KR102202917B1 - Compositions for sterilization and disinfection and the manufacturing method thereof - Google Patents

Abstract

The present invention relates to a disinfection composition with a sterilization effect and a manufacturing method thereof and relates to a disinfection composition for a medical device and skin that does not cause skin irritation and unpleasant odors, has the excellent cleaning power of the blood that is not easily decomposed, and has a low risk of corrosion of easily corroded medical devices. More specifically, the disinfection composition with a sterilization effect consists of 1.8 to 3.3 wt% of alkyldimethylbenzylammonium chloride, 1.8 to 3.3 wt% of didecyldimethylammonium chloride, 1.3 to 1.7 wt% of sodium edetate hydrate, 1.2 to 1.6 wt% of cocodimethylamine oxide, 0.4 to 0.8 wt% of sodium hydroxide, 0.001 to 0.003 wt% of a colorant, and the remainder of purified water and mixes them so that the mass ratio of the content of the alkyldimethylbenzylammonium chloride and the content of didecyldimethylammonium chloride (alkyldimethylbenzylammonium chloride/ didecyldimethylammonium chloride) is 0.7 to 1.5.

Description

Compositions for sterilization and disinfection and the manufacturing method thereof

The present invention relates to a disinfectant composition having a sterilizing effect and a method of manufacturing the same, and more particularly, it does not cause skin irritation and unpleasant odor, has excellent cleaning power of blood that is difficult to be easily decomposed, and there is a risk of corrosion of medical devices that are easily corroded It relates to a small medical device and a composition for skin disinfection and a method of manufacturing the same.

In order to safely reprocess used medical devices such as various medical devices, laryngoscope blades, breathing circuits, suction bottles, scalpels, scissors, etc., remove all biological contaminants such as blood, fat, tissue fragments, etc. from medical devices before sterilization or disinfection treatment. It is desirable to remove. Disinfection and cleaning of contaminated medical devices is a very important procedure because if any residual contaminants remain on the used medical devices, the next visited patient can be infected in the hospital.

In addition, in the case of blood, once it comes into contact with medical devices and skin, it may remain without being thoroughly cleaned even after washing with running water or detergent, so disinfectants and detergents that can completely clean contaminated blood are required.

In addition, in the case of medical devices that are reused several times through cleaning and sterilization with at least the 2nd~3rd procedure, corrosion reactions can easily occur, so there may be a possibility of infection during patient surgery with invisible dissolved metal ions. . Accordingly, there is a need to develop a disinfectant and detergent capable of preventing a corrosion reaction of medical devices.

Conventionally, hand sanitizers are widely used disinfectants using ethanol, isopropyl alcohol, octenidine, phosphoric acid, propylene glycol, etc., and these components destroy the cell membrane of bacteria, the envelope of viruses, and coagulation of proteins such as enzymes. It is known to have a disinfecting action against. However, when disinfecting with a disinfectant containing these ingredients, it irritates the user's skin, removing each layer and sebaceous film, falling off each layer, and may cause loss of skin barrier function. There may be a possibility of infection by invading the virus.

Accordingly, the present inventors have invented a disinfectant composition having excellent antibacterial and sterilizing power without causing irritation and unpleasant odor to the skin, having excellent blood cleaning power, low risk of corrosion of medical devices.

Korean Patent Application Publication No. 10-2019-0126135 (November 08, 2019)

The present invention was invented to solve the above problems and is to produce a composition for disinfecting skin without skin irritation and unpleasant odor by minimizing chemical components that are harmful to humans.

In addition, the present invention is to prepare a disinfectant composition suitable for disinfection and cleaning of medical devices for preventing cross-infection in a hospital because it has excellent decomposition power against organic contaminants in order to completely clean blood that is difficult to decompose.

In addition, the present invention is to prepare a composition for disinfecting medical devices with a low risk of corrosion of devices during disinfection for immersion of medical devices.

In the present invention, the disinfecting composition having the sterilizing effect in order to achieve the above object is 1.8 to 3.3% by weight of alkyldimethylbenzylammonium chloride, 1.8 to 3.3% by weight of didecyldimethylammonium chloride, 1.3 to 1.7% by weight of sodium edetate hydrate %, cocodimethylamine oxide 1.2 to 1.6% by weight, sodium hydroxide 0.4 to 0.8% by weight, colorant 0.001 to 0.003% by weight, and the remaining amount of purified water, wherein the content of the alkyldimethylbenzylammonium chloride content and the didecyldimethylammonium chloride content A disinfectant composition having a sterilizing effect is prepared by mixing so that the mass ratio (alkyldimethylbenzyl ammonium chloride/didecyldimethylammonium chloride) is 0.7 to 1.5.

More specifically, the pH of the disinfecting composition may be 6 to 8.

In addition, the present invention relates to a method for producing a disinfecting composition having a sterilizing effect.

The method for preparing a disinfecting composition having the sterilizing effect includes the steps of (a) preparing a first composition by mixing 35 to 45% by weight of purified water and 1.8 to 3.3% by weight of alkyldimethylbenzylammonium chloride, (b) the preparation Preparing a second composition by mixing 1.3 to 1.7% by weight of sodium edetate hydrate in the first composition, (c) 1.8 to 3.3% by weight of didecyldimethylammonium chloride and cocodimethylamine oxide in 15 to 25% by weight of purified water Preparing a third composition by mixing 1.2 to 1.6% by weight, (d) mixing the prepared second composition and the prepared third composition, and mixing 0.001 to 0.003% by weight of a colorant to prepare a fourth composition Step, (e) 0.4 to 0.8% by weight of sodium hydroxide and the remaining amount of purified water are added to the prepared fourth composition so that the total composition is 100% by weight and the pH is adjusted to 6 to 8 to prepare a disinfecting composition.

More specifically, the method for preparing a disinfecting composition having a sterilizing effect includes (a) adding 35 to 45% by weight of purified water to a warming stirrer and stirring at a speed of 30 rpm while adding 1.8 to 3.3% by weight of alkyldimethylbenzylammonium chloride. The step of preparing a first composition by adding and reacting for 10 to 20 minutes, (b) adding 1.3 to 1.7 wt% of sodium edetate hydrate to the prepared first composition and reacting at a rate of 20 rpm for 5 to 10 minutes to prepare a second composition (C) 1.8 to 3.3% by weight of didecyldimethylammonium chloride and 1.2 to 1.6% by weight of cocodimethylamine oxide are added to 15 to 25% by weight of purified water at a temperature of 40°C, and reacted for 25 to 35 minutes at a speed of 50 rpm. After cooling to room temperature to prepare a third composition, (d) mixing the prepared second composition and the prepared third composition, adding 0.001 to 0.003% by weight of a colorant, and stirring at a speed of 40 rpm to prepare a fourth composition In the step of preparing (e) sodium hydroxide 0.4 to 0.8% by weight and the remaining amount of purified water were added to the prepared fourth composition so that the total composition was 100% by weight, stirred for 15 to 20 minutes at 50 rpm, and the pH was 6 to By adjusting to be 8, a disinfecting composition is prepared.

The disinfectant composition of the present invention has the effect of significantly lowering skin irritation and unpleasant odor by minimizing chemical components that are harmful to humans.

In addition, the present invention has excellent decomposition power for organic contaminants in order to completely clean blood that is difficult to decompose, and thus has an effect suitable for disinfection and cleaning of medical devices for preventing cross-infection in hospitals.

In addition, the present invention has a safety effect with less damage such as secondary infection because there is less risk of corrosion of the device during disinfection for immersion of medical devices.

1 is a summary result of bactericidal and fungal sterilization test results of the disinfecting composition of the present invention.
2 is a test report of virus sterilization ability of the disinfecting composition of the present invention.
3 is a detailed result of a virus sterilization test of the disinfecting composition of the present invention.

Hereinafter, the disinfecting composition having a sterilizing effect according to the present invention and a method of manufacturing the same will become apparent with reference to the examples described below in detail. However, the present invention is not limited to the embodiments disclosed below, and may be implemented in various different forms, and is provided to completely inform the scope of the invention to those of ordinary skill in the technical field to which the present invention belongs. It becomes. In addition, the present invention should be construed as including all embodiments falling within the scope of the appended claims.

The first step for preparing the disinfecting composition of the present invention is a step of preparing a first composition by mixing purified water and alkyldimethylbenzyl ammonium chloride.

More specifically, in the first composition, 35 to 45% by weight of purified water is added to a warming stirrer, 1.8 to 3.3% by weight of alkyldimethylbenzyl ammonium chloride is added while stirring at 30 rpm, and reacted for 10 to 20 minutes. The composition may be prepared, and it may be more preferable to add 2.2 to 3.3% by weight of alkyldimethylbenzyl ammonium chloride in order to maximize the sterilizing power, blood cleaning power, and mechanism corrosion preventing ability of the disinfecting composition according to the present invention.

Alkyldimethylbenzylammonium chloride (Benzalkonium chloride) is a nitrogen cationic surfactant belonging to the quaternary ammonium salt, and it has the effect of sterilizing by destroying cell membranes or inhibiting the synthesis of cell membranes. It has the advantage of being less safe. It is well soluble in ethanol and acetone and is not soluble in water, but the aqueous solution is easy to handle, so the aqueous solution is preferred. The pH of the solution is 6.5~8, and the color is colorless or pale yellow. When the solution is shaken, a lot of bubbles appear and it tastes bitter.

The next step of preparing the first composition is a step of preparing a second composition by adding sodium edetate hydrate to the prepared first composition.

In more detail, 1.3 to 1.7 wt% of sodium edetate hydrate may be added to the prepared first composition and reacted at 20 rpm for 5 to 10 minutes to prepare a second composition, and the sterilizing power of the disinfecting composition according to the present invention , It may be more preferable to add 1.4 to 1.6% by weight of sodium edetate hydrate in order to maximize the ability to clean blood and prevent device corrosion.

The sodium edetate hydrate (Ethylenediaminetetraacetic acid, C ₁₀ H ₁₆ N ₂ O ₈ ) is used as a chelating agent and is also used to remove metal ions in water, and because it has a strong affinity with Pb2+ ions, it is a treatment for lead poisoning. It has also been used as. The complex of iron ions is used to supply iron components to plants, and it can prevent edible oil from rotting by removing metal ions, which are catalysts for oxidation reactions present in edible oil, and also used as an anticoagulant of blood, a component of a buffer solution In analytical chemistry, it is mainly used for analysis, separation, and removal of metal ions.

The next step of preparing the second composition is a step of preparing a third composition by adding and mixing didecyldimethylammonium chloride and cocodimethylamine oxide to purified water.

More specifically, 1.8 to 3.3% by weight of didecyldimethylammonium chloride and 1.2 to 1.6% by weight of cocodimethylamine oxide were added to 15 to 25% by weight of purified water at a temperature of 40°C, followed by reaction at 50 rpm for 25 to 35 minutes, and then to room temperature. A third composition can be prepared by cooling, and 2.2 to 3.3% by weight of didecyldimethylammonium chloride and 1.3 to 1.5% by weight of the disinfectant composition according to the present invention maximize the sterilizing power, blood cleaning power, and device corrosion prevention ability. It may be more desirable to add cocodimethylamine oxide.

In addition, it may be preferable to add so that the mass ratio of the content of the alkyldimethylbenzylammonium chloride and the content of didecyldimethylammonium chloride (alkyldimethylbenzylammonium chloride/didecyldimethylammonium chloride) is 0.7 to 1.5, and disinfection according to the present invention In order to maximize the sterilization power, blood cleaning power, and mechanism corrosion prevention ability of the solvent composition, the mass ratio of the content of the alkyldimethylbenzyl ammonium chloride and the content of didecyldimethylammonium chloride (alkyldimethylbenzyl ammonium chloride / didecyldimethylammonium chloride) is 0.9 to 1.5 It may be more preferable to add so as to be.

Didecyldimethylammonium chloride was used as a surfactant, and is often used as a preservative. Didecyldimethylammonium chloride causes disruption of intermolecular interactions and dissociation of lipid bilayers, and can be used as a broad spectrum disinfectant and disinfectant, disinfectant for linen, and is recommended for use in hospitals, hotels and industries. It is also used in obstetrics and gynecology, surgery, ophthalmology, pediatrics, OT, and surgical tools and endoscopy and surface sterilization.

The cocodimethylamine oxide (C ₁₄ H ₃₁ NO: 229.40) was used as a surfactant, with a pale yellow color of about 7.5pH (5w/v% aqueous solution), a specific gravity of about 0.97, a boiling point of about 100°C and a refractive index (N20/ D) It is a liquid between 1.376-1.380. Like other amine oxide surfactants, it has an effective antibacterial effect against common bacteria, and can be used to dissolve Staphylococcus aureus and Escherichia coli, and non-denaturing proteins.

In the step of preparing the third composition, in order to further maximize the anticorrosive effect of the disinfecting composition according to the present invention, a process of further adding and mixing the fruit extract of carob may be additionally performed.

More specifically, it may be prepared by adding 0.9 to 2.1 parts by weight of the carob fruit extract to the prepared third composition, and it may be more preferable to add 1.3 to 1.9 parts by weight of the carob fruit extract to maximize the anti-corrosion effect. have.

The scientific name of carob is Ceratonia siligua, and it is a species of shrub or tree belonging to the evergreen plant and is classified as legume. It is called Kerup Tree, Kerup Bean, and Red Bean Tree. Karov Native to southern Europe, North Africa, the Mediterranean Islands, the Levant, and the Middle East of Western Asia to Iran, the Canary Islands and Macaronesia, it grows up to 15 meters (49 feet). The leaves are 10-20 centimeters (3.9-7.9 inches) long, and male trees do not bear fruit. Although carob is widely used in agriculture, it can also be seen growing in the wilderness of the eastern Mediterranean, and it occurs naturally in the west. Carob fruit extract is known to act as an anti-corrosion effect by adsorbing the extract on the southern surface to create a barrier for material and charge transfer.

The carob fruit can be extracted by methods such as ethanol, hot water, or carbon dioxide supercritical extraction method, and extraction by carbon dioxide supercritical extraction method maximizes the effect of preventing corrosion of medical devices without lowering the sterilizing power of the disinfecting composition of the present invention. It can be made to be desirable. The method of extracting using the carbon dioxide supercritical is to extract carbon dioxide using supercritical carbon dioxide by introducing carbon dioxide for 20 to 35 minutes at a pressure of 250 to 310 bar and a temperature of 35 to 45°C after pulverizing the carob fruit. In order to maximize the disinfecting effect of the disinfecting composition according to the present invention to be prepared, and to maximize the disinfecting effect of the disinfecting composition according to the present invention, carbon dioxide is introduced into the neem tree seeds at a pressure of 280 to 300 bar and a temperature of 38 to 42°C for 25 to 29 minutes. It may be more preferable to extract and manufacture using supercritical carbon dioxide.

The next step of preparing the third composition is a step of preparing a fourth composition by mixing the prepared second composition and the prepared third composition and adding a colorant.

More specifically, a fourth composition may be prepared by mixing the prepared second composition and the prepared third composition, adding 0.001 to 0.003% by weight of a colorant, and stirring at a speed of 40 rpm, and the colorant is 0.0015 to 0.0025 wt. It may be more desirable to add %.

In the embodiment of the present invention, red No. 102 was used, but various colorants may be used according to the use, but the colorant is not limited thereto.

The next step of preparing the fourth composition is a step of preparing a disinfecting composition by adding sodium hydroxide and purified water to the prepared fourth composition to adjust the pH.

More specifically, in the prepared fourth composition, 0.4 to 0.8% by weight of sodium hydroxide and the remaining amount of purified water were added to make the total composition 100% by weight, stirred at 50 rpm for 15 to 20 minutes, and the pH was adjusted to be 6 to 8. In order to minimize skin irritation of the disinfectant composition of the present invention, it may be more preferable to adjust the pH to a neutral pH. The higher the pH of the alkyldimethylbenzyl ammonium chloride, the stronger the sterilizing power, but since the skin irritation becomes stronger, it may be preferable to prepare it in a neutral region of pH 8 or less.

The sodium hydroxide was used as a pH stabilizer. Sodium hydroxide (NaOH) is dissolved in water to make a strong basic aqueous solution. It is widely used in industries such as textiles, food and beverages, and soap, and is the most widely used base in chemical experiments, and is commonly referred to as caustic soda in the industry. Pure hydroxide. It absorbs water vapor and carbon dioxide from the atmosphere well and dissolves well in water regardless of temperature, and a lot of heat is generated at this time.

The disinfectant composition of the present invention may be preferably diluted with a 1% solution (1:100) when disinfecting and washing the skin, and does not need to be washed separately with water.

When disinfecting and cleaning medical devices, it can be immersed in a 1% solution (1:100 diluted solution) for 4 to 6 minutes and used as it is. When sterilized, the medical devices sterilized and washed with the disinfectant composition of the present invention are rinsed with water and It may be desirable to disinfect and sterilize by autoclaving at 137°C for at least 1 minute.

The disinfectant composition of the present invention can be used for disinfection and cleaning of medical devices and for disinfection and cleaning of the skin, and the medical devices include a Laryngoscope blade, a breathing circuit, a suction bottle, an oxygen container, an artificial respirator, a newborn baby room incubator, and a medical device ( Medical equipment), endoscopy equipment, dental equipment (jabari tube, silicone tube, vinyl tube, silicone cap, silicone stopper, mass, endoscope oil), dental equipment, as a primary disinfectant for medical equipment used in wards, operating rooms, intensive care units, etc. Can be used.

Hereinafter, the disinfecting composition of the present invention will be described in detail by the following test examples and preparation examples.

<Test Example 1> General strain and virus bactericidal power test

1) Preparation of test bacteria solution

Test strains grown on SABLP medium Pseudomonas aeruginosa NCTC 6749, Staphylococcus epidermidis NCTC 11047, Salmonella enteritidis NCTC 4444, Salmonella typhimurium NCTC 5710, Klebsiella pneumoniae ATCC 4352, Enterococcus hirae ATCC10541, Salmonella cholera 053, NCTC 157, NCtc 11994, Proteus vulgaris NCIMB 4175, Campylobacter jejuni NCTC 11951, Corynebacterium bovis NCTC 3224, Serratia marcescens NCTC 10211, Rhodococcus equi NCTC 1621, Candida albicans ATCC 10231, Clostridium difficile (spores) NCTC 11209, Bacillus subtilis IP It was collected with platinum, and a bacterial liquid was prepared with distilled water. This was used as a test bacterial solution.

Virus activation (CPE/MTT titer measurement) was measured using Simian Rotavirus using MA104 cell line at room temperature for 1 minute and 5 minutes at room temperature for 1 minute and 5 minutes. According to the procedure, the virus sterilizing power of the disinfecting composition of the present invention was measured.

2) Measurement of initial viable cell count

150 µL of the test bacteria solution was added to 3 mL of distilled water and mixed well. Immediately, 0.5 mL of this bacterial mixture was added to 4.5 mL of a neutralizing agent and mixed well. This was diluted 50 times, 100 times, and 200 times. 1 mL of the diluted solution was dispensed into the dish, and about 15 mL of the SABLP medium stored in the warm bath was added to prepare a mixed stone plate. After the mixed stone plate was solidified, it was inverted and aerobic cultured at 35±2° C. for 2 days. Colonies grown on the mixed stone plate were visually counted. This operation was carried out 3 times.

3) Measurement of the number of viable cells after the action of the test substance

Example 6 150 µL of the test bacteria solution was added to 3 mL and mixed well. This was taken as a reaction solution. The reaction was carried out at room temperature (23.0±3.0°C). After 30 seconds and 60 seconds, 0.5 mL of the reaction solution was added to 4.5 mL of a neutralizing agent and mixed well. This was made into a 50-fold, 100-fold, and 200-fold diluted solution. 1 mL of the diluted solution was dispensed into the dish, and about 15 mL of the SABLP medium stored in the warm bath was added to prepare a mixed stone plate. After the mixed stone plate solidified, it was inverted and aerobic cultured at 35±2° C. for 2 days. Colonies grown on the mixed stone plate were visually counted. This operation was carried out 3 times.

4) Calculation of Log Reduction

The commercial logarithmic value of the initial viable cell count (CFU/mL) and the average value were calculated. From this average value and the average value of the logarithmic value of the number of bacteria (CFU/mL) after the action of the test substance at each action time, Log Reduction was calculated by the following equation.

Log Reduction=B-C

B: Average value of initial viable cell count (common logarithmic value)

C: Average value of the number of viable cells (common logarithmic value) after the action of each test substance

5) result

As shown in FIGS. 1 to 3, it was found that the disinfecting composition of the present invention (NewGen High-level disinfectant) was excellent in disinfecting effect on all of the tested viruses, bacteria, and fungi.

<Test Example 2> MRAb, VRE, NTM (M. bovis) strain disinfection test

Mycobacteria are resistant to antibiotics and disinfectants due to the high proportion of fat in the cell wall, so it is difficult to prevent bacteria and experimental methods and data are also insufficient. In particular, Mycobacterium tuberculosis mainly causes lung disease, leading to death, and treatment is difficult and takes a long time, and several antibiotics are administered. It is estimated that one third of the world's population is infected with Mycobacterium tuberculosis, acting as a risk factor worldwide. In 2006, the WHO announced the eradication project and is carrying out the project, and Korea also has the highest infection rate among OECD countries, so research is needed to eradicate tuberculosis. Since M. tuberculosis is highly pathogenic, it is similar to M. tuberculosis, has little pathogenicity to the human body, grows relatively quickly, and uses M.bovis, which is usefully used as an alternative strain of M. tuberculosis in many experiments, to disinfect the composition of the present invention. Was conducted an experiment on

2-1. Strain and medium

1) Multi-drug resistant Acinetobacter baumannii (MRAb)

A. baumannii (R-Ab) standard strain was A. baumannii (ATCC 19606) sold by ATCC, and MRAb strain was clinically isolated. Compared to the standard strain, Cefepime, Imipenem, Ticarcillin/Clavulanic acid, As a strain resistant to Tetracycline and Colistin, it was confirmed that it is resistant to Aminoglycosides, Penicillin, Monobactam, Cephalosporin, Quinolone, Carbapenem, T-lactamase, and Tetracycline [Table 1, Comparison of antimicrobial susceptibility between Reference

Acinetobacter baumannii and Multi-drug resistant Acinetobacter baumannii]. Tryptic soy agar (TSA) and Tryptic soy broth (TSB) were used as culture media, and cultured in an incubator at 37°C for 18 hours.

2) Vancomycin resistant Enterococcus spp (VRE)

Enterococcus faecium (ATCC 19434) sold by ATCC as Reference Enterococcus faecium (R-Ef) was used, and as a VRE strain, it is a clinically isolated strain. Van A phenotype was confirmed as a strain, and as a result of gene analysis, it was confirmed that vanA gene was expressed [Table 2, Comparison of antimicrobial susceptibility between VREnterococcus spp and Reference Enterococcus spp]. Tryptic soy agar (TSA) and Tryptic soy broth (TSB) were used as culture media, and cultured in an incubator at 37°C for 18 hours.

3) NTM (Mycobacterium bovis)

The experiment was performed using the attenuated strain Mycobacterium bovis (M.bovis) used for BCG as the NTM strain. M.bovis culture medium was cultured using Middle brook 7H10 agar and Middle brook 7H9 broth, and cultured in an incubator at 37°C for 1 week.

2-3. Experiment method

1) Minimum inhibitory concentration (MIC, minimum inhibitory concentration)

One colony of strain cultured in TSA was inoculated into 5 ml of TSB and cultured for 18 hours in an incubator at 37°C. After incubation, the absorbance was measured at 600 nm, and the number of bacteria was diluted to 0.132 nm, which is 0.5 X 108 cfu/ml absorbance. Dilute the experimental detergent 10 times in a 96-well microplate and dispense 100 μl each. Dispense the diluted bacterial solution in an equal amount and incubate for 18 hours in a 37°C incubator. At this time, the negative control is distilled water. After incubation, 100-fold serial dilution is applied to TSA, followed by incubation at 37°C for 24 hours. Check the Log10 reduction rate.

2) Time kill test (TKT)-American Society for Testing and Materials (ASTM) E2315

Disinfectant composition Example 6 After injecting an equal amount of 0.5 X 103 cfu/ml bacteria into 1 ml, reacting immediately and for 15, 30, and 60 seconds, then diluting and dispensing 100 μl in agar, smearing, and counting colony to measure antibacterial activity The amount of viable test bacteria was measured at each contact time, and the lethal concentration (%) of the test bacteria was calculated for each contact time.

3) Suspension test AOAC Use-dilution method

0.1 ml of 0.5 x 108 cfu/ml of bacterial solution was reacted with 0.9 ml of detergent. Control group uses distilled water instead of detergent. After reacting for 1 min, 0.1 ml of the reaction solution was serially diluted 100 times, applied to TSA, and incubated at 37°C for 24 hours. In case of tuberculosis bacteria, incubate for 7 days. Check the minimum 3 log CFU reduction rate.

4) Carrier test-Association of Official Analytical Chemists (AOAC) Use-dilution method

Cut 0.75mm thick stainless steel sheet, latex, glass, and fabric into 1 cm horizontally and vertically, and put them in a plate. Add 20 μl of 0.5×108 cfu/ml bacteria solution and air dry for 2 hours. Apply 20 μl of detergent to the contaminated area and react for 1 min. Add saline to the control group and react. Add 980 μl of saline and dilute. The collected samples are diluted 10 times, applied to TSA, and incubated at 37°C for 24 hours. In case of tuberculosis bacteria, incubate for 7 days. Check the minimum 3 log CFU reduction rate.

5) Disinfection composition efficacy test (based on the Ministry of Agriculture, Forestry and Fisheries Quarantine and Inspection), EN 1276

Bacteria should be planted in a medium and cultured for 22 to 26 hours (7 days for Mycobacterium tuberculosis) in which vitality is recognized, but the concentration of bacteria used should be at least 108 per ml. Disinfectant composition Example 6 dissolves 123% of the corresponding concentration of the product to 100 ml with distilled water, hard water, and organic matter, and then puts the diluted 2.5 ml stepwise into 5 test tubes with a difference in concentration of 10%. At this time, the desired dilution concentration is placed in the middle of the five test tubes, and the test tube, in which the disinfectant composition Example 6 diluent treatment is completed, is set to 4°C. After mixing 4ml of bacteria at 37℃ with distilled water, hard water and 96ml of organic diluent at 4℃, take out 2.5ml of the mixed solution, put it in a test tube stored at 4℃, mix, and react at 4℃ for exactly 30 minutes. At this time, each test tube treatment is carried out in turn at an interval of 1 minute, and mixed every 10 minutes on the way. After exactly 30 minutes of reaction, in order to neutralize the efficacy of the disinfecting composition, immediately take out 1.0 ml, put it in 9.0 ml neutralization medium at 37°C, and mix, and then disinfecting composition Example 6 After mixing in a test tube containing nutrient medium, grow in a constant temperature room at 37℃ for 48 hours. The final disinfection and dilution step in which no more than two growths are recognized in the nutrient medium of the same dilution factor of the five disinfectant compositions is used as the dilution factor. Hard water means that 1 liter of distilled water contains 0.305 g of CaCl2 and 0.139 g (w/v) of MgCl2.·6H2O, and the organic matter diluent means hard water containing organic matter used for dilution of the disinfectant composition. , Dissolve in hard water to contain 20% (w/v) of yeast extract, then autoclave (121℃ for 15 minutes) and store at 4℃. When using, dilute 4 times with hard water to make a 5% diluent of organic matter, 1N It was adjusted to pH 7.0 with sodium hydroxide solution. Drug ingredient neutralization medium refers to a medium containing 5% horse serum that has been unassisted (treated at 56°C for 30 minutes) in a nutrient medium. It is carried out under three conditions of distilled water dilution solution, hard water dilution solution, and organic matter dilution solution. Treatment groups-2 and -3 are compared with treatment group-4, and treatment group-1 is treated as follows. [Table 3, Composition for disinfection Treatment at the time of designing the efficacy test]

2-4. Test result

2-4-1. Minimum inhibitory concentration (MIC, minimum inhibitory concentration)

1) MRAb

As a result of treating the standard strains A. baumannii (R-Ab) and Multi-drug resistant A. baumannii (MRAb) by concentration in the disinfecting composition of the present invention, R-Ab did not grow from 0.1% concentration, and was 0.0001% At, bacterial growth was observed, and there was no significant difference in log10 values in 0, 0.0001, and 0.001% treatment groups, respectively, as log9.0, log8.8, and log8.3, but the values decreased with concentration. In the case of MRAb, at a concentration of 0.5% or more, the growth of bacteria was not observed, and at 0.1%, the microbial growth was log0.3, and at 0.01%, the microbial growth was log1.3. Compared to R-Ab, MRAb showed higher resistance to the disinfecting composition. There was little difference in log10 values of the 0, 0.001, and 0.0001% MRAb treatment groups [Table 4, Minimum inhibitory concentration of Disinfectant].

2) VRE

As a result of treating the standard strains Enterococcus faecium (R-Ef) and vancomycin resistant Enterococcus faecium (VRE) by concentration in the disinfecting composition of the present invention, at the concentration of 0.1% or more of the disinfecting composition, both bacteria do not grow and grow more than log 8 bacteria. It showed an inhibitory effect. At a concentration of less than 0.001%, the bacterial growth inhibitory effect was not shown when compared to the untreated group. At a concentration of 0.01%, the standard strain was log 6.3 and VRE was log 5.8. Compared to the untreated group, log 2.8 and log 2.4 were inhibited. The effect appeared. That is, at the recommended concentrations of 1% and 2% of the disinfectant composition, it was confirmed that there was a proliferation inhibitory effect of log 8 or more, and the efficacy as a disinfecting composition was excellent [Table 5, Minimum inhibitory concentration of Disinfectant].

3) NTM (M. bovis)

As a result of treating the disinfecting composition of the present invention in M.bovis by concentration, growth of bacteria was not observed from 0.0001%. At 0.00001%, the growth of bacteria was similar to that of NC, but the growth of bacteria was lower than that of NC. [Table 6] [Table 6] [Table 6, Minimum inhibitory concentration of Disinfectant].

2-4-2. Time kill test (TKT)

-American Society for Testing and Materials (ASTM) E2315

1) MRAb

As a result of reacting 0, 0.5, 1, 2, 10% of the disinfecting composition of the present invention to the experimental strain for 0, 15, 30, 60, 300, 600 seconds, both strains reacted at a concentration of 0.5% or more of the disinfecting composition It showed 100% antibacterial activity from 0 seconds immediately [Table 7, The result of Time kill test of Disinfectant].

2) VRE

As a result of diluting the disinfecting composition of the present invention at various concentrations (0, 0.5, 1, 2, 10% disinfecting composition) and reacting to the experimental strain for 0, 15, 30, 60, 300, 600 seconds, both strains At a concentration of 0.5% or more of the disinfectant composition, it exhibited 100% sterilization effect from 0 seconds immediately to the reaction completion time to 600 seconds [Table 8, The result of Time kill test (TKT) of Disinfectant]. That is, it showed a sterilization effect of log 8 or more.

3) NTM (M. bovis)

As a result of confirming the survival of the bacteria by treating the disinfecting composition of the present invention at intervals of 0, 1, 10, 30, and 60 minutes, unlike the above other bacteria, the antibacterial effect was not confirmed immediately after treatment, but the growth of the bacteria after 1 minute This was not confirmed. In addition, it was confirmed that the efficacy continued up to the maximum time of the experiment, 60 minutes. There was no difference between 1% and 2%, and even 1% showed a sufficient antibacterial effect of 100% [Table 9, The result of Time kill test (TKT) of Disinfectant].

3. Suspension test AOAC Use-dilution method

1) MRAb

As a result of reacting 1, 2% of the disinfecting composition of the present invention to the experimental strain for 0, 1, 5, and 10 minutes, both strains showed 100% antibacterial activity from 0 seconds immediately after the reaction, and even if reacted for 10 minutes Antimicrobial was maintained continuously [Table 10, The result of Suspension test of Disinfectant].

2) VRE

As a result of diluting the disinfecting composition of the present invention at the recommended dilution concentrations of 1 and 2% of the disinfecting composition and reacting to the VRE test strain for 0, 1, 5, 10 minutes, both strains reacted immediately from 0 seconds to 10 minutes. It showed 100% antibacterial activity until [Table 11, The result of Suspension test of Disinfectant]. That is, the disinfectant composition exhibited an antimicrobial activity of log 8 or more at 1 and 2% dilution concentrations.

3) NTM (M. bovis)

As a result of confirming the survival of the bacteria by treating the disinfecting composition of the present invention at intervals of 0, 1, 10, 30, and 60 minutes, unlike the above other bacteria, the antibacterial effect was not confirmed immediately after treatment, but the growth of the bacteria after 1 minute This was not confirmed. In addition, it was confirmed that the efficacy continued up to the maximum time of the experiment, 60 minutes. There was no difference between 1% and 2%, and even 1% showed a high antibacterial effect of 100% [Table 12, The result of Time kill test (TKT) of Disinfectant].

4. Carrier test-AOAC Use-dilution method of Disinfectant

1) MRAb

As a carrier material in hospitals, as a result of treating bacteria on typical fabric, iron, glass, and gloves, and using 1% and 2% disinfectant compositions, R-Ab In the case, in both the 1,2% disinfecting composition, the strain was hardly reduced in the cloth, but the remaining carrier showed 100% disinfecting power, thereby inhibiting the growth of the strain. In the case of MRAb, 1,2% strains in cloth inhibited the bacteria of log1.6 and log1.9, respectively, and in iron, both concentrations showed 100% disinfecting power. On the surface of glass and rubber, the 1% disinfecting composition did not show perfect disinfecting power, but showed about log8 disinfecting power, and the 2% disinfecting composition showed 100% disinfecting power. Thus, 1, 2% of the disinfecting composition of the present invention did not show a significant difference in efficacy, but showed an antibacterial effect in a concentration-dependent manner [Table 13, Carrier test-AOAC Use-dilution method of Disinfectant].

2) VRE

In the case of cloth, R-Ef decreased by log 1.7 and log 1.8 in 1% and 2% hand sanitizer, respectively, and in VRE, log 1.2 and log 1.9 showed low decrease rates. However, as a result of treatment on the surface of iron, glass, and rubber, most of them showed a reduction rate of log 6.2 or more.In particular, the 1% cleaner showed 100% disinfecting power only on the glass surface treated with R-Ef, but in the case of 2% cleaner, R-Ef showed 100% disinfecting power on iron, glass, and rubber surfaces, and 100% disinfecting power only on iron and glass surfaces in VRE [Table 14, Carrier test-AOAC Use-dilution method of Disinfectant].

3) NTM (M. bovis)

In the case of M. bovis, as a result of treating bacteria on fabric, iron, glass, and gloves, and using 1% and 2% disinfectant compositions, the carrier and the present invention Regardless of the concentration of the disinfectant composition, it was confirmed that the growth of all bacteria was inhibited [Table 15, Carrier test-AOAC Use-dilution method of Disinfectant]. In particular, in the carrier test, the disinfectant composition had a high antibacterial effect even on cloth, and thus showed a particularly high antibacterial activity against NTM.

2-5. Agriculture, Forestry and Fisheries Quarantine and Inspection Division efficacy test

1) MRAB

According to the efficacy test of the Ministry of Agriculture, Forestry and Fisheries Quarantine and Inspection, the efficacy in 1% and 2% of the disinfecting composition of the present invention was confirmed. Distilled water, hard water, and organic diluent of R-Ab showed growth of bacteria in log11.7, log11.9, log11.9, whereas 1% disinfection composition experimental range of 0.8, 0.9, 1, 1.1, 1.2% The growth of the bacteria could not be confirmed at, and the growth of the bacteria could not be confirmed in the experimental ranges of 1.6, 1.8, 2, 2.2, and 2.4% of the 2% disinfecting composition. In the case of MRAb, the control group of distilled water, hard water, and organic diluent showed growth of log11.9, log11.9, and log11.9, whereas bacteria in the experimental range of 1% disinfectant composition were 0.8, 0.9, 1, 1.1, and 1.2%. The growth of could not be confirmed, and the growth of bacteria could not be confirmed in the experimental range of the 2% disinfecting composition of 1.6, 1.8, 2, 2.2, and 2.4%. In both bacteria, no difference was found according to distilled water, hard water, or diluent of organic matter [Table 16, 1% results of the efficacy test by the Ministry of Agriculture, Forestry and Fisheries Quarantine of the present disinfectant composition].

2) VRE

According to the efficacy test of the Ministry of Agriculture, Forestry and Fisheries Quarantine and Inspection, the efficacy in 1% and 2% of the disinfecting composition of the present invention was confirmed. Distilled water, hard water, and organic diluents of R-Ef showed growth of log7.0, log7.7, log7.7, whereas 1% disinfectant composition experimental range of 0.8, 0.9, 1, 1.1, 1.2% The growth of the bacteria could not be confirmed at, and the growth of the bacteria could not be confirmed in the experimental ranges of 1.6, 1.8, 2, 2.2, and 2.4% of the 2% disinfecting composition. In the case of VRE, the control group of distilled water, hard water, and organic diluent showed growth of log8.4, log8.1, and log8.1, while bacteria were found in 0.8, 0.9, 1, 1.1, and 1.2% of the experimental range of 1% disinfectant composition. The growth of could not be confirmed, and the growth of bacteria could not be confirmed in the experimental range of the 2% disinfecting composition of 1.6, 1.8, 2, 2.2, and 2.4%. In both bacteria, no difference was found according to distilled water, hard water, or diluent of organic matter [Table 17, 1%, 2% Results of the efficacy test by the Ministry of Agriculture, Forestry and Fisheries Quarantine of the present disinfectant composition].

3) NTM (M. bovis)

As a result of confirming the efficacy in 1% and 2% of the disinfecting composition of the present invention according to the efficacy test of the Ministry of Agriculture, Forestry and Fisheries Quarantine, 1% in the experimental range of the disinfecting composition of the present invention of 0.8, 0.9, 1, 1.1, 1.2% The growth of the bacteria could not be confirmed, and the growth of the bacteria could not be confirmed in the experimental ranges of 2% of the disinfecting composition of the present invention, 1.6, 1.8, 2, 2.2, and 2.4%. In both bacteria, no difference was found depending on distilled water, hard water, or diluent of organic matter [Table 18, 1%, 2% Results of the efficacy test by the Ministry of Agriculture, Forestry and Fisheries Quarantine of the present disinfectant composition].

<Test Example 3> Evaluation of the composition

1) Evaluation of blood cleaning power of the composition

In order to evaluate the blood cleaning power of the disinfectant composition, blood was applied to the hands, dried for 30 minutes, and the hands were washed using the disinfecting compositions of Examples and Comparative Examples, and then the blood cleaning power of the composition was measured using a luminol reagent.

In more detail, blood from a man in his mid-20s was used, and the collected blood was stored in a K2 EDTA tube (Becton Dickinson, 367525, UK). Blood was thoroughly stirred at room temperature for at least 30 minutes using a roller mixer (Wincom.Co.Ltd., KJMR-II, China) before use in the experiment.

1000 ul of the blood was evenly applied to the hands, and after drying the blood for 30 minutes, the hands were washed. When washing the hands, after washing the hands for 10 seconds in running water, the hands were washed with the disinfecting compositions of the Examples and Comparative Examples for 30 seconds, and the hands were washed in running water for 10 seconds to completely wash the composition. After washing the hands, the hands were strongly shaken to remove moisture first. Thereafter, the hands were lightly shaken for about 90 seconds to remove water secondarily, and a sample was collected by rubbing the palm of the hand with a sterile cotton swab moistened with sterile distilled water. The reaction was observed by dropping 2-3 drops of the prepared luminol working reagent by placing a cotton swab rubbed on the palm of the hand on a flat floor, and recording the following evaluation criteria based on the average value measured five times.

The luminol working solution was prepared according to the Weber manufacturing method, and the equipment was 100-1000 ul micro pipette (Eppendorf, 3120000062, German), and a conical tube (SPL Life sciences, Korea) was used. When taking pictures, a DSLR camera (Nikon, D7000, Japan), a macro lens (Tamron, SP AF 90mm F/2.8 Di MACRO 1:1, Japan), and a copy stand (RPS Lighting, RS-CS920, Australia) were used. The intensity of the luminol reaction was measured using the Adobe Photoshop version 8.0 (Adobe Systems, USA) program. The measured cleaning power of the blood was evaluated by the following evaluation criteria based on the average value of the following ratings.

[grade]

4 points: Blood was completely washed by the composition

3 points: more than 1/2 of the blood was washed by the composition

2 points: blood was washed to less than 1/2 by the composition

1 point: The blood was washed to less than 1/4 by the composition

[Evaluation standard]

◎: 4.0 points

○: 3.0 or more and less than 4.0

△: 2.0 points or more and less than 3.0 points

×: less than 2.0 points

2) Evaluation of the composition for preventing corrosion of machinery

In order to evaluate the anti-corrosion ability of the disinfectant composition, medical instruments were immersed in the disinfecting compositions of Examples and Comparative Examples, rinsed in water, and then sterilized 50 times, and then the corrosion characteristics were measured through an electrochemical method.

More specifically, after immersing the surgical blade in the disinfecting compositions of Examples and Comparative Examples for 5 minutes, rinsing in purified water for 30 seconds, sterilizing by autoclaving at 135 degrees for 10 minutes was repeated 50 times, and then through anodic polarization test. Corrosion properties were measured.

The surgical blade, which had been treated repeatedly for 50 times, was placed in a reaction tank containing a solution and connected to a Potentiostat (Model 263, EG&G) to conduct an experiment. The cell used two high-density carbon electrodes as auxiliary electrodes and a saturated calomel electrode (SCE) as the counter electrode. The test solution was carried out by simulating in vivo conditions in degassed 37°C and 0.9wt% NaCl, and dissolved oxygen that may exist in the solution was removed by injecting nitrogen gas into the solution at a rate of 10 ml/min for 30 minutes. Then, in order to remove the influence of oxides or impurities generated on the surface, a cathode potential of -600mV was applied and forcibly reduced for 10 minutes, and then maintained at an open circuit potential for 10 minutes. Thereafter, the test was repeated three times while increasing the potential at a scanning speed of 1 mV/sec in the anode direction from a potential low of about -150 mV from the measured corrosion potential. The corrosion characteristics of the instruments exposed to the measured disinfecting composition were evaluated based on the average value of the following ratings, based on the following evaluation criteria.

[grade]

4 points|pieces: The composition had good resistance to appliance corrosion

3 points: The composition had resistance to corrosion of equipment

2 points: The composition was susceptible to instrument corrosion

1 point: The composition was very susceptible to instrument corrosion

[Evaluation standard]

◎: 4.0 points

○: 3.0 or more and less than 4.0

△: 2.0 points or more and less than 3.0 points

×: less than 2.0 points

3) odor sensory evaluation of the composition

Regarding the odor evaluation, the sensory evaluation method using the human sense of smell in accordance with the current laws and regulations was conducted to evaluate the smell of the disinfectant composition.

In more detail, 50 professional panelists according to the criteria of the odor process test method (Notification No. 2007-17, National Institute of Environmental Sciences), 1 ml of the disinfecting composition of the above Examples and Comparative Examples, were applied to their hands under an environment of 25°C. About the smell generated after taking and rubbing the palm and the back of the hand, sensory evaluation was performed based on the following rating, and the following evaluation criteria were evaluated based on the average value of the rating.

[grade]

4 points: The composition does not have any unpleasant odor

3 points: The composition has a fine unpleasant odor

2 points: The composition has a slight unpleasant odor

1 point: The composition has a lot of unpleasant odor

[Evaluation standard]

◎: 4.0 points

○: 3.0 or more and less than 4.0

△: 2.0 points or more and less than 3.0 points

×: less than 2.0 points

4) Evaluation of skin irritation of the composition

In order to evaluate the skin irritation of the disinfectant composition, a skin irritation sensory evaluation was performed.

In more detail, 50 professional panelists took 1 ml of the disinfecting composition of the above Examples and Comparative Examples on their hands under an environment of 25°C and rubbed them on the palms and backs of the hands, according to the following rating. Based on the sensory evaluation, it evaluated by the following evaluation criteria based on the average value of the rating.

[grade]

4 points: No stimulation is felt by the composition

3: No stimulation by the composition

2 points: I feel stimulation by the composition

1 point: I feel very irritated by the composition

[Evaluation standard]

◎: 4.0 points

○: 3.0 or more and less than 4.0

△: 2.0 points or more and less than 3.0 points

×: less than 2.0 points

As shown in Tables 19 to 23, in the evaluation of blood cleaning power, device corrosion preventing ability, composition odor, and skin irritation, the blood cleaning power of the disinfecting compositions of Examples 1 to 7, device corrosion preventing ability, composition odor, and skin irritation It was confirmed that the disinfecting compositions of Comparative Examples 1 to 24 exhibited more excellent results than blood cleaning power, anti-corrosion ability, composition odor, and skin irritation.

In the evaluation of blood detergency of the disinfecting composition, the content of didecyldimethylammonium chloride contained in the disinfecting composition is 2.2% by weight or more, and the sum of the contents of didecyldimethylammonium chloride and alkyldimethylbenzylammonium chloride is 5% by weight or more. Dimethylbenzylammonium chloride/alkyldimethylbenzyl ammonium chloride" was found to have the most excellent blood cleaning power of the treatment group in the range of 0.9 to 1.5. In the evaluation of the anti-corrosion ability of the disinfectant composition, It was found that the anti-corrosion ability of the treatment group with a cocodimethylamine oxide content of 1.3 wt% or more and a sum of cocodimethylamine oxide and didecyldimethylammonium chloride content of 4 wt% or more was the most excellent. In the odor evaluation and skin irritation evaluation of the disinfecting composition, it was confirmed that the disinfecting compositions of Examples 1 to 7 of the present invention did not produce an unpleasant odor and did not irritate the skin at all.

Claims (4)

delete delete In the method for producing a disinfectant composition having a bactericidal effect on viruses, bacteria, and fungi,
The method for preparing a disinfectant composition having the sterilizing effect
(a) preparing a first composition by mixing 35 to 45% by weight of purified water and 1.8 to 3.3% by weight of alkyldimethylbenzyl ammonium chloride in a warming stirrer and stirring at a speed of 30 rpm;
(b) preparing a second composition by mixing 1.3 to 1.7% by weight of sodium edetate hydrate in the first composition and reacting with stirring at a speed of 20 rpm for 5 to 10 minutes;
(c) 1.8 to 3.3% by weight of didecyldimethylammonium chloride and 1.2 to 1.6% by weight of cocodimethylamine oxide were mixed in 15 to 25% by weight of purified water at a temperature of 40°C, and reacted with stirring at 50 rpm for 25 to 35 minutes. After cooling to room temperature to prepare a third composition;
(d) mixing the prepared second composition and the prepared third composition, mixing 0.001 to 0.003% by weight of a colorant, and stirring at a speed of 40 rpm to prepare a fourth composition; And
(e) Add 0.4 to 0.8% by weight of sodium hydroxide and the remaining amount of purified water to the prepared fourth composition so that the total composition is 100% by weight, and then stir at 50 rpm for 15 to 20 minutes, and the pH is 6 to 8 A method for producing a disinfecting composition having a sterilizing effect on viruses, bacteria, and fungi, characterized in that to prepare a disinfecting composition by controlling.
A disinfectant composition having a bactericidal effect on viruses, bacteria and fungi prepared by the method of claim 3

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