KR102397365B1 - Antiviral composition comprising chlorine dioxide solution and natural product-derived substance - Google Patents

Abstract

The present invention relates to an antiviral composition containing a chlorine dioxide solution and a natural product-derived substance. The antiviral composition according to the present invention has excellent virucidal activity against viruses recently becoming a worldwide problem, such as a corona virus and an influenza virus. In addition, the antiviral composition uses the chlorine dioxide solution prepared through a series of processes, thereby improving preservation and functionality of the chlorine dioxide solution, which has had a problem in preservation in the past, so that excellent antiviral activity may be maintained even during long-term storage.

Description

Antiviral composition comprising chlorine dioxide water and a material derived from natural products {ANTIVIRAL COMPOSITION COMPRISING CHLORINE DIOXIDE SOLUTION AND NATURAL PRODUCT-DERIVED SUBSTANCE}

The present invention relates to an antiviral composition comprising chlorine dioxide water and a material derived from a natural product.

With the recent outbreak of swine flu (influenza virus) and corona viruses (SARS, MERS, COVID-19, etc.) around the world, countries around the world are keen to establish quarantine measures.

As the influenza virus is an RNA virus, antigen mutation is relatively easy, and in the case of corona virus, various mutations are formed rapidly to cause repeated re-infection and serious new infectious diseases. is a time when you need

In order to prevent virus infection, the concept of 'contact defense' such as washing hands and wearing a mask has gone one step further and the concept of 'space defense' is emerging, and interest in related products is increasing. 'Space defense' refers to a method of reducing the possibility of virus propagation by inactivating or killing the virus in the space itself where the virus may exist in order to minimize the possibility of infection of various bacteria or viruses floating in the air of a specific space. do. In other words, it is a preventive method to minimize virus droplet infection in everyday living spaces such as homes, offices, elevators, restaurants, cars, hotels, and childcare facilities, or in public places such as churches, educational centers, schools, and performance halls. In particular, according to the World Health Organization (WHO), swine flu and coronavirus are transmitted from person to person, and it is reported that there is a high possibility of droplet infection, which is mainly transmitted through droplets spread in the air through coughing or sneezing. Therefore, the importance of quarantine against virus particles present in the atmosphere of the space where many people work or live is increasing day by day.

On the other hand, spray-type disinfectants using ethanol or hypochlorous acid water are representative products for space defense, and products using natural extracts known to have antiviral effects or using chlorine dioxide are being studied.

However, even if a natural extract known to have a general antiviral effect is used, it is practically ineffective or low on a specific virus in most cases. There is a problem in that long-term storage is weak because it is sensitive to changes in pH, and effective chlorine is volatilized according to changes in pH, so that it is difficult to remain or maintain effective chlorine in chlorine dioxide water.

The present inventors have recognized the problems of the prior art, and have completed the present invention by proving that the antiviral composition comprising chlorine dioxide water and cypress extract has excellent antiviral effect and preservation.

The present invention relates to an antiviral composition comprising chlorine dioxide water and a cypress extract.

The present invention relates to a cosmetic composition comprising the antiviral composition.

The present invention relates to an antiviral aqueous dispersion composition comprising the antiviral composition.

The present invention relates to an antiviral quasi-drug composition comprising the antiviral composition.

The present invention relates to a method for preparing the antiviral composition.

Hereinafter, this will be described in detail. All combinations of the various elements disclosed herein are within the scope of the present invention. In addition, it cannot be considered that the scope of the present invention is limited by the following specific description.

In addition, unless otherwise defined in this specification, all terms used in the specification should be understood to have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs.

Also, the singular expression includes the plural expression unless the context clearly dictates otherwise.

Also, in this specification, terms such as first, second, etc. may be used to distinguish or describe one component from other components, but the components should not be construed as being limited by the terms. For example, within the scope of the present invention, a first component may be termed a second component or vice versa.

In addition, in the present specification, the combination of alphabets and numbers is used to indicate each manufacturing step, and the precedence and succession of each manufacturing step including the corresponding alphabet is not determined according to the precedence of the alphabet.

The present invention provides an antiviral composition comprising chlorine dioxide water and cypress extract.

In the present invention, "chlorine dioxide" means a compound consisting of chlorine and oxygen, and "chlorine dioxide water" means an aqueous solution containing the chlorine dioxide.

In general, chlorine dioxide water is prepared by simply mixing chlorine dioxide with purified water. Therefore, in the present invention, in order to solve the above problems, the preservation property is improved by using a manufacturing method including a series of processes in the manufacturing process of chlorine dioxide water.

In the present invention, the chlorine dioxide water may be prepared by a method comprising the following steps:

A1) mixing chlorine dioxide with purified water; and

A2) using a nano-bubble generator (Nano generator) in the mixture to prepare nano-emulsified chlorine dioxide water.

The method for producing the chlorine dioxide water will be described in detail.

In the method for producing chlorine dioxide water of the present invention, step A1 is a step of mixing chlorine dioxide with purified water.

The chlorine dioxide may be mixed with purified water so that the concentration of effective chlorine in the prepared chlorine dioxide water is 30 to 70 ppm, and according to embodiments of the present invention, it can be mixed with purified water so that the concentration of effective chlorine is 50 ppm However, the present invention is not limited thereto.

In the method for producing chlorine dioxide water of the present invention, step A2 is a step of applying a nanobubble generator to the mixture.

In the present invention, "nano bubble generator (Nano generator)" refers to a device that generates nano-sized bubbles by repeating the chain reaction of compression and destruction of water molecules, and the nano-bubble generator is a nano-bubble-formed, nano-emulsion (Nano). It enables the production of emulsified chlorine dioxide water.

In the present invention, the nano-emulsion generator may use a known device capable of generating nano-sized bubbles, for example, a nano bubble generator of NEWMANTECH Co., Ltd. may be used, but limited thereto it is not going to be

In the present invention, the nano-bubble (nano-emulsion) may have a diameter of 1 to 500 nm, but is not limited thereto. In addition, according to embodiments of the present invention, the nano-bubble (nano-emulsion) diameter may be an average of 160 nm, but is not limited thereto.

In the present invention, when the size of the bubble is in the micro unit, there is a problem that the storage stability is low due to the deterioration of the chlorine dioxide water as the period elapses due to the strong tendency of the bubble to rise, but the bubble size of the emulsified chlorine dioxide water is nano In the case of a unit, it is possible to lower the tendency of bubbles to rise, which is very advantageous in terms of preservation. In particular, in the present invention, when nanobubbles having the above diameter range are generated, it has been specifically demonstrated that the preservation property is increased.

The application time of the nanobubble generator in the present invention may be 2 minutes to 10 minutes, preferably 4 minutes to 8 minutes, but is not limited thereto.

When applied less than the time range, chlorine dioxide water may not be sufficiently nano-emulsified, and when applied outside the time range, the nano-emulsification may be rather deteriorated.

In the present invention, "cypress (Chamaecyparis obtusa)" is also referred to as cypress, and is an evergreen arboreous tree in the gymnospermaceae Coniferaceae family. Due to its unique scent, it is used as a deodorant and antibacterial agent.

Phytoncide produced from cypress is a plant's self-defense material. It is a substance emitted or secreted by plants to resist pathogens, pests, and fungi, and contains sterilizing and insecticidal components. The constituent substances of phytoncide are organic compounds composed of terpenes, phenolic compounds, alkaloids, glycosides, etc. These phytoncides are natural substances, not chemically synthesized substances, and are easily absorbed by the human body, and selectively sterilize bacteria harmful to humans.

As a raw material in the present invention, the cypress tree may be harvested from nature or grown directly, or may be commercialized and sold.

In addition, as a raw material in the present invention, the cypress tree may be at least one selected from the group consisting of cypress logs, cypress leaves, and cypress fruits, preferably cypress logs, leaves and fruits, but is limited thereto. it is not

In the present invention, "extract" means the result of extraction using an appropriate extraction solvent and extraction method, and the extract is an extract obtained by extraction, a diluted or concentrated solution of the extract, a dried product obtained by drying the extract, a prepared product thereof, or purified products, or fractions.

In the present invention, the cypress extract may be prepared by a method comprising the following steps:

B1) crushing and mixing logs, leaves and fruits of cypress;

B2) immersing the mixture in brine;

B3) heating the immersed mixture to 57-58° C. for 20 to 28 hours and condensing the generated water vapor by passing it through a cooling device;

B4) separating the condensate into an essential sap and essential oil by aging for 20 to 28 hours; and

B5) purifying the essential sap.

The method for preparing the cypress extract will be described in detail.

In the method for producing a cypress extract of the present invention, step B1 is a step of crushing and mixing raw materials, leaves and fruits of cypress, which are raw materials, to increase the surface area of the cypress to facilitate extraction.

In step B1, the pulverization of cypress logs may be carried out to have a size of 0.5 to 1.5 cm ³ , and cypress leaves and cypress fruits may be carried out to have a size of 0.5 to 1.5 cm ² , but is not limited thereto. .

When pulverized to a size smaller than the above range, time and energy efficiency may be reduced in the process of pulverizing the raw material, and when pulverized larger than the above range, the extraction of the active ingredient contained in the extract is not sufficiently performed. You may not be able to fully demonstrate the effect you are doing.

According to embodiments of the present invention, the logs, leaves and fruits of the cypress tree may be mixed in a weight ratio of 1:0.1:0.05, but is not limited thereto.

In the method for preparing a cypress extract of the present invention, step B2 is a step of immersing the mixture in brine.

In step B2, the brine penetrates into the raw material to increase the extraction yield of the active ingredient contained in the cypress and is used for shortening the extraction time, and the brine has a concentration of 1 to 5% (w/v). And, according to embodiments of the present invention, it may be 3.5% (w / v), but is not limited thereto.

In the present invention, "active ingredient" means a component that can exhibit the desired activity (effect) alone or with a carrier that has no activity by itself, and can be used interchangeably with the active ingredient in the present specification. .

In addition, the B2 step is preferably carried out for a time during which the brine can be sufficiently absorbed in the raw material mixture, the immersion time may be 30 minutes to 90 minutes, preferably 40 minutes to 80 minutes, more preferably 50 minutes minutes to 70 minutes.

When immersed for less than the above time, the effect of increasing the extraction yield of the active ingredient and shortening the extraction time may be insignificant. This may be undesirable in terms of manufacturing efficiency.

In the present invention, step B3 is a step of condensing the immersed mixture by passing it through a cooling device while heating the immersed mixture at 57-58° C. for 20 to 28 hours.

In step B3, heating is performed at a low temperature of 57-58° C., which minimizes the destruction of active ingredients contained in cypress and preserves the unique flavor of cypress.

In addition, the B3 step may be performed for 20 to 28 hours, and if it is performed for a time less than the above range, the extraction of the active ingredient contained in the cypress tree may not be sufficiently performed, and the time exceeding the above range If it is carried out during the period, the effect of increasing the extraction of the active ingredient relative to time and energy consumption may not be large, so it is not appropriate in terms of manufacturing efficiency.

In the present invention, step B4 is a step of aging the condensate (condensed water vapor) for 20 to 28 hours to separate it into an essential sap and essential oil.

In the present invention, "essential SAP (Essential SAP) means an aqueous solution obtained when extracting essential oils from plants by steam distillation.

In the present invention, “essential oil” is a 100% natural aromatic oil extracted from a plant, and refers to a unique substance possessed by a plant to defend itself from the surrounding environment, survive, and reproduce.

In step B4, the condensate for separation into essential sap and essential oil may be aged for 20 to 28 hours, preferably for 24 to 28 hours, but is not limited thereto.

The essential sap separated in step B4 may be used as the cypress extract of the present invention by itself or after additional mixing of the separated essential oil and a series of additional steps.

When the essential sap is used by itself, the essential sap may contain essential oil at a concentration of 0.25±0.05% (v/v), but is not limited thereto.

In the present invention, step B5 is a step of further purifying the essential sap obtained in step B4.

The purification may be, for example, to produce a more purified cypress extract by passing through a tank made of SUS 304, in which a bubble generator and a sediment remover are attached, and remove the bubbles of fine sedimentation suspended matter generated by the bubble generator. It is not limited, and any known method can be used without limitation as long as it is used for purification of the extract.

In the present invention, the cypress extract may be prepared by a method further comprising the following steps:

B6) mixing the obtained essential oil so that the essential oil contained in the purified essential sap obtained in step B5 has a concentration of 2 to 4% (v/v);

B7) irradiating the mixture with ultrasonic waves for 1 to 5 minutes with an ultrasonic device; and

B8) Condensing the generated water vapor by passing it through a cooling device while heating the mixture to 57-58° C. for 15 to 20 hours while applying pressure to the mixture.

Step B6 of the present invention is a step of mixing the essential oil obtained in step B4 with the purified essential sap obtained in step B5. According to embodiments of the present invention, the additionally mixed essential oil is added to the essential sap. The included essential oil may be included so that the concentration is 2 to 4% (v/v).

If the essential oil is included below the concentration range, the intended effect of the present invention may be lowered due to the obtained cypress extract, and when the essential oil is included in the concentration range above the concentration range, dispersion of the essential oil in the essential sap If this is not done well, the yield of the cypress extract may be lowered.

Step B7 of the present invention is a step of irradiating ultrasonic waves to the mixture of essential sap and essential oil. In the present invention, the ultrasonic irradiation serves to facilitate the dispersion of the essential oil in the essential sap.

In the present invention, the ultrasonic wave may be irradiated using a known device, and according to embodiments of the present invention, the ultrasonic wave may have a frequency of 60 to 120 kHz, and an intensity of 100 to 1000 W, of the present invention. According to embodiments, the ultrasonic wave may have a frequency of about 90 kHz and an intensity of 200 W, but is not limited thereto.

In addition, the ultrasonic device may be, for example, an ultrasonic device manufactured by Sonics & Materials, but is not limited thereto.

In addition, the ultrasonic irradiation time, according to embodiments of the present invention, may be 1 to 5 minutes, but is not limited thereto.

Step B8 of the present invention is a step of condensing the generated water vapor by passing it through a cooling device while putting the mixture in a vacuum pressure tank and applying pressure to 57-58° C. for 15 to 20 hours.

In step B8, according to embodiments of the present invention, the pressure applied to the mixture may be 5 bar or more, preferably 5 to 10 bar, more preferably 7 bar, but is not limited thereto.

In addition, in the step B8, heating is performed at a low temperature of 57-58° C., which minimizes the destruction of the active ingredients contained in the cypress, and makes it possible to preserve the unique flavor of the cypress.

In addition, the B8 step may be performed for 15 to 20 hours, and if it is performed for a time less than the above range, the extraction of the active ingredient contained in the cypress may not be sufficiently performed, and the above range may be exceeded. If it is carried out for one hour, the effect of increasing the extraction of the active ingredient in relation to time and energy consumption may not be large, so it is not appropriate in terms of manufacturing efficiency.

In addition, the step B8 may be performed only once or repeatedly from 1 to 10 times, but may be preferably performed once in view of manufacturing efficiency.

The conventionally used cypress extract is generally prepared in a short time at high temperature and high pressure, which destroys the molecular structure of the components included in the cypress extract, causing the active ingredient and flavor to change.

In contrast, in the present invention, the cypress extract prepared by the method comprising the steps B1 to B5, or B1 to B8 has the advantage of preserving the active ingredient and flavor by preventing the destruction of the active ingredient, so the functional And in terms of effectiveness, it has a differentiation from the cypress extract that has been conventionally used.

In the present invention, the antiviral composition may be prepared by a method comprising the following steps:

C1) mixing chlorine dioxide water and cypress extract; and

C2) irradiating the mixture with ultrasonic waves for 5 to 15 minutes with an ultrasonic device.

In the method for preparing the antiviral composition of the present invention, step C1 is a step of mixing chlorine dioxide water and cypress extract.

According to embodiments of the present invention, the antiviral composition may include chlorine dioxide water and cypress extract in a weight ratio of 20:1 to 10:1, but is not limited thereto.

In the experimental examples to be described later, it was specifically confirmed that the composition mixed in parts by weight has excellent antiviral activity.

In step C1, chlorine dioxide water and cypress extract may be prepared by a specific method, as described above.

That is, the chlorine dioxide water may be prepared by a manufacturing method comprising a step including A1 and A2, and the cypress extract is prepared by a manufacturing method comprising the steps B1 to B5, or B1 to B8. it may have been

Step C2 is a step of irradiating ultrasonic waves to the mixture.

In the C2 step, when ultrasonic waves are irradiated, ultrasonic cavitation occurs, which leads to bubble formation, growth, and implosive collapse, thereby determining the shape of the particle and stabilizing it at the same time.

In the present invention, the ultrasonic wave may be irradiated using a known device, and according to embodiments of the present invention, the ultrasonic wave may have a frequency of 60 to 120 kHz, and an intensity of 100 to 1000 W, of the present invention. According to embodiments, the ultrasonic wave may have a frequency of 90 kHz and an intensity of 200 W, but is not limited thereto.

In addition, the ultrasonic device may be, for example, an ultrasonic device manufactured by Sonics & Materials, but is not limited thereto.

In addition, the antiviral composition of the present invention may be prepared by a method further comprising the following steps:

C3) Putting the mixture obtained in step C2 into a container equipped with an anion generator and generating anions for 20 to 60 minutes.

When generating an anion in the antiviral composition through the anion generator (or generating and including it in the composition), it can help to improve preservation and functionality.

In the present invention, the vessel in which the anion generator is installed may use a known device, and the C3 step may be applied sequentially or simultaneously with the C2 step.

In the present invention, the antiviral composition may have improved preservation.

In the present invention, "preservation" means that the content of effective chlorine is preserved in the chlorine dioxide water contained in the composition, and specifically, the antiviral effect of the composition is at least 30 days or more, preferably 90 days or more, more preferably Preferably, it means that it is maintained for 120 days or more, and more preferably, it is maintained for 180 days or more.

In the present invention, the term "antiviral" means inactivation, preferably permanent inactivation, of a pathogen virus.

Specifically, viruses that can be inactivated or permanently inactivated by the composition may be DNA viruses and RNA viruses, and specific examples include influenza A virus (human, bird, swine (new)), influenza B virus, parainfluenza. Virus, hepatitis (A~E) virus, measles virus, herpes virus, mumps virus, rabies virus, norovirus, HIV virus, SARS, avian flu, swine flu, Ebola virus, vaccinia virus, MERS coronavirus ( MERS-CoV) and may be one or more selected from the group consisting of COVID-19, but is not limited thereto.

According to embodiments of the present invention, the virus may be enveloped viruses, and preferably, may be one or more selected from influenza A virus, vaccinia virus or coronavirus, but is not limited thereto.

"Influenza" of the present invention is an acute respiratory disease accompanied by chills, fever, muscle pain, and cough, and is usually infected by human-to-human transmission through an aerosol discharged into the air through coughing or sneezing of an infected person do. Influenza infection is caused by an influenza virus belonging to the orthomyxoviridae family, and as an RNA virus, antigenic mutation is relatively easy, so repeated reinfection is possible within the infected population.

In the present invention, "Coronavirus" is a generic term for RNA viruses belonging to the Coronavirinae of the Coronaviridae, and refers to viruses that cause respiratory and digestive system infections in humans and animals. It is mainly transmitted by mucosal infection and droplet transmission, and it usually causes mild respiratory infections in humans, but it can also cause fatal infections, diarrhea in cattle and pigs, and respiratory diseases in chickens. .

Another aspect of the present invention provides a cosmetic composition comprising the antiviral composition.

The cosmetic composition of the present invention is a solution, external ointment, cream, foam, nourishing lotion, flexible lotion, pack, soft water, emulsion, makeup base, essence, soap, liquid detergent, bath agent, sunscreen cream, sun oil, suspension, emulsion It can be prepared in a formulation selected from the group consisting of liquid, paste, gel, lotion, powder, soap, surfactant-containing cleansing, oil, powder foundation, emulsion foundation, wax foundation, patch and spray, specifically, soap , may be a liquid detergent or hand cream, but is not limited thereto.

The cosmetic composition of the present invention may further include one or more cosmetically acceptable carriers to be formulated in general skin cosmetics, and common ingredients include, for example, oil, water, surfactant, humectant, lower alcohol, and thickener. , a chelating agent, a colorant, a preservative, a fragrance, and the like may be appropriately mixed, but the present invention is not limited thereto.

The cosmetically acceptable carrier included in the cosmetic composition of the present invention varies depending on the formulation of the cosmetic composition.

When the formulation of the present invention is an ointment, paste, cream or gel, as a carrier component, animal oil, vegetable oil, wax, paraffin, starch, tracanth, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc, zinc oxide, etc. may be used, but is not limited thereto. These may be used alone or in combination of two or more.

When the formulation of the present invention is a powder or a spray, lactose, talc, silica, aluminum hydroxide, calcium silicate, polyamide powder, etc. may be used as a carrier component, and in particular, in the case of a spray, additional chlorofluorohard propellants such as, but not limited to, carbon, propane/butane or dimethyl ether. These may be used alone or in combination of two or more.

When the formulation of the present invention is a solution or emulsion, a solvent, solubilizer or emulsifier may be used as a carrier component, for example, water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, Propylene glycol, 1,3-butylglycol oil, etc. can be used, and in particular, cottonseed oil, peanut oil, corn germ oil, olive oil, castor oil and sesame oil, glycerol aliphatic ester, fatty acid ester of polyethylene glycol or sorbitan may be used, but is not limited thereto. These may be used alone or in combination of two or more.

When the formulation of the present invention is a suspension, as a carrier component a liquid diluent such as water, ethanol or propylene glycol, a suspending agent such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol esters and polyoxyethylene sorbitan esters; Crystalline cellulose, aluminum metahydroxide, bentonite, agar or tracanth may be used, but is not limited thereto. These may be used alone or in combination of two or more.

In addition, the composition of the present invention can be used as a transdermal administration method, such as directly applied to the skin or sprayed, and the administration route of the composition of the present invention can be administered through any general route as long as it can reach the target tissue.

The usage amount of the composition of the present invention may be appropriately adjusted according to individual differences or formulations such as age, degree of lesion, etc., and may be used for one week to several months by applying an appropriate amount to the skin once to several times a day.

Another aspect of the present invention provides an antiviral water dispersion composition for spray comprising the antiviral composition.

In the case of the antiviral composition of the present invention, considering the purpose of virus suppression, it may be prepared in the form of a spray for convenience of use, but is not limited thereto.

Another aspect of the present invention provides a quasi-drug composition comprising the antiviral composition.

In the present invention, "quasi-drugs" refer to fibers, rubber products or the like, which are used for the purpose of treating, alleviating, treating or preventing diseases of humans or animals, have weak action on the human body, or do not act directly on the human body, and are devices or machines It refers to products that are not sterilized and similar, and products that are one of the preparations used for sterilization, insecticide, and similar purposes to prevent infection. Specifically, it includes insecticides, rodenticides, and disinfectants that are not directly applied to the human body used for the purpose of quarantine for public health and hygiene management, and more specifically, alcohols, aldehydes, cresols, sterilizing disinfectants in the form of soap formulations and It includes preparations used for other quarantine purposes.

When the composition of the present invention is added to a quasi-drug composition for the purpose of virus suppression, the composition may be added as it is or used together with other quasi-drug ingredients, and may be used appropriately according to a conventional method. The mixing amount of the active ingredient may be appropriately determined according to the purpose of use.

Another aspect of the present invention provides a disinfection method using the antiviral composition.

In the present invention, "disinfection" refers to an operation to suppress infectivity by killing or inactivating microorganisms on the surface of an object, etc., and has the purpose of hygiene management, infection and prevention of infectious diseases.

The antiviral composition of the present invention may further include emulsion stabilizers. The emulsion stabilizer is a substance that enhances the emulsification properties of the emulsion produced when the emulsion is diluted with water, for example, lower alcohols having less than 8 carbon atoms, glycols, higher alcohols having more than 11 carbon atoms, urea, magnesium chloride, sodium chloride, calcium chloride , sodium nitrate, or a mixture of two or more thereof, more specifically, ethanol, isopropyl alcohol, ethylene glycol, propylene glycol, hexylene glycol, cetyl alcohol, stearyl alcohol, magnesium chloride, sodium chloride, calcium chloride, nitric acid It may be sodium or the like, but is not limited thereto. The content of the emulsion stabilizer is not limited as long as it does not impair the disinfection effect of the active ingredient.

In addition, as long as the antiviral composition of the present invention does not inhibit the disinfection effect of the active ingredient, a fragrance, a pigment, a preservative, an antioxidant, an antifoaming agent, a carrier, etc. may be additionally included according to the purpose in addition to the active ingredient. For the carrier, clay (eg, kaolin, bentonite, acid clay, etc.), talc (eg talc powder, pyrophyllite powder, etc.), silica (eg diatomaceous earth, silicic anhydride, mica powder, etc.), alumina, sulfur powder and activated carbon One or two or more of them may be selected, but the present invention is not limited thereto.

The disinfection method of the present invention includes all acts of suppressing infectivity by losing the activity of the virus using the antiviral composition. Disinfection method in a broad sense refers to both a physical method or a chemical method, but since the disinfection method of the present invention is a method of removing microorganisms using an antiviral composition with disinfecting power, it is not a chemical disinfection method. desirable.

Another aspect of the present invention provides a method for preparing an antiviral composition comprising the following steps:

Mixing chlorine dioxide water and cypress extract; and

In the method for preparing an antiviral composition comprising; irradiating the mixture with ultrasonic waves for 5 to 15 minutes with an ultrasonic device,

The chlorine dioxide water,

A1) mixing chlorine dioxide with purified water; and

A2) using a nano-bubble generator in the mixture to prepare nano-emulsified chlorine dioxide water; prepared by a method comprising:

The cypress extract is

B1) crushing and mixing logs, leaves and fruits of cypress;

B2) immersing the mixture in brine;

B3) heating the immersed mixture to 57-58° C. for 20 to 28 hours and condensing the generated water vapor by passing it through a cooling device;

B4) separating the condensate into an essential sap and essential oil by aging for 20 to 28 hours; and

B5) purifying the essential fluid; antiviral composition manufacturing method prepared by a method comprising a.

In the preparation method of the present invention, the composition may be prepared by a method further comprising the following steps:

Putting the ultrasonically irradiated mixture into a container in which an anion generator is installed and generating anions for 20 to 60 minutes.

In the preparation method of the present invention, the preparation method of the cypress extract may be prepared by a method further comprising the following steps:

B6) mixing the essential oil so that the essential oil contained in the purified essential sap obtained in step B5 has a concentration of 2 to 4% (v/v);

B7) irradiating the mixture with ultrasonic waves for 1 to 5 minutes with an ultrasonic device; and

B8) Condensing the generated water vapor by passing it through a cooling device while heating the mixture to 57-58° C. for 15 to 20 hours while applying pressure to the mixture.

Specific details of the cosmetic composition, the aqueous dispersion composition for spraying, the quasi-drug composition and the antiviral composition manufacturing method in the present specification are the same as those mentioned in the antiviral composition unless the opposite content is described, avoid excessive repetition of the same content omitted for

The antiviral composition of the present invention has an excellent antiviral effect and excellent formulation stability and long-term storage.

In addition, the antiviral composition of the present invention is derived from a natural product, has no toxicity, and does not cause side effects even when applied to the human body, so its utility is high.

In addition, the antiviral composition of the present invention and a spray using the same have an effect of preventing damage (contagion) from bacteria or viruses at an early stage from places such as hospitals, classrooms, and public transportation that are the main routes of transmission.

In addition, the antiviral composition of the present invention and the spray using the same dries quickly and is sticky even though the composition of the present invention remains on the inner wall, outer wall, ceiling, article, etc. There is no such thing, so it is practically easy to use.

In addition, the antiviral composition of the present invention has not only an antiviral effect, but also antibacterial, antifungal, indoor air purification, humidity control and insect repellent, sick house syndrome, formaldehyde neutralization, forest bathing effect and stress relief, sterilization and deodorization, hand sanitizer, suppressing super bacteria It can help prevent and treat improvement of , sleep effect, house mite avoidance, allergy and atopic dermatitis.

Hereinafter, the present invention will be described in more detail by way of Examples. However, these examples are for illustrative purposes only, and the scope of the present invention is not limited by these examples. In addition, it will be understood that terms not specifically defined in this specification have meanings commonly used in the technical field to which the present invention pertains.

Example One

(1) Preparation of cypress extract

After cleaning the logs, leaves and fruits of the cypress tree, crushing (log 1 cm ³ , leaves/fruit 1 cm ² ), mixing the logs, leaves and fruits in a weight ratio of 1:0.1:0.05, and brine ( Concentration: 3.5%) for 1 hour.

Then, the immersed mixture was put into a stainless steel (SUS 304) container, heated at 57-58 ° C. for 24 hours, and the generated water vapor was passed through a cooling device to condense, and through an aging process for 24 hours, essential sap and separated with essential oils.

Then, the obtained essential sap was purified by passing through a tank (SUS 304 material) equipped with a bubble generator and a sediment remover.

Then, essential oil was added to the purified essential sap to a concentration of about 3% (v/v), and ultrasonic wave was irradiated for about 3 minutes using an ultrasonic device (90 kHz, 200 W, manufacturer: Sonics & Materials). . Then, it was placed in a stainless steel vacuum pressure tank and heated at 57-58° C. for about 18 hours while applying pressure (7 bar), and the generated water vapor was passed through a cooling device and condensed to prepare a cypress extract.

(2) production of chlorine dioxide water

Chlorine dioxide is mixed with purified water, and the resulting mixture is put into a nanobubble generator (manufacturer: NEWMANTECH Co., Ltd.), and the device is operated for 7 minutes to form a nanoemulsion (about 160 nm) with effective chlorine of about 50 ppm Chlorine dioxide water was produced.

(3) Preparation of antiviral composition

50 to 100 parts by weight of the prepared cypress extract are mixed with respect to 1000 parts by weight of the prepared chlorine dioxide water, and ultrasonic wave is irradiated for about 10 minutes using an ultrasonic device (90 kHz, 200 W, manufacturer: Sonics & Materials). An antiviral composition of the present invention was prepared.

Example 2

In the preparation of the antiviral composition of Example 1 (the table of contents (3)), the antiviral composition of Example 2 was prepared in substantially the same manner as in Example 1, except that the composition was prepared by the following method. said:

50 to 100 parts by weight of the prepared cypress extract were mixed with respect to 1000 parts by weight of the prepared chlorine dioxide water, and ultrasonic wave was irradiated for about 10 minutes using an ultrasonic device (90 kHz, 200 W, manufacturer: Sonics & Materials). .

Then, it was placed in a container in which an anion generator was installed, and anions were generated for 30 minutes to prepare the antiviral composition of the present invention.

comparative example One

In the preparation of the cypress extract of Example 1 (Table of Contents (1)), the antiviral composition of Comparative Example 1 was prepared in substantially the same manner as in Example 1, except that the composition was prepared by the following method. prepared.

After cleaning the logs, leaves, and fruits of cypress trees, crush them (log 1 cm ³ , leaves/fruit 1 cm ² ), mix them in a weight ratio of 1:0.1:0.05, and brine (concentration: 3.5%) Immerse for 1 hour.

Then, the immersed mixture was put into stainless steel (SUS 304), heated at 100-120° C. for 3 hours, and the generated water vapor was passed through a cooling device to condense, and after aging for 24 hours, essential sap and essential oil separated into

Then, the obtained essential sap was purified by passing through a tank (SUS 304 material) equipped with a bubble generator and a sediment remover.

Then, essential oil was added to the purified essential sap to a concentration of about 3% (v/v), and ultrasonic wave was irradiated for about 3 minutes using an ultrasonic device (90 kHz, manufacturer: Sonics & Materials). Then, it was placed in a stainless steel vacuum pressure tank and heated at 100-120° C. for about 3 hours while applying pressure (7 bar), and the generated water vapor was passed through a cooling device and condensed to prepare a cypress extract.

Comparative Example 2

In the preparation of the chlorine dioxide water of Example 1 (Table of Contents (2)), the antiviral composition of Comparative Example 2 was prepared in substantially the same manner as in Example 1, except that the composition was prepared by the following method. prepared.

Purified water was supplied to a chlorine dioxide water production device (manufacturer: Ilyeong), and chlorine dioxide water having an effective chlorine content of about 50 ppm was prepared.

comparative example 3

In the preparation of the antiviral composition of Example 1 (Table of Contents (3)), the antiviral composition of Comparative Example 3 was prepared in substantially the same manner as in Example 1, except that the composition was prepared by the following method. did

The antiviral composition of the present invention was prepared by mixing 50 to 100 parts by weight of the prepared cypress extract with respect to 1000 parts by weight of the prepared chlorine dioxide water.

Experimental Example 1. Verification of cytotoxicity and antiviral effect

For cytotoxicity and antiviral activity, it was carried out according to a quantitative suspension test.

The experimental conditions were as follows:

- Standard: EN 14476 + A2:07-2019

- Test temperature: 20 ± 1℃

- Test final concentration: 97%

- Titration method: log TCID ₅₀

- Exposure time: 1 minute

- Diluent used for testing: distilled water

-Strain: Vaccinia virus (ATCC reference number VR-1508) grown in BHK-21 cells in an atmosphere of 5% CO ₂ atmosphere

(1) of the virus titer

The virus titer was expressed as log TCID ₅₀ (calculated by Spearman-Karber method), and the virus titer against vaccinia virus was 6.750 log TCID ₅₀ .

(2) cytotoxicity

In the case of Vaccinia virus, BHK-21 cells were exposed to the composition of Example 1, and showed no cytotoxicity at 10 ^-1 dilution.

(3) antiviral activity

An experiment was conducted to confirm the cytotoxicity and virus inhibitory effect using the compositions of Examples and Comparative Examples.

Specifically, the virus suspension was titrated to 6.750 log TCID ₅₀ , and the decrease in virus titer was measured, and the results are shown in Table 1.

sample density exposure time temperature virus titer
(log TCID ₅₀ ) Decrease in virus titer Example 1 97% 1 min 20℃ 2.375 4.375

(In the case of the concentration of the tested product, if the decrease in virus titer is 4.0 log or more, it has an antiviral effect)

As shown in the table above, it was confirmed that the composition of Example 1 of the present invention had an antiviral (or virucidal) effect with a decrease in virus titer of 4.375.

Experimental Example 2. Verification of preservation improvement effect

In this experiment, in order to confirm the preservation improvement effect of the composition of the present invention, the decrease in the antiviral effect according to the storage period was measured and compared.

Specifically, it was compared whether the antiviral effect was maintained at 1 month, 3 months and 6 months immediately after the composition was prepared, and the experimental method is as follows.

As the test virus, influenza virus A (A/Brisbane/59/2007, NCCP 42464) and MERS virus (MERS-CoV/KOR/KNIH/002_05_2015) were used, and the test virus was cultured in a tissue culture flask, and cells When the adherent cells fell due to the lesion effect, freezing and thawing were repeated twice, centrifuged at 1,500 × g for 5 minutes, and the supernatant was extracted and stored frozen and used for the experiment.

The cell line was vero-E6, and was prepared by maintenance passage using DMEM (Dulbecco's modified Eagle's medium) medium supplemented with 5% FBS and penicillin/streptomycin.

In a culture medium, vero-E6 cells were inoculated into each well at 4.0×10 ⁴ cells per 100 μL in a 96-well plate, and cultured (5% CO ₂ , 37° C.) for 24 hours. Then, it was washed 2-3 times with PBS, and 100 μL of the culture solution and 100 μL of the compositions of Examples and Comparative Examples were inoculated.

And, after inoculating 100 μL of virus 10 times the amount of TCID ₅₀ (50% tissue culture infective dose) in 100 μL of each 100 μL of the inoculation culture solution containing the compositions of Examples and Comparative Examples, incubated for 2 days, and cell lesion effect The degree of inhibition was observed with a microscope, and as a control group, normal cells, cells inoculated with virus only, and cells added with only the compositions of Examples and Comparative Examples (infection titer of inoculation virus TCID ₅₀ , influenza virus A is 3.36x10 ² /mL, MERS-CoV virus is 2.35×10 ⁷ /mL).

The evaluation criteria for the results are as follows, and the results for influenza A are shown in Table 2, and the results for MERS virus are shown in Table 3.

[Evaluation standard]

(-): no virus suppression

(+): Partial inhibition of virus (about 50% or less)

(++): Partial inhibition of virus (more than about 50%)

(+++): Complete Virus Suppression

immediately after manufacturing 1 month 3 months 6 months Example 1 +++ +++ +++ +++ Example 2 +++ +++ +++ +++ Comparative Example 1 ++ + + - Comparative Example 2 +++ ++ + - Comparative Example 3 +++ ++ + +

immediately after manufacturing 1 month 3 months 6 months Example 1 +++ ++ ++ ++ Example 2 +++ +++ +++ ++ Comparative Example 1 + + - - Comparative Example 2 +++ ++ + - Comparative Example 3 +++ ++ + +

As shown in the above table, in the case of the present invention, it was confirmed that the antiviral activity of the composition of the present invention can be excellently maintained even after long-term storage because the decrease in antiviral activity is small even after 6 months have elapsed.

In contrast, in the case of the composition prepared by changing a part of the manufacturing method, it was not as good as the composition of the Example in terms of preservation, and in Comparative Example 1 in which the preparation method of the extract was partially changed, the antiviral effect was better than that of the Example can confirm that it is not.

Experimental Example 3. Sensory evaluation

The composition of Examples was subjected to sensory evaluation when sprayed in the air.

Specifically, 20 men and women in their 10s and 40s were selected, sprayed about 1 ml into the air in an enclosed space, and evaluated for scent, discomfort, dizziness, discomfort, and overall preference. The experiment was conducted 3 times, and after each experiment was completed, ventilation was given for 30 minutes and the subjects were given a break.

The results were evaluated using a 10-point rating method (10 points: positive to 1: negative), and are shown in Table 4.

sample incense pain in the neck
(Smell of chlorine) dizziness awkward overall preference Example 1 9.0 9.1 8.7 8.7 8.9

As can be seen in the table above, the composition of the present invention received an excellent evaluation of 8.5 points or more in terms of fragrance, discomfort, dizziness and overall preference, so that the composition of the present invention is an automatic injector or humidifier for suppressing viruses present in the atmosphere It was confirmed that it can be used usefully by applying it to others.

Claims (14)

delete delete delete delete delete delete delete delete delete delete delete mixing chlorine dioxide water and cypress extract in a weight ratio of 20:1 to 10:1;
irradiating the mixture with ultrasonic waves for 5 to 15 minutes with an ultrasonic device; and
In a manufacturing method comprising; putting the ultrasonically irradiated mixture into a container in which an anion generator is installed and generating anions for 20 to 60 minutes,
The chlorine dioxide water,
A1) mixing chlorine dioxide with purified water; and
A2) preparing nano-emulsified chlorine dioxide water using a nano-bubble generator in the mixture obtained in step A1;
The concentration of effective chlorine in the chlorine dioxide water is 30 to 70 ppm,
The cypress extract is
B1) crushing the logs, leaves and fruits of the cypress tree, and mixing them in a weight ratio of 1:0.1:0.05;
B2) immersing the mixture obtained in step B1 in brine;
B3) heating the immersed mixture to 57-58° C. for 20 to 28 hours and condensing the generated water vapor by passing it through a cooling device;
B4) separating the condensate into an essential sap and essential oil by aging for 20 to 28 hours;
B5) purifying the essential sap;
B6) mixing the essential oil obtained in step B4 so that the essential oil has a concentration of 2 to 4% (v/v) in the purified essential sap obtained in step B5;
B7) irradiating the mixture obtained in step B6 with ultrasonic waves having a frequency of 60 to 120 kHz and an intensity of 10 to 1000 W for 1 to 5 minutes with an ultrasonic device; and
B8) while applying pressure to the ultrasonically irradiated mixture obtained in step B7, heating to 57-58° C. for 15 to 20 hours, and condensing the generated water vapor by passing it through a cooling device; A method of preparing a composition for inhibiting influenza A virus or coronavirus activity, which was prepared by. delete delete