KR20150001021A - Antiseptic Composition without Skin Irritation, and Goods Containing the Same - Google Patents

Abstract

The present invention relates to a preservative composition which has an excellent antimicrobial ability against harmful microbes and simultaneously does not irritate the skin of human body; and to an article including the preservative composition. The preservative composition comprises propylene glycol, benzoic acid, cetyl pyridinium chloride and climbazole. According to the present invention, the preservative composition and the article including the same have excellent antimicrobial effects against various microbes such as bacteria, yeasts, fungi, etc. and are free from change in components even when stored for a long period of time, thereby exhibiting excellent persistency. In addition, the preservative composition and the article including the same comprise components which are safe for the skin, hypoallergenic and harmless, thereby can be used securely for the skin of the human body, and can safely protect the skin exposed to the outside from the surrounding harmful environment.

Description

[0001] Antiseptic Composition without Skin Irritation, and Containing the Same [

The present invention relates to an antiseptic composition and an article containing the anticancer composition which do not irritate human skin while having excellent antibacterial ability against harmful microorganisms.

The skin of the human body is an indispensable body for maintaining life by biochemically functioning to block the harmful substances physically and chemically entering from the outside world while protecting the body and metabolizing the whole body.

However, skin is constantly being attacked from harmful microorganisms of the outside world. In the case of a weakened skin condition or weak immunity, it is often caused by the attack of microorganisms, resulting in an abnormal symptom,

Microorganisms such as germs and molds encountered in everyday life are not only highly abundant but also widely distributed in the natural world such as soil, air, water, and seawater, and can grow and reproduce whenever the growth conditions are met. Human diseases, food corruption, housing, clothing, and industrial products are all seriously affected by microorganisms.

Accordingly, soaps or disinfectants are used to remove and eliminate unwanted pollutants such as dirt and germs from the skin. These products are applied to the skin and then washed with water and removed from the skin together with dirt and bacteria in the washing process So that it has a limited temporal effect.

Accordingly, there has been developed a skin product that minimizes harmful bacteria and viruses and continuously protects the skin from contaminants in contact with the skin after being applied to the skin. For example, cosmetics, external preparation for skin, wipes, diapers, sanitary products, A preservative is added to the product of the present invention to prevent deterioration or sterilization of microorganisms due to incorporation of microorganisms such as bacteria or fungi at the time of manufacture and use.

Preservative components used in these products include, for example, isopropylmethylphenol, p-oxybenzoic acid ester, phenols such as phenoxyethanol and hinokitiol, salicylic acid and its salts, dehydroacetic acid and its salts, sorbic acid and its Quaternary ammonium salts such as benzalkonium chloride, benzethonium chloride and alkyltrimethylammonium chloride, amphoteric surfactants such as alkylaminoethylglycine hydrochloride and stearylhydroxyethylbetaine sodium chloride, polyhexamethylene guanidine (PHMG) Guanidinium compounds such as polyhexamethylene biguanide (PHMB) and oligo (2- (2-ethoxy) -ethoxyethyl guanidium chloride), isothiazolinone compounds such as chloromethyl isothiazolinone and methyl isothiazolinone Compounds, imidazoline compounds, triazine compounds, formaldehyde releasing compounds, 3-iodo-2-propynyl butyl Carbodiimide, carbamate, iodopropynyl butylcarbamate, photosensitizer, zinc undecylate, biphenyl, iodine and alcohol.

However, the preservatives are restricted in use or restricted in use due to human toxicity and skin irritation. In particular, PHMG and PGH are guanidinium chemicals which cause acute lung injury syndrome caused by a humectant detergent, and 3- Since iodine-2-propynylbutylcarbamate is a substance regulated for use in infant products due to harmfulness, it is required to develop a preservative that can replace them.

Due to these problems, natural materials having the ability to improve skin health and preservation performance have been used in the skin hygiene industry. These natural substances tend to be unstable and decomposed depending on time and temperature, There is a problem that the efficacy is limited.

Therefore, the antiseptic should have sterilization, antibacterial or antiseptic ability, and it should not harm the skin, minimize the skin irritation, be stable to the external environment change, and not impair the quality of the product due to the addition of preservative.

To satisfy these conditions, Korean Patent Publication No. 1195724 discloses a preservative composition which avoids the use of a preservative of harmful components in the human body and has the same or higher repelling force and is non-irritating to the skin and harmless to the human body .

The invention relates to cetylpyridinium chloride; Sodium dihydroacetate; And one kind selected from sodium benzoate, potassium sorbate, sodium propionate, calcium propionate, glucono delta lactone, and a mixture thereof, to the wet tissue to provide an excellent antibacterial and antifungal effect on the microorganism.

However, although the compositions are found to be safe as food preservatives, their safety has not been confirmed when they are applied to skin, and they are irritating to human skin, which may cause allergies or atopy. There is a restriction on its use as a preservative because odor is generated.

Korean Patent Laid-Open Publication No. 2002-0092774 discloses an antiseptic and repellent composition comprising a natural antiseptic and an insect repellent component in a maleic anhydride adduct of a terpene compound. The composition is applied to human and animal It has excellent safety and low impact on the environment, so it can be widely applied to a wide range of fields.

However, since the composition has insufficient preservative effect, it has to be used at a high concentration in order to obtain a sufficient preservative effect, and the natural material is easily deteriorated during storage, shortening the distribution period.

A problem to be solved by the present invention is to provide a preservative which is excellent in antiseptic ability and is safe to skin and has no change in composition due to external environmental change, and can be used for a long period of time while being stored, and an article containing the same.

In order to solve the above problems, the present invention provides a preservative composition comprising propylene glycol, benzoic acid, cetylpyridinium chloride and climbazole.

At this time, it is preferable that the preservative composition is composed of 65 to 80% by weight of propylene glycol, 1 to 20% by weight of benzoic acid, 3 to 20% by weight of cetylpyridinium chloride and 2 to 10% by weight of climbazole.

The antiseptic composition preferably further comprises sodium benzoate, and the sodium benzoate is more preferably contained in an amount of 0.1 to 5.0% by weight of the antiseptic composition.

The preservative composition preferably has a pH of 3 to 7, and the preservative composition is preferably an aqueous solution of 0.1 to 1.0 wt%.

The present invention also relates to a diaper, a tissue, a wet tissue, a cosmetic, a detergent, a skin external preparation, a sanitary article, a sanitary article, a sanitizer, an oral cleanser, a shampoo, a soap, a shower gel, a water treatment agent, Additives or fiber additives.

The preservative composition according to the present invention and the article containing the same exhibit an excellent antimicrobial effect against various microorganisms such as bacteria, yeast, fungi,

In addition, it can be safely used on the skin of the human body, composed of harmless ingredients that are safe to the skin and low in stimulus, and can safely protect the skin exposed to the outside from the surrounding harmful environment.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a photograph showing a result of a sterilizing test of a preservative composition according to the present invention. FIG.
FIG. 2 is a photograph showing the results of a test of maintaining the sterilizing power of the preservative composition according to the present invention. FIG.
FIG. 3 is a photograph showing the results of the parallel partition line test of the preservative composition according to the present invention. FIG.

The present invention provides a preservative composition comprising propylene glycol, benzoic acid, cetyl pyridinium chloride and climbazole.

The propylene glycol is a colorless, transparent, tasteless, odorless liquid similar to glycerin, which is superior in dissolving power compared to glycerin, stable in heat and sunlight, and not volatile.

It is also used for emulsifying stabilizers, humectants, preservatives and air disinfection because it has a lower freezing temperature than saline solution, prevents the growth of fungi, and has a lowering effect on water activity without corrosiveness or toxicity.

The propylene glycol is preferably contained in the total antiseptic composition in an amount of 65 to 80% by weight, and serves as a solvent in the present invention.

The benzoic acid is a colorless or white crystal which is well soluble in an organic solvent, stable to light and heat, continuously exhibiting a bacteriostatic action and an antibacterial effect, and is used as a disinfectant and an anti-infectious drug.

Benzoic acid has a strong antiseptic effect against bacteria, but the antibacterial effect against emulsified products is lowered, and propylene glycol prevents the deterioration of such repelling force.

The benzoic acid preferably contains 1 to 20% by weight of the antiseptic composition. If the content is less than 1% by weight, the antibacterial activity is lowered and the pH of the preservative composition can not be sufficiently lowered. If the content exceeds 20% by weight, solubility in the propylene glycol solvent And the pH of the preservative composition becomes too low to change the skin to acidic and destroy the balance of the skin, thereby causing side effects such as skin discoloration, rash, and burn.

The cetylpyridinium chloride is a cationic surfactant and has no odor, is harmless to human body, and has excellent bactericidal and microbial activity against bacteria and microorganisms. Therefore, it is mainly used for mouth cleaner, toothpaste, oral spray, nasal spray, ) And provides the effect of reducing bad breath, periodontal disease, stones, tooth decay and reducing gingivitis.

Cetylpyridinium chloride starts to freeze at about 15 캜 when it is dissolved in purified water and recrystallization starts at about 13 캜. However, since propylene glycol as a solvent of the present invention does not cause freezing or recrystallization at the image temperature, There is no.

The cetylpyridinium chloride is preferably contained in an amount of 3 to 20% by weight of the antiseptic composition. If the content is less than 3% by weight, the antimicrobial and antifungal activity against the microorganism is lowered and the broad spectrum antimicrobial spectrum is not obtained. It is possible to dry or sensitize the skin and lower the immune system of the skin, which may lead to an abnormality in the skin toxicity and physiological function to the human body, and it is difficult to control the physical properties at the time of manufacture and the compatibility with other compounds is poor have.

The climbazole is a white crystalline powder, exclusively for ovarian nasal fungi and tricophyte bacteria, has a germicidal effect with continuous sterilization effect, and has a skin-soothing effect. It blocks the production pathway of fungi and dandruff to stop dandruff and prevent itching, Soft and resilient.

In addition, it does not cause precipitation and separation of layers by mixing with various anionic, nonionic and cationic surfactants. It is stable to light and heat without deterioration and hydrolysis at pH 3 ~ 8, low toxicity Belong to the compound.

If the content is less than 2% by weight, the sterilizing effect on the fungus is insufficient. If the content exceeds 10% by weight, the climbazole will precipitate from the propylene glycol solvent and will not irritate the skin. There is a problem that the dispersibility is deteriorated.

In order to further improve the preservative ability of the preservative composition, sodium benzoate may be further added to the preservative composition.

The sodium benzoate is a white crystalline powder which has no odor and is water-soluble more than benzoic acid and neutral or weakly alkaline in aqueous solution. It prevents or delays the growth of various microorganisms such as bacteria, fungi and yeast, Is used.

Sodium benzoate has a broad antibacterial range and exhibits bactericidal action to kill germs under acidic conditions. Since benzoic acid is dissolved in water to exhibit acidity, the preservative composition is acidic so that it is suitable for weakly acidic skin, while sodium benzoate exhibits antibacterial activity do.

The sodium benzoate preferably contains 0.1 to 5.0% by weight of the preservative composition. If the content is less than 0.1% by weight, the antibacterial activity is insufficient and the antibacterial effect is difficult to be maintained for a long time. When the content is more than 5.0% by weight, Etc., and the dispersibility is lowered, making it difficult to obtain a homogeneous composition.

As described above, propylene glycol prevents the deterioration of the preservative strength of benzoic acid and inhibits freezing and recrystallization of cetylpyridinium chloride, and benzoic acid prevents deterioration and hydrolysis of climbazole and improves the bactericidal effect of sodium benzoate.

In this way, propylene glycol, benzoic acid, cetylpyridinium chloride, climbazole and sodium benzoate components can be sterilized and bacteriostatically enhanced through synergistic action of each component even if a small amount is used, so that irritation or skin trouble It is possible to exert the preservative effect without inducing.

The preservative composition preferably exhibits an acidity of pH 3 to 7 in order to be suitable for weakly acidic skin while suppressing freezing and recrystallization of climbazole and improving the bactericidal effect of sodium benzoate.

If the concentration is less than 0.1% by weight, the preservative effect is insufficient. If the concentration is more than 1.0% by weight, the preservative composition may be applied to the skin A stimulation can be given and a sufficient preservative effect can be obtained at a concentration of 1.0% by weight.

The antiseptic composition of the present invention has a high antimicrobial activity and broad spectrum of antimicrobial activity and exhibits rapid efficacy and long-lasting properties. Therefore, the antimicrobial composition of the present invention can be applied to diapers, tissues, wet tissues, cosmetics, detergents, external skin preparations, sanitary products, Water treatment such as microbial control, sterilization and disinfection of cooling towers as well as cooling towers, construction fields such as water-based emulsion paints, solvent-based paints and latex, anticorrosive agents for textile weaving, paper slime control agents, And can be used for more effective and wide-ranging control of microorganisms in various industrial fields, such as a field of fiber papermaking,

Hereinafter, the present invention will be described in more detail with reference to the following examples, comparative examples and test examples.

It is to be understood, however, that the invention is not to be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Will be apparent to those skilled in the art to which the present invention pertains.

≪ Example 1 >

69 kg of propylene glycol was added to a stirring vessel and stirred while heating.

7 kg of climbazole was dissolved in the stirring vessel, and 14 kg of benzoic acid was dissolved therein.

Next, 10 kg of cetylpyridinium chloride was added to the stirring vessel to completely dissolve the mixture to prepare a clear preservative composition, the pH of which was 4.5.

≪ Example 2 >

In Example 1, 1 kg of sodium benzoate was mixed with a solution prepared by mixing propylene glycol, climbazole, benzoic acid, and cetylpyridinium chloride and completely dissolved to prepare a preservative composition.

≪ Comparative Example 1 &

In Example 1, a preservative composition containing only propylene glycol, benzoic acid, and cetylpyridinium chloride was prepared without adding climbazole in the preparation of the preservative composition.

≪ Comparative Example 2 &

In Example 1, an antiseptic composition containing only propylene glycol, climbazole and cetylpyridinium chloride was prepared without adding benzoic acid in the preparation of the preservative composition.

≪ Test Example 1 > Test of sterilizing power of preservative composition

For each of the preservative compositions of Examples 1 and 2 and Comparative Examples 1 and 2, 10 ml of water was added to a test tube and 0.4% by weight of the preservative composition was added thereto to prepare a test solution.

In addition, 10 ml of water was added to a test tube, and Escherichia coli coli ), Staphylococcus aureus ), Pseudomonas aeruginosa ), Candida albicans ( Candida albicans ) and fungus Aspergillus niger were added and cultured to prepare a test mixture.

Immediately after adding 0.1 ml of test mixture to 10 ml of each test solution, the sample was inoculated into TSA (Tryptic soy agar) medium and PDA (Potato dextrose agar) medium and incubated in an incubator at 30 ° C for 24 hours And the initial number of bacteria was measured.

The colony was counted by inoculating the TSA medium and the PDA medium in an incubator at 30 ° C for 24 hours in the same manner as described above after the sample was set for 24 hours. Table 1 shows the results.

The results of the sterilizing power measurement of the preservative composition Example 1 Example 2 Comparative Example 1 Comparative Example 2 Initial number of bacteria TNTC ^{Note 1)} One-day political sample (TSA medium) cfu ^{Note 2)} <10 <10 35 42 Sterility (%) > 99.99 > 99.99 94.2 91.5 One-day political sample (PDA badge) cfu <10 <10 32 39 Sterility (%) > 99.99 > 99.99 94.7 92.1 Note 1) TNTC: Too Numerous To Count
Note 2) cfu: colony forming unit

As shown in Table 1, the initial number of bacteria was observed to be TNTC (about 10 ⁶ to 10 ⁷ cfu) in each group, but when the sample was incubated for one day in a medium after standing for one day, The number of colonies was observed to be less than 10. In Comparative Example 1 in which no climbazole was contained in the preservative composition, the number of microorganisms was 35 (TSA medium) and 32 (PDA medium) The number of colonies (TSA medium) and 39 (PDA medium) were observed, and it was found that the composition could contain 99.99% or more of buoyancy by containing all of propylene glycol, climbazole, benzoic acid and cetylpyridinium chloride components have.

Further, it can be seen that the benzoic acid plays a more important role than the climbazole in the preservative composition of the present invention, as a result of the low repelling force of Comparative Example 2, as compared with Comparative Example 1.

The results of the buoyancy test for Example 2 are shown in FIG. 1, and the initial number of bacteria in the TSA medium and the PDA medium was very high. After the test bacteria were added to the test solution to which the preservative composition was added, Most of them are dead.

&Lt; Test Example 2 > Test for maintaining the sterilizing power of the preservative composition

In Example 1, the preservative composition of Example 2 having excellent sterilizing power was added to the wet tissue to prepare a wet tissue sample containing 0.4% by weight of the preservative composition in the wet tissue.

In addition, 10 ml of water was added to the test tube, and the bacteria Escherichia coli, Staphylococcus aureus, (10 ⁶ to 10 ⁷ cfu) was prepared by adding 10 ml of water to a test tube, adding Candida albicans, which is a lactic acid bacterium, and black germ, which is a fungus, and culturing the mixture.

0.1 ml of each of the bacterial mixed solution and the mixture of fungi was inoculated separately to the wet tissue sample, and the wet tissue sample was cut to an appropriate size to prepare a bacterial specimen and a mold specimen.

The bacterial mixture and the fungal mixture were inoculated into TSA medium and PDA medium in an amount of 0.1 ml, respectively. The bacterial and fungal specimens were placed in each medium and incubated in an incubator at 30 ° C for 24 hours to confirm the initial number of bacteria.

In addition, 0.1 ml of the mixture of the bacterial mixture and the fungus was inoculated again to the specimen (the first inoculation) in which the bacterial specimen and the mold specimen were allowed to stand for 24 hours, the first inoculum specimen was again inoculated, and the specimen ) And the second inoculum were again inoculated with 0.1 ml of each of the bacterial mixture and the fungal mixture, and the test pieces (the third inoculation), which had been allowed to stand for 24 hours, were inoculated into TSA medium and PDA medium and incubated in an incubator at 30 ° C for 24 hours The number of colonies was measured and the results are shown in Table 2 below.

The result of the measurement of the sterilizing power of the wet tissue containing the preservative composition Initial number of bacteria First inoculation
Psalter Second inoculation
Psalter 3 doses
Psalter Bacterial mixture TSA badge
(cfu ^{note 1} ) TNTC ^{Note 2)} Nd ^{Note 3)} - - Mold mixture TSA badge
(cfu) Nd Nd Nd PDA badge
(cfu) Nd Nd Nd Note 1) cfu: colony forming unit
Note 2) TNTC: Too Numerous To Count
Note 3) Nd: not detected

As can be seen from Table 2 above, the microbial growth test in the wet tissue containing 0.4 wt.% Of the preservative composition of Example 2 resulted in the death of bacteria and molds in both primary, secondary and tertiary inoculations , And that the preservative force of the preservative composition according to the present invention is maintained at a certain level or more over time.

FIG. 2 shows the result of the test for maintaining the sterility of the mold against Test Example 2. The initial number of bacteria in the TSA medium and the PDA medium was very high, but all of the molds died after 24 hours from the first and the third inoculation have.

Test Example 3 Parallel streak test of preservative composition

The preservative composition of Example 2 was added to the wet tissue so that the preservative composition contained 0.4 wt% of the wet tissue, and then cut into strips to prepare a wet tissue specimen.

The bacterial mixture of Test Example 2 was plated three times in TSA medium at intervals of 10 mm to a length of 60 mm. In the same manner, the fungus mixture of Test Example 2 was inoculated into the PDA medium.

The above wet tissue specimen was gently placed on each surface of the medium to be inoculated, and gently pressed with a sterilizing rod, followed by incubation in an incubator at 30 ° C to observe microorganism death.

FIG. 3 shows the appearance of the culture medium after 24 hours of inoculation. In the TSA medium inoculated with the bacterial mixed solution, no microbial low zone was formed, but the microbial low zone was not proliferated in the wet tissue specimen. In the PDA medium inoculated with the fungal mixture, And thus the preservative force of the preservative composition according to the present invention can be confirmed.

&Lt; Test Example 4 > Skin irritation test

20 persons without skin disease were subjected to a patch test of the preservative compositions prepared in Examples 1 and 2 and Comparative Examples 1 and 2, and the results are shown in Table 3 below.

Water was mixed with each of the above-mentioned preservative compositions to prepare an aqueous solution of 0.4% by weight. Then, 15 ㎕ of each solution was dropped onto Finn Chamber (SmartPractice Co., USA) having a diameter of 8 mm on the Scanpor tape.

The inner part of the upper left part of the subject was wiped with 70% ethanol and dried. Then, the prepared Finn chambers were sealed and attached for 24 hours. Then, the patches were removed and marking areas were marked with a marking pen. After 48 hours, the test site was observed.

According to the criteria of the International Contact Dermatitis Research Group (ICDRG), the degree of skin irritation was classified, and the mean score was calculated according to the average skin response calculation formula. Respectively.

Skin Info Test Results Reactivity ^{Note 1 )} (persons) Mean score ^{Note 2) Note 3 )} - ± ++++ ++ +++ Example 1 30 minutes 19 One 0 0 0 0.28 No stimulation 24 hours 20 0 0 0 0 48 hours 20 0 0 0 0 Example 2 30 minutes 18 2 0 0 0 0.56 No stimulation 24 hours 20 0 0 0 0 48 hours 20 0 0 0 0 Comparative Example 1 30 minutes 18 2 0 0 0 0.56 No stimulation 24 hours 20 0 0 0 0 48 hours 20 0 0 0 0 Comparative Example 2 30 minutes 19 One 0 0 0 0.28 No stimulation 24 hours 20 0 0 0 0 48 hours 20 0 0 0 0 (Score: 0), ±: irritation (uncertain or mild reaction and erythema) (score: 0.5), +: light stimulus (weak erythema, (Score: 2), +++: severe irritation (severe erythema, hardening and algebra) (score: 3)
(+ Score × number of subjects) + (+ score × number of subjects) + (+ score × number of subjects) + (++ score × number of subjects) Number of subjects to be examined)} / (maximum stimulus value x total number of subjects x evaluation number) x 100
Note 3) Judgment: 0.00 to 0.75 (no irritation), 0.76 to 1.50 (irritation), 1.51 to 2.50 (irritation), 2.51 to 4.00 (irritation)

As shown in Table 3, the mean scores of Examples and Comparative Examples were determined to be 0.28 and 0.56, respectively, as non-stimulated, and it can be seen that the respective components of the composition according to the present invention are composed of ingredients that do not irritate the skin .

As described above, the preservative composition of the present invention exhibits excellent antimicrobial effect against various microorganisms such as bacteria, yeast, fungi,

In addition, it can be safely used on the skin of the human body, composed of harmless ingredients that are safe to the skin and low in stimulus, and can safely protect the skin exposed to the outside from the surrounding harmful environment.

Claims (7)

Propyleneglycol, benzoic acid, cetylpyridinium chloride, and climbazole. The method according to claim 1,
Wherein the preservative composition comprises from 65 to 80% by weight of propylene glycol, from 1 to 20% by weight of benzoic acid, from 3 to 20% by weight of cetylpyridinium chloride and from 2 to 10% by weight of climbazole. The method according to claim 1,
Wherein the preservative composition further comprises sodium benzoate. The method of claim 3,
Wherein the sodium benzoate comprises from 0.1 to 5.0% by weight of the antiseptic composition. The method according to claim 1,
Wherein the preservative composition has a pH of 3-7. The method according to claim 1,
Wherein the preservative composition is an aqueous solution at a concentration of 0.1 to 1.0 wt%. 6. A composition containing the preservative composition according to any one of claims 1 to 6 for the preparation of a diaper, a tissue, a wet tissue, a cosmetic, a detergent, a skin external preparation, a sanitary article, a sanitary article, a disinfectant, a mouthwash, a shampoo, Leather product additive or fiber additive.

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