preservative was added. In addition, as shown in Table 6, the effect on the emulsification stability is also very small, had excellent cosmetic raw material properties, it was also confirmed that it is a suitable antiseptic-free cosmetic composition having a very good antimicrobial activity and a broad antimicrobial spectrum (Fig. 5).

In the case of milky milk containing 0.2% of Gaza extract of Example 14, 0.1% of Gallja extract, and 0.2% of sesame oil extract, most of Gram-positive bacteria and Gram-negative bacteria were killed 7 days after inoculation. After one day, most of the test bacteria were killed, and it was confirmed to have a very good antiseptic activity compared with Comparative Example 1 to which 0.5% of the chemical preservative was added. In addition, as shown in Table 6, the effect on the emulsification stability is also very small, had excellent cosmetic raw material properties, it was also confirmed that it is a suitable antiseptic-free cosmetic composition having a very good antimicrobial activity and a broad antimicrobial spectrum (Fig. 5).

As can be seen from the results of Figure 6, in the case of Comparative Example 1 containing the chemical preservatives methyl paraben 0.2%, propyl paraben 0.1%, imidazolidinyl urea 0.2%, it shows an appropriate antiseptic activity against both bacteria and fungi, As shown in Table 6, the effect on the emulsion stability was also small. And in the case of Comparative Example 2 containing no chemical preservatives and antimicrobial extract, it was confirmed that most of the test bacteria were detected or rather increased after 28 days (Fig. 6).

Experimental Example 4: Skin irritation potential test

The possibility of skin irritation was confirmed by a closed patch test. Thirty healthy men and women of 20 to 40 years of age with no abnormality on the skin were placed in the upper arms of the arms of Examples 12 to 14 and a certain amount of latex containing the chemical preservative of Comparative Example 1 was buried in the chamber, and closed for 48 hours. After the patch test was performed, the degree of erythema formation and irritation of the test subjects were confirmed through questions.

Determination of skin irritation was made according to the skin irritation index criteria of Table 7 made by using sodium lauryl sulfate, no irritation of skin irritation index of 0 to 1, no irritation of 2 to 3 irritation, 4 or more The stimulus was judged to be a strong stimulus. The experimental results are shown in Table 8.

division Stimulus index Criteria No irritation 0 No erythema has formed and the investigator does not complain of irritation or itching. One Erythema did not form, but the investigator complained of minor itching. Slight irritation 2 There is a slight skin change or the investigator complains of minor irritation. 3 Weak erythema is formed and the investigator complains of irritation Strong stimulation 4 A clear form of erythema was formed and the investigator complained of irritation. 5 Vivid red erythema formed, and test subject complains of strong irritation

division Stimulus Stimulus rate Mean stimulation index No irritation Slight irritation Strong stimulation Example 12 29 One 0 3.3% 0.50 Example 13 27 3 0 10.0% 0.90 Example 14 28 2 0 6.7% 0.70 Comparative Example 1 21 9 0 30.0% 1.23

As can be seen from the results of Table 8, in the case of Comparative Example 1 containing the chemical preservatives methyl paraben 0.2%, propyl paraben 0.1%, imidazolidinyl urea 0.2%, the stimulation incidence of stimulation index 2 or more averaged 30% A stimulation index of 1.23 was shown, indicating a very high probability of stimulation or mild irritation. However, all of the emulsions of Examples 12 to 14, in which the mixture of Gaza extract, Fructus extract, Cinnamon extract and Fructus extract were mixed in an appropriate ratio, 10% irritation rate Very low irritation incidence was shown below, and the average irritation index was also 0.9 or lower, indicating that the cosmetic composition was very low in the possibility of irritation.

As described above, the cosmetic composition according to the present invention contains the Gaza extract, the Gallja extract, the cinnamon extract, the sesame oil extract in an appropriate ratio, exhibits very good antimicrobial activity, and the antimicrobial spectrum is wide, so that the antiseptic ability on cosmetics is excellent. .

In addition, the effect on the physicochemical stability and cosmetic formulations is very small, and since there is no chemical preservative added, the possibility of skin irritation is very low.

In the above description of the preferred embodiment of the present invention, those skilled in the art will be able to perform various modifications without departing from the gist of the present invention, and such modifications are within the protection scope of the present invention. The protection scope of the present invention should be construed as described in the claims.

Claims (3)

Preservative containing 0.05-2.0% by weight of Gaza extract and 0.05-2.0% by weight of gallnut extract, and further comprising one or more extracts selected from the group consisting of cinnamon extract 0.01-0.5% by weight and sewage extract 0.05-2.0% by weight. Cosmetic composition having activity. delete delete

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