WO2022004975A1 - Antibacterial and rodent-repelling master batch composition using perilla frutescens extract and preparation method therefor - Google Patents

Abstract

The present invention relates to an antibacterial composition comprising eicosane, perillaldehyde, or a salt thereof, an antibacterial and rodent-repelling master batch comprising the antibacterial composition or a Perilla frutescens extract, and a preparation method therefor. The antibacterial composition exhibits excellent antibacterial activity against a broad spectrum of microorganisms such as Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, and methicillin-resistant Staphylococcus aureus. The master batch comprises the antibacterial composition and the Perilla frutescens extract containing same and as such, can provide an antibacterial effect on various synthetic resin products and exhibit the effect of preventing rodents from approaching thereto.

Description

Masterbatch composition for antibacterial and rodent repellent using perilla extract and method for manufacturing the same

The present invention relates to a method for producing an antibacterial and rodent repelling masterbatch using a perilla extract and a compound derived therefrom, and more particularly, to a variety of synthetic resin products containing a perilla extract and a compound derived therefrom, as well as an antibacterial effect on various synthetic resin products. It relates to a masterbatch composition for antibacterial and rodent repelling using a perilla extract and a compound derived therefrom, which gives the effect of inhibiting access of rodents, and a method for preparing the same.

As the environment changes, the spread of microorganisms that threaten human health, such as viruses, bacteria, and fungi that are harmful to the human body, is becoming a problem, and efforts to effectively block it are continuing.

The external symptoms of the product against bacteria may include decay odor and gas generation, pH drop, and consequent deterioration of physical and chemical properties. Home appliances such as refrigerators, air conditioners, etc., as well as transportation means such as automobiles and motorcycles, bowls, bathtubs, and flooring materials are widely distributed throughout the household.

An antibacterial agent is a substance having an antibacterial action on microorganisms, and means a substance or a substance manufactured from such a substance that has an antibacterial action by inhibiting a system in which the microorganism synthesizes a cell wall or protein. Antibacterial agents are widely used to treat diseases caused by bacterial infection, and have mainly been prepared by separating them from natural products including fungi or by chemically synthesizing them.

In particular, in the case of a food material packaging film or food storage container, it is necessary to provide antibacterial properties in order to prevent the food from being deteriorated by microorganisms. For this reason, various types of antibacterial films or plastic products are being developed, and mainly inorganic antibacterial agents or organic antibacterial agents prepared through chemical synthesis are added. However, recently, the harmfulness of these antibacterial agents to the human body has been highlighted, and they have many limitations, such as high cost and side effects.

Perilla frutescens (L) Britton var acuta (Thunb) Kudo) is an annual medicinal plant belonging to the angiosperm phylum, dicotyledonous family, and Lamiaceae, distributed in Korea and China. Stems are upright and square, with purple color on the entire pole, fragrant, and the leaves are opposite, broad ovate, pointed at the tip, round or somewhat wedge-shaped at the bottom, with serrated edges, hairs on both sides, and especially veins. It has long hairs on top and the petiole is long. Flowers bloom in August-September in light purple and run in raceme at the tips of stems and branches, and in the interstitial space of the upper leaf. The calyx is split into two, the upper one has 3 rows again and the lower one has 2 rows, and there are hairs inside and out of the tube. The corolla is short, usually pure, and the lower lip is slightly longer than the upper lip, and the stamens are two-fold. The whole species is purple, and the branches are round and have a net pattern. The leaves and stems are used for medicinal purposes, and the young leaves and seeds are edible. Young leaves are so similar that it is difficult to distinguish them from perilla leaves, and the sugar made from perylaldehyde in perilla is a sweetener 2,000 times stronger than normal sugar, so it is used in tobacco medicine. If the leaves are green instead of purple, they are called for viridis. The green leaves have white flowers and a stronger fragrance than perilla, and are often used medicinally.

Accordingly, the present inventors found that the perilla perilla contains ingredients such as icosane, perylaldehyde, caryophyllene and palmitic acid to exhibit antibacterial performance as well as a repelling effect from harmful rodents such as mice, and the active ingredient and synthetic resin of perilla extract to improve the mixing performance of As a result, the present invention was completed by developing a masterbatch through the process of extruding the perilla extract and the antimicrobial compound derived therefrom, supported on a carrier, mixed with a synthetic resin component, and extruded.

One object of the present invention is to provide an antibacterial composition comprising icosan or a salt thereof, or perylaldehyde or a salt thereof as an active ingredient.

Another object of the present invention is to inhibit the access of rodents as well as antibacterial effect to various synthetic resin products by containing the icosane or its salt, or perylaldehyde or its salt, or the perilla extract containing the compound or its salt. It is to provide a masterbatch composition for antibacterial and rodent avoidance using perilla extract that imparts an effect, and a method for manufacturing the same.

In one aspect, the present invention provides an antibacterial composition comprising icosane or a salt thereof, or perylaldehyde or a salt thereof as an active ingredient.

Specifically, the present invention provides an antibacterial composition comprising, as an active ingredient, one or two or more selected from the group consisting of eicosane, a salt of icosan, perylaldehyde, and a salt of perillaldehyde. to provide.

The antibacterial composition may include icosan (eicosane), perillaldehyde or a salt of the compound, preferably icosane or a salt thereof. In particular, the icosane and perylaldehyde, preferably icosane, can have an excellent antibacterial effect on microorganisms, and specifically inhibit the proliferation or growth of microorganisms such as Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, and metacillin-resistant Staphylococcus aureus. Therefore, there is an advantage of having excellent antibacterial activity.

The icosane or perylaldehyde may be chemically synthesized, but preferably may be derived from a plant extract. The plant extract may be, for example, a perilla extract. The perillafrutescens is an annual herb in the family Lamiaceae and is used to treat various diseases such as cough, sputum, sore throat, indigestion, swelling, paralysis symptoms, diabetes, and back pain. The perilla extract may be extracted from any one or more parts selected from the group consisting of leaves, stems and outposts of perilla, preferably leaves, stems and outpost parts.

The icosane or perylaldehyde may be used in the form of a salt, and these salts include an acid addition salt formed by a pharmaceutically, cosmetic, or food-acceptable free acid or a metal salt formed by a base. . An inorganic acid and an organic acid may be used as the free acid, and hydrochloric acid, sulfuric acid, hydrobromic acid, sulfurous acid or phosphoric acid may be used as the inorganic acid, and citric acid, acetic acid, maleic acid, humic acid, gluconic acid, methanesulfonic acid, etc. may be used as the organic acid. may be used, but is not limited thereto. The metal salt includes an alkali metal salt or an alkaline earth metal salt, and sodium, potassium or calcium salts are useful.

The antimicrobial extract contains icosan, perylaldehyde or a salt of the compound in an amount of 0.001 to 50% by weight, preferably 0.01 to 30% by weight, more preferably 1 to 20% by weight based on 100% by weight of the total composition can do. At this time, if the content of the compound is less than 0.001, the antibacterial activity may be insignificant, on the contrary, if it exceeds 50% by weight, the antibacterial activity may not be improved any more, so it may be inefficient, and stability in the formulation may not be secured.

As described above, the antimicrobial composition is icosane (eicosane) or a salt thereof, or perylaldehyde (perillaldehyde) or a salt thereof by including a microorganism, for example, E. coli (Escherichia coli), Pseudomonas aeruginosa (Pseudomonas aeruginosa), Staphylococcus aureus It can exert a remarkable antibacterial effect against microorganisms such as Staphylococcus aureus and metacillin-resistant Staphylococcus aureus (Staphylococcus aureus subsp. aureus).

The antibacterial composition not only has antibacterial activity, but is also environmentally friendly because it is derived from a natural substance, and has fewer side effects such as toxicity or skin allergy induction, skin irritation, potential as an environmental hormone, and resistance bacteria compared to chemical synthetic products. have.

Accordingly, the antibacterial composition may be applied to a product containing the same, or may be applied to a field selected from the group consisting of a pharmaceutical composition, a cosmetic composition, a food additive, a feed additive, an antiseptic composition, and a quasi-drug composition, but is not limited thereto does not

In addition, there is provided a product comprising the antibacterial composition. In the case of a product including the antimicrobial composition, a plastic product included in food packaging requiring antibacterial properties may be a packaging film, a packaging container, or a packaging material, but is not limited thereto.

When the antibacterial composition is used as an antibacterial pharmaceutical composition, the antibacterial pharmaceutical composition may be administered orally or parenterally during clinical administration, and may be used in the form of a general pharmaceutical formulation. Parenteral administration may refer to administration via a route other than oral administration, such as rectal, intravenous, peritoneal, muscle, arterial, transdermal, nasal, inhalation, ocular and subcutaneous. When the antibacterial pharmaceutical composition is used as a pharmaceutical, it may contain one or more active ingredients having the same or similar function.

That is, the antibacterial pharmaceutical composition may be administered in various oral or parenteral formulations, and when formulated, commonly used fillers, extenders, binders, wetting agents, disintegrants, surfactants such as diluents or excipients are used. is prepared Formulations for parenteral administration include sterile aqueous solutions, non-aqueous solutions, suspensions, emulsions, freeze-dried preparations, and suppositories. Non-aqueous solvents and suspensions may include propylene glycol, polyethylene glycol, vegetable oils such as olive oil, and injectable esters such as ethyl oleate. As a base of the suppository, Witepsol, macrogol, Tween 61, cacao butter, liulinji, glycerogelatin, etc. may be used.

In addition, the antibacterial pharmaceutical composition can be used by mixing with various pharmaceutically acceptable carriers such as physiological saline or organic solvents, and carbohydrates such as glucose, sucrose or dextran to increase stability or absorbability; Antioxidants such as ascorbic acid or glutathione, chelating agents, low molecular weight proteins or other stabilizers may be used as pharmaceuticals.

The effective dose of the antibacterial pharmaceutical composition is 0.01 to 100 mg/kg, preferably 0.1 to 10 mg/kg, and may be administered 1 to 3 times a day.

In the antibacterial pharmaceutical composition, the total effective amount may be administered to the patient in a single dose (Single does), such as in the form of a bolus or by infusion for a relatively short period, and multiple doses It can be administered by this long-distance fractionated treatment protocol. Since the concentration is determined by considering various factors such as the patient's age and health condition, as well as the administration route and number of treatments, the effective dosage of the patient is determined. It will be possible to determine an appropriate effective dosage according to the particular use as a pharmaceutical composition.

In addition, the antimicrobial adjuvant as the antibacterial pharmaceutical composition may be administered together with the antibiotic, before the antibiotic treatment, after the antibiotic treatment, and may be used as an adjuvant for enhancing the antimicrobial activity of the antibiotic. The antibacterial adjuvant preferably has a synergistic effect on the antibiotic and antibacterial activity.

When the antibacterial composition is used as a cosmetic composition, it may be prepared in any formulation conventionally prepared in the art, for example, a solution, suspension, emulsion, paste, gel, cream, lotion, powder, soap , surfactant-containing cleansing, oil, powder foundation, emulsion foundation, wax foundation, spray, and the like, but is not limited thereto. More specifically, it may be prepared in the form of a flexible lotion, a nourishing lotion, a nourishing cream, a massage cream, an essence, an eye cream, a cleansing cream, a cleansing foam, a cleansing water, a pack, a spray, or a powder.

When the formulation of the cosmetic composition is a paste, cream or gel, animal oil, vegetable oil, wax, paraffin, starch, tragacanth, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc or zinc oxide, etc. can be used

When the formulation of the cosmetic composition is a powder or a spray, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder may be used as a carrier component, and in particular, in the case of a spray, additional chlorofluorohydrocarbon, propellants such as propane/butane or dimethyl ether.

When the formulation of the cosmetic composition is a solution or emulsion, a solvent, solubilizer or emulsifier is used as a carrier component, for example, water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1,3-butylglycol oil, glycerol fatty esters, fatty acid esters of polyethylene glycol or sorbitan.

When the formulation of the cosmetic composition 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 ester, and polyoxyethylene sorbitan ester; Crystalline cellulose, aluminum metahydroxide, bentonite, agar or tragicant may be used.

When the formulation of the cosmetic composition is surfactant-containing cleansing, aliphatic alcohol sulfate, aliphatic alcohol ether sulfate, sulfosuccinic acid monoester, isethionate, imidazolinium derivative, methyl taurate, sarcosinate, fatty acid as carrier components Amide ether sulfates, alkylamidobetaines, fatty alcohols, fatty acid glycerides, fatty acid diethanolamides, vegetable oils, lanolin derivatives or ethoxylated glycerol fatty acid esters can be used.

When the antibacterial composition is used as a food additive, the icosane, perylaldehyde, or salts thereof may be added as it is or may be used together with other food ingredients, and may be appropriately used according to a conventional method. The mixing amount of the active ingredient may be appropriately determined according to the purpose of its use. In general, the icosane, perylaldehyde or a salt thereof is added in an amount of 15 parts by weight or less, preferably 10 parts by weight or less, based on the raw material. However, in the case of long-term intake, the amount may be less than the above range, and since there is no problem in terms of stability, the active ingredient may be used in an amount above the above range.

Examples of the food include meat, sausage, bread, chocolate, candy, snacks, confectionery, pizza, ramen, other noodles, gum, dairy products including ice cream, various soups, beverages, tea, drinks, alcoholic beverages and vitamin complexes, etc. and includes all foods in the ordinary sense.

When the antibacterial composition is used as a feed additive, it replaces the existing antibiotics for animals and suppresses the growth of harmful pathogenic microorganisms to improve the health of the animal body, improve the weight and meat quality of the animal, and increase the milk production and immunity has an increasing effect. The feed composition may be prepared in the form of fermented feed, compound feed, pellet form, silage, and the like.

The fermented feed can be prepared by fermenting organic matter by adding various microbial groups or enzymes other than the icosane, perylaldehyde or salts thereof, and the compounded feed includes several types of general feed and the icosane or salts thereof, Alternatively, perylaldehyde or a salt thereof may be prepared alone or by mixing. The feed in the form of pellets can be prepared by applying heat and pressure to the compounded feed, etc. in a pellet machine, and silage can be prepared by fermenting the feed with microorganisms. Wet fermented feed collects and transports organic matter such as food waste, mixes excipients for sterilization process and moisture control in a certain ratio, and ferments it at a temperature suitable for fermentation for 24 hours or more so that the moisture content is about 70%. It can be adjusted and manufactured. Fermented dry feed can be prepared by adjusting the moisture content of the wet fermented feed to 30% to 40% through an additional drying process.

When the antibacterial composition is used as an antiseptic composition, the antiseptic composition includes a food preservative, a cosmetic preservative, or a pharmaceutical preservative. The food preservatives, cosmetic preservatives and pharmaceutical preservatives are additives used to prevent deterioration, spoilage, discoloration and chemical changes of pharmaceuticals. These include sterilizing agents and antioxidants, and inhibiting the growth of microorganisms such as bacteria, mold, yeast, etc. and functional antibiotics, such as inhibiting the growth or sterilization of putrefactive microorganisms in pharmaceuticals. Ideal conditions for such a preservative composition should be non-toxic and effective even in a small amount.

When the antibacterial composition is used as a quasi-drug composition, the icosane or its salt, or perylaldehyde or its salt can be added alone or mixed and used as it is, or used together with other quasi-drugs or quasi-drug ingredients, and appropriate according to a conventional method can be used The mixing amount of the active ingredient may be suitably determined according to the purpose of use. Specifically, the quasi-drug composition may be a disinfectant cleaner, shower foam, gargrin, wet tissue, detergent soap, hand wash, humidifier filler, mask, ointment, patch, or filter filler.

As another aspect, the present invention provides a masterbatch composition for antibacterial and rodent repelling using a perilla extract, characterized in that it consists of a resin mixture and a perilla extract and/or a carrier mixture on which the antibacterial composition is supported.

The antibacterial and rodent repelling masterbatch composition using the perilla extract and/or the antibacterial composition according to the present invention consists of a resin mixture and a perilla extract and/or a carrier mixture on which the antibacterial composition is supported, 100 parts by weight of the resin mixture and 2 to 4 parts by weight of the perilla extract or the carrier mixture on which the antibacterial composition is supported.

The resin mixture serves to provide a masterbatch for resin by mixing with the perilla extract and/or the carrier mixture on which the antibacterial composition is supported. Various synthetic resins according to the type of resin to which the masterbatch manufactured through the present invention is applied In general, it is preferable to use a polyolefin resin in consideration of the compatibility without significantly reducing the physical properties of the general-purpose resin, and 100 parts by weight of linear low-density polyethylene and 10 to 50 parts by weight of ethylene vinyl acetate. It is most desirable to do

In addition, the perilla extract and / or the carrier mixture on which the antibacterial composition is supported is made by mixing 60 to 70 parts by weight of the carrier mixture with 100 parts by weight of the perilla extract and / or the antibacterial composition, the masterbatch composition according to the present invention It is applied in a supported form in a carrier mixture so that the perilla extract or the antibacterial composition, which imparts an antibacterial and rodent repelling effect, can be well dispersed in the resin mixture.

At this time, the carrier mixture is made by mixing 10 to 1000 parts by weight of montmorillonite with improved interlayer spacing in 100 parts by weight of crystalline calcium carbonate, and the crystalline calcium carbonate is α-D-glucose of 0.05% by weight or less of calcium dichloride and sodium carbonate 1: After reacting at a molar ratio of 1, it is prepared by stabilizing for 20 to 30 hours, and the montmorillonite with improved interlayer spacing is 30 to 50 parts by weight of a 0.2 mol/L polyethylene glycol solution in 100 parts by weight of a 0.2 mol/L montmorillonite solution. It is prepared by mixing and stirring for 3 to 5 hours and then drying.

As another aspect, the present invention provides a method for producing a masterbatch for antibacterial and rodent repelling using a perilla extract and/or the antibacterial composition.

As a specific aspect, the present invention provides an extract / composition preparation step (S101) for preparing a perilla extract or preparing the antibacterial composition, a carrier mixture preparation step for mixing calcium carbonate and montmorillonite (S103), the extract / composition preparation step ( The supporting step (S105) of supporting the perilla extract and/or the antibacterial composition prepared or prepared through S101) on the carrier mixture prepared through the carrier mixture preparation step (S103), the supporting step (S105) on the resin mixture. Antibacterial and rodent avoidance consisting of a raw material mixing step (S107) of mixing the perilla extract and/or a carrier mixture on which the antibacterial composition is supported and an extrusion step (S109) of extruding the mixture prepared through the raw material mixing step (S107) A method for preparing a masterbatch is provided.

The extract/composition preparation step (S101) is a step of preparing a perilla extract or preparing the antibacterial composition described above.

The perilla extract of the present invention can be prepared from any one or more selected from the group consisting of perilla leaves, stems, roots and outages.

The perilla extract can be obtained by extraction with water or various organic solvents. At this time, the organic solvent used is not particularly limited as long as an extract having antibacterial and rodent repelling effects can be obtained, but preferably water, a polar solvent or a non-polar solvent, and more preferably water, carbon number 1 to 4 lower alcohols (ethanol, methanol, propanol or butanol, etc.), a mixed solvent thereof, etc. may be used, and most preferably water may be used.

The method for obtaining the perilla extract is also not particularly limited thereto, as long as an extract having antibacterial and rodent repelling effects can be obtained. The extraction method includes hot water extraction, cold extraction, ultrasonic extraction, supercritical extraction, or reflux cooling extraction method, and it is preferably performed by a hot water extraction method or a supercritical extraction method.

As an example, in the case of hot water extraction, pre-treatment by drying and pulverizing perilla after washing, mixing 500 to 1000 parts by weight of purified water with 100 parts by weight of pre-treated perilla, and heating at a temperature of 80 to 90° C. for 10 to 30 minutes is done by At this time, in order to improve the dissolution efficiency of the active ingredient contained in the perilla perilla, the process of roasting the pre-treated perilla at a temperature of 100 to 110° C. for 30 to 50 seconds may be performed.

As an example, in the case of supercritical extraction, pretreatment is performed by drying and pulverizing perilla perilla after washing, and putting the pretreated perilla into a crystallization tank at 38 to 42 ° C using a high-pressure pump and injecting CO2 to extract at a pressure of 200 to 400 bar. can In the case of supercritical extraction of perilla under the above-described conditions, the yield is excellent and the antibacterial and rodent repelling effects are excellent.

The perilla extract prepared through the above process may be subjected to a process such as filtration after cooling to room temperature. Repels harmful rodents such as rats.

The antibacterial composition of the present invention is a composition comprising as an active ingredient at least one material selected from the group consisting of icosane, perylaldehyde, or salts of these compounds. Since the antibacterial composition is the same as described above, a detailed description thereof will be omitted below.

The carrier mixture preparation step (S103) is a step of preparing a carrier mixture by mixing calcium carbonate and montmorillonite.

It is preferable to use crystalline calcium carbonate as the calcium carbonate, and it is preferable to use the montmorillonite with improved interlayer spacing. desirable.

The crystalline calcium carbonate is prepared by reacting calcium dichloride having α-D-glucose of 0.05 wt% or less and sodium carbonate in a molar ratio of 1:1, then stabilizing for 20 to 30 hours, filtering and drying, which is prepared through the above process. As shown in FIG. 6 below, it can be seen from the scanning electron microscope (FE-SEM) image that the crystalline calcium carbonate is a cauliflower-type vaterite crystalline calcium carbonate that has a round shape as an aggregate. Calcium carbonate of flower-type vaterite crystal phase improves the ratio of perilla extract supported between crystal phases.

In addition, the montmorillonite with the improved interlayer spacing is prepared by mixing 30 to 50 parts by weight of a polyethylene glycol solution having a concentration of 0.2 mol/L to 100 parts by weight of a montmorillonite solution having a concentration of 0.2 mol/L, followed by stirring for 3 to 5 hours, and then drying.

In general, montmorillonite, a kind of clay mineral, is a mineral of a layered structure with a smectite crystal structure. It is divided into K5 to K30 grades depending on the degree of acid treatment, and the currently common montmorillonite is K10 grade. Montmorillonite K30 has a wider specific surface area than K10, so it shows high efficiency when used as a carrier or catalyst.

Therefore, through the above process, low molecular weight polyethylene glycol is inserted between the silicate layers of montmorillonite to increase the interlayer distance, so that the loading efficiency of the perilla extract is improved.

At this time, the polyethylene glycol has a molecular weight of 200 g/mol to 4000 g/mol, and modified montmorillonite with improved interlayer spacing prepared using polyethylene glycol having the same molecular weight as above was analyzed by X-ray diffraction analysis, and is shown in FIGS. 7 and 1 below. indicated. When the interlayer gap is widened, the peak detected at the diffraction angle corresponding to the intrinsic interlayer gap of the clay moves to a lower angle or disappears, and this can be evaluated as evidence. The change in the interlayer distance of montmorillonite modified using polyethylene glycol was confirmed according to Bragg's law of Equation 1 below.

[Equation 1]

(λ wavelength, d: interlayer distance, θ diffraction angle)

Sample	Degree (2θ)	d-spacing(Å)
M10	8.918	9.90808
M10PEG200	8.841	9.99433
M10PEG400	8.854	9.97901
M10PEG1000	8.855	9.97851
M10PEG2000	8.859	9.97379
M10PEG4000	8.859	9.97383

As shown in Table 1 and below, in the case of montmorillonite K30, the interlayer spacing was 9.98 Å, whereas that of montmorillonite of K10 grade was as low as 9.91 Å. It can be seen that a better or equivalent interlayer spacing is exhibited.

The supporting step (S105) is a step of supporting the perilla extract and/or the antibacterial composition prepared through the extract/composition preparation step (S101) on the carrier mixture prepared through the carrier mixture preparation step (S103). 60 to 70 parts by weight of the carrier mixture prepared through the carrier mixture preparation step (S103) is mixed with 100 parts by weight of the perilla extract and/or the antibacterial composition prepared through the extract/composition preparation step (S101), and for 5 to 7 hours After stirring, it is made by filtration and drying, and most preferably, 100 parts by weight of the perilla extract and/or antibacterial composition prepared through the extract/composition preparation step (S101) through the carrier mixture preparation step (S103) After mixing 66.6 parts by weight of the prepared carrier mixture and stirring for 6 hours, it is preferable to prepare by filtration and drying.

The carrier mixture prepared through the above process was photographed with a scanning electron microscope (FE-SEM), and is shown in FIG. 8 below.

As shown in FIG. 8 below, it can be confirmed that the particle size of the carrier increases after the perilla extract and the antibacterial composition are supported on the carrier, which indicates that the perilla extract and the antibacterial composition have excellent loading efficiency on the carrier.

The raw material mixing step (S107) is a step of mixing the carrier mixture in which the perilla extract and/or the antibacterial composition is supported through the supporting step (S105) in the resin mixture, and the supporting step (S105) in 100 parts by weight of the resin mixture. It is made by mixing 0.5 to 5 parts by weight of the carrier mixture on which the perilla extract and/or the antibacterial composition is supported. If the content of the carrier mixture is less than 0.5, the antibacterial effect or rodent repelling effect of the prepared masterbatch is insignificant, and the When the content of the carrier mixture exceeds 5 parts by weight, the antibacterial effect or rodent repelling effect of the prepared masterbatch is not greatly improved, but the physical properties of the masterbatch are reduced and the manufacturing cost is increased.

At this time, the resin mixture can be used by mixing various synthetic resins depending on the type of resin to which the masterbatch is applied. In general, when considering the compatibility without significantly reducing the physical properties of the general-purpose resin, it is better to use a polyolefin resin. Preferably, 100 parts by weight of linear low-density polyethylene and 10 to 50 parts by weight of ethylene vinyl acetate are mixed and used.

The extrusion step (S109) is a step of extruding the mixture prepared through the raw material mixing step (S107), and the mixture prepared through the raw material mixing step (S107) is extruded with an extruder and then cooled and cut is commonly used This is the stage of manufacturing the masterbatch size.

As another aspect, the present invention provides an antibacterial and rodent repelling resin composition, characterized in that it contains the antibacterial and rodent repelling masterbatch composition using the perilla extract and/or the antimicrobial composition.

More specifically, it is possible to prepare a plastic or rubber resin product by containing the antibacterial and rodent repelling masterbatch using the perilla extract and/or the antibacterial composition according to the present invention in the resin composition. The products include, but are not necessarily limited to, kitchenware, household goods, and baby products.

The antibacterial composition of the present invention is excellent in a wide range of microorganisms such as E. coli, Pseudomonas aeruginosa, Staphylococcus aureus and metacillin-resistant Staphylococcus aureus by including eicosane or a salt thereof, or perillaldehyde or a salt thereof It may have antibacterial activity.

In addition, the antimicrobial composition of the present invention not only has a wide range of antibacterial activity against microorganisms, but is also environmentally friendly as it is a material extracted from natural substances, and is toxic or skin allergy-induced, skin irritation, potential as an environmental hormone, compared to chemical synthetic products, There is an advantage in that there are few side effects such as inducing resistant bacteria.

Moreover, the method for producing a masterbatch for antibacterial and rodent repelling using the perilla extract and antibacterial composition according to the present invention contains the perilla extract and/or antibacterial composition to provide an antibacterial effect to various synthetic resin products as well as the effect of inhibiting the access of rodents It shows an excellent effect of providing a masterbatch that gives

1 is a photograph showing the results of an antimicrobial activity test against E. coli, Pseudomonas aeruginosa, Staphylococcus aureus, and metacillin-resistant Staphylococcus aureus (MRSA) using humulene according to an embodiment of the present invention.

2 is a photograph showing the results of an antibacterial activity test for E. coli, Pseudomonas aeruginosa, Staphylococcus aureus, and metacillin-resistant Staphylococcus aureus (MRSA) using eicosane according to an embodiment of the present invention.

3 is a photograph showing the results of an antimicrobial activity test against E. coli, Pseudomonas aeruginosa, Staphylococcus aureus, and metacillin-resistant Staphylococcus aureus (MRSA) using perillaldehyde according to an embodiment of the present invention.

4 is a photograph showing the results of an antibacterial activity test against E. coli, Pseudomonas aeruginosa, Staphylococcus aureus, and metacillin-resistant Staphylococcus aureus (MRSA) using caryophyllene according to an embodiment of the present invention.

5 is a photograph showing the antibacterial activity test results for E. coli, Pseudomonas aeruginosa, Staphylococcus aureus, and metacillin-resistant Staphylococcus aureus (MRSA) using palmitic acid according to an embodiment of the present invention.

6 is a photograph showing the crystalline calcium carbonate used in the present invention taken with a scanning electron microscope (FE-SEM).

7 is a graph showing the analysis of montmorillonite with improved interlayer spacing used in the present invention by X-ray diffraction analysis.

8 is a photograph showing the carrier mixture used in the present invention taken with a scanning electron microscope (FE-SEM).

Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited by the following examples.

Example 1: Evaluation of antibacterial activity of antibacterial composition

Antibacterial activity was evaluated for icosane and perylaldehyde, which are antibacterial compositions according to the present invention. For comparison, the antibacterial activity was also evaluated for Comparative Example 1 (humulene), Comparative Example 2 (caryophyllene), and Comparative Example 3 (palmitic acid) as additional compounds for comparison. Among the components, caryophyllene, palmitic acid, humlen and perylaldehyde are dissolved with DMSO (dimethyl sulfoxide) and icosane is dissolved at a concentration of 10 mg/mL with acetone, and the solution in which each compound is dissolved is distilled with 10 An antibacterial activity test was performed using a concentration of 1,000 ppm as a concentration by weight as a sample for an antimicrobial activity test.

Antibacterial activity was commissioned by the Korea Institute of Construction and Living Environment and was performed according to the test method of KCL-FIR-1002:2018. The bacterial reduction rate was tested by inoculating the strain on the sample for testing antibacterial activity of 1,000 ppm and checking the concentration of the bacteria present in the test specimen 24 hours later. The strains used were Escherichia coli ATCC25922 for Escherichia coli, Pseudomonas aeruginosa ATCC15442 for Pseudomonas aeruginosa, Staphylococcus aureus ATCC6538 for Staphylococcus aureus, and Staphylococcus aureus subsp. Aureus ATCC33591 was used. Each inoculum had a concentration of E. coli 8.3×10 ⁴ CFU/mL, Pseudomonas aeruginosa 8.0×10 ⁴ CFU/mL, Staphylococcus aureus 3.1×10 ⁴ CFU/mL and metacillin-resistant Staphylococcus aureus 9.0×10 ⁴ CFU/mL, respectively. injected. The results are shown in Table 2 and FIGS. 1 to 5 below.

division

coli

Pseudomonas aeruginosa

Staphylococcus aureus

MRSA

initial concentration (CFU/mL)

concentration after 24 hours (CFU/mL)

decrease rate (%)

initial concentration (CFU/mL)

concentration after 24 hours (CFU/mL)

decrease rate (%)

initial concentration (CFU/mL)

concentration after 24 hours (CFU/mL)

decrease rate (%)

initial concentration (CFU/mL)

concentration after 24 hours (CFU/mL)

decrease rate (%)

Control (BLANK)

8.3×10 4

7.3×10 5

-

8.0×10 4

8.7×10 5

-

3.1×10 4

4.1×10 5

-

9.0×10 4

4.1×10 5

-

humulene

8.3×10 4

7.0×10 3

99.0

8.0×10 4

5.2×10 3

99.4

3.1×10 4

<10

99.9

9.0×10 4

<10

99.9

eicosane

8.3×10 4

<10

99.9

8.0×10 4

<10

99.9

3.1×10 4

<10

99.9

9.0×10 4

<10

99.9

perillaldehyde

8.3×10 4

<10

99.9

8.0×10 4

<10

99.9

3.1×10 4

<10

99.9

9.0×10 4

<10

99.9

caryophyllene

8.3×10 4

9.0×10 4

87.6

8.0×10 4

7.0×10 3

91.9

3.1×10 4

1.8×10 4

95.6

9.0×10 4

1.4×10 4

96.1

palmitic acid

8.3×10 4

5.1×10 4

93.0

8.0×10 4

6.7×10 3

92.2

3.1×10 4

3.6×10 4

91.2

9.0×10 4

1.7×10 4

95.0

According to the antibacterial activity evaluation results shown in Table 1 and FIGS. 1 to 5, in the case of icosane and perylaldehyde, the growth of bacteria was inhibited for the 4 types of tested bacteria, and it was confirmed that the antibacterial action was very excellent at 99.9%.

On the other hand, in the case of Comparative Example 1 (Humlen), it showed relatively low antibacterial activity of 99.0% or more compared to the icosane and perylaldehyde for the 4 types of tested bacteria, and the antibacterial properties of E. coli of Comparative Example 2 (caryophyllene) Except for, Comparative Example 1 (humlen), Comparative Example 2 (caryophyllene), and Comparative Example 3 (palmitic acid) were found to show antibacterial activity of 90% or more.

Through this, it was found that the icosane and perylaldehyde exhibit excellent antibacterial activity against E. coli, Pseudomonas aeruginosa, Staphylococcus aureus, and metacillin-resistant Staphylococcus aureus.

Preparation Example 1: Preparation of perilla extract

After washing, drying and pulverizing perilla, 800 parts by weight of purified water was mixed with 100 parts by weight of pulverized perilla, and filtered after heating at a temperature of 90° C. for 20 minutes to prepare a perilla extract.

Preparation Example 2: Preparation of crystalline calcium carbonate

After reacting calcium dichloride and sodium carbonate having α-D-glucose of 0.05 wt% or less in a molar ratio of 1:1, the mixture was stabilized for 24 hours, filtered and dried to prepare crystalline calcium carbonate.

Preparation Example 3: Preparation of montmorillonite with improved interlayer spacing

40 parts by weight of a polyethylene glycol solution having a concentration of 0.2 mol/L was mixed with 100 parts by weight of a montmorillonite solution having a concentration of 0.2 mol/L, stirred for 4 hours, and then dried to prepare montmorillonite with improved interlayer spacing.

Preparation Example 4: Preparation of carrier mixture

A carrier mixture was prepared by mixing 100 parts by weight of crystalline calcium carbonate prepared in Preparation Example 2 and 100 parts by weight of montmorillonite having improved interlayer spacing prepared in Preparation Example 3.

Example 2: Preparation of masterbatch for antibacterial and rodent repellent

66 parts by weight of the carrier mixture prepared in Preparation Example 4 was mixed with 100 parts by weight of the perilla extract prepared in Preparation Example 1, stirred for 6 hours, filtered and dried to prepare a carrier mixture on which the perilla extract was supported, After mixing 3 parts by weight of the carrier mixture on which the perilla extract is supported in 100 parts by weight of a resin mixture (100 parts by weight of linear low-density polyethylene and 30 parts by weight of ethylene vinyl acetate), it is extruded with an extruder to use antibacterial and rodent avoidance master batches was prepared.

Example 3: Preparation of masterbatch for antibacterial and rodent repellent

Antibacterial using icosane in the same manner except that a solution obtained by dissolving icosane at a concentration of 10 mg/mL with acetone instead of the perilla extract of Example 2 was used at a concentration of 1,000 ppm with distilled water at a concentration of 10 parts by weight. And a master batch for repelling rodents was prepared.

Example 4: Preparation of masterbatch for antibacterial and rodent repellent

In the same manner except that a solution obtained by dissolving perylaldehyde at a concentration of 10 mg/mL with DMSO (dimethyl sulfoxide) instead of the perilla extract of Example 2 was used at a concentration of 1,000 ppm at a concentration of 10 parts by weight with distilled water. A masterbatch for antibacterial and rodent repellent was prepared using icosan.

Example 5: Measurement of antibacterial activity of masterbatch for antibacterial and rodent repelling

The antibacterial activity of the masterbatch prepared in Example 2 was measured and shown in Table 3 below.

{However, the antibacterial activity of the masterbatch was evaluated by requesting the SGS Korea test institute, and the '4. A method of evaluating the antibacterial activity of various bacterial groups, including the number of general bacteria, was used according to the 'microbiological test method'.

In more detail, including the number of general bacteria, E. coli, Escherichia coli, Salmonella, Listeria monocytogenes, Clostridium perfringens, Staphylococcus aureus, Campylobacter jejuni, enterohaemorrhagic Escherichia coli, Yersinia enterocolica, enteritis vibrio, and Quantitative and qualitative analysis was performed on Bacillus cereus.}

division			Classification of tests	result	unit
One	TPC	general number of bacteria	dose	0	cfu/g (mL)
2	Coli Forms Count	coliform	dose	0	cfu/g (mL)
3	E. Coli Count	coli	dose	0	cfu/g (mL)
4	Salmonella	Salmonella	Qualitative	voice	**
5	Listeria monocytogenes	Listeria monocytogenes	Qualitative	voice	**
6	Clostridium perfringens	Clostridium perfringens	Qualitative	voice	**
7	Clostridium perfringens Count	Clostridium perfringens	dose	0	cfu/g (mL)
8	S. Aureus	Staphylococcus aureus	Qualitative	voice	**
9	S. Aureus Count	Staphylococcus aureus	dose	0	cfu/g (mL)
10	Campylobacter jejuni /coli	Campylobacter jejuni / coli	Qualitative	voice	**
11	EHEC	enterohemorrhagic Escherichia coli	Qualitative	voice	**
12	Yersinia	Yersinia Enterocolica	Qualitative	voice	**
13	Vibrio parahaemolyticus	enteritis vibrio	Qualitative	voice	**
14	Vibrioa parahaemolyticus Count	enteritis vibrio	dose	0	cfu/g (mL)
15	Bacillus cereus	bacillus cereus	Qualitative	voice	**
16	Bacillus cereus Count	bacillus cereus	dose	0	cfu/g (mL)

As shown in Table 3, the masterbatch containing the active ingredient of the perilla extract is E. coli group, E. coli, Salmonella, Listeria monocytogenes, Clostridium perfringens, Staphylococcus aureus, Campylobacter jejuni, enterohaemorrhagic Escherichia coli, Yeoshi It was found that it exhibited excellent antibacterial properties against nia enterocolica, enteritis vibrio and Bacillus cereus.

In addition, a film was prepared using the masterbatch prepared in Example 1, and the antibacterial activity of the film was measured by requesting a FITI testing institute, and it was carried out according to the test method of JIS Z 2801:2010, and the results were It is shown in Table 4 below. Specifically, a 5cm×5cm test piece and a 5cm×5cm control piece (Stomacher ^® 400 POLY BAG) were used. in RH environment for 24 hours determine the bacterial concentration of the after culturing was used how to determine antibacterial hwalseongchi, using strain was as Staphylococcus aureus using Staphylococcus aureus ATCC6538P, inoculum was injected at a concentration of 1.4 × 104CFU / mL did.

division	contrast	test piece
Initial number of bacteria	1,4×10 4	1,4×10 4
after 24 hours	2,4×10 4	1,2×10 4
Antibacterial activity (%)	-	99.5

As shown in Table 4, it was found that the film using the masterbatch containing the perilla extract of the present invention also exhibited excellent antibacterial activity.

On the other hand, although not specifically described herein, the masterbatch containing icosane and perylaldehyde of Examples 3 and 4 and a film prepared using the same also exhibited excellent antibacterial activity.

Therefore, the method for producing a masterbatch for antibacterial and rodent avoidance using perilla extract, icosane, or perylaldehyde according to the present invention contains not only antibacterial effect but also an effect of inhibiting access of rodents to various synthetic resin products by containing perilla extract. It provides a master batch and resin using the same.

Claims (19)

1. An antibacterial composition comprising as an active ingredient one or two or more selected from the group consisting of icosan (eicosane), a salt of icosan, perylaldehyde, and a salt of perylaldehyde.
2. According to claim 1, wherein the antimicrobial composition is selected from the group consisting of Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, and metacillin-resistant Staphylococcus aureus (Staphylococcus aureus subsp. aureus). An antibacterial composition having antibacterial activity against one or more bacteria.
3. A product comprising the antibacterial composition of any one of claims 1 or 2.
4. The product according to claim 4, wherein the product is a packaging film, packaging container or packaging material.
5. Characterized in that it consists of a resin mixture, and a carrier mixture on which one or more substances selected from the group consisting of perilla extract, eicosane, icosan salt, perillaldehyde, and perylaldehyde salt are supported. Masterbatch composition for antibacterial and rodent repellent.
6. According to claim 5, wherein the antibacterial and rodent repellent masterbatch composition is 100 parts by weight of a resin mixture and perilla extract, icosan (eicosane), a salt of icosan, perylaldehyde (perillaldehyde), and the group consisting of a salt of perylaldehyde Antibacterial and rodent repellent masterbatch composition, characterized in that it consists of 2 to 4 parts by weight of a carrier mixture on which one or more substances selected from among are supported.
7. [Claim 6] The masterbatch composition for antibacterial and rodent repelling according to claim 5, wherein the resin mixture comprises 100 parts by weight of linear low-density polyethylene and 10 to 50 parts by weight of ethylene vinyl acetate.
8. According to claim 5, wherein the perilla extract, icosane (eicosane), icosan salt, perylaldehyde (perillaldehyde), and the carrier mixture on which one or more substances selected from the group consisting of peryl aldehyde salt is supported is a perilla extract , icosan (eicosane), icosane salt, perylaldehyde (perillaldehyde), and at least one material selected from the group consisting of perylaldehyde salts 100 parts by weight of the carrier mixture 60 to 70 parts by weight characterized in that A masterbatch composition for antibacterial and rodent repelling.
9. [Claim 6] The masterbatch composition for antibacterial and rodent repelling according to claim 5, wherein the carrier mixture is prepared by mixing 10 to 1000 parts by weight of montmorillonite with improved interlayer spacing in 100 parts by weight of crystalline calcium carbonate.
10. The antibacterial and antibacterial and A masterbatch composition for repelling rodents.
11. The method of claim 9, wherein the montmorillonite with improved interlayer spacing is mixed with 100 parts by weight of a 0.2 mol/L montmorillonite solution and 30 to 50 parts by weight of a 0.2 mol/L polyethylene glycol solution and stirred for 3 to 5 hours and then dried. A masterbatch composition for antibacterial and rodent repelling, characterized in that it is prepared by
12. 12. An antibacterial and rodent repelling resin composition, characterized in that it contains the antimicrobial and rodent repelling masterbatch composition according to any one of claims 5 to 11.
13. An extract/composition preparation step of preparing a perilla extract or preparing the antibacterial composition of claim 1;

    Carrier mixture preparation step of mixing calcium carbonate and montmorillonite;

    A supporting step of supporting the perilla extract and/or the prepared antibacterial composition through the extract/composition preparation step on the carrier mixture prepared through the carrier mixture preparation step;

    A raw material mixing step of mixing the perilla extract and/or the prepared antibacterial composition through the supporting step in the resin mixture, the carrier mixture; and

    An extruding step of extruding the mixture prepared through the raw material mixing step;
14. [Claim 14] The method of claim 13, wherein the preparation of the carrier mixture comprises mixing 10 to 1000 parts by weight of montmorillonite with improved interlayer spacing in 100 parts by weight of crystalline calcium carbonate.
15. 16. The antibacterial and antibacterial and A method for producing a masterbatch for repelling rodents.
16. The method of claim 15, wherein the montmorillonite with improved interlayer spacing is mixed with 100 parts by weight of a 0.2 mol/L montmorillonite solution and 30 to 50 parts by weight of a 0.2 mol/L polyethylene glycol solution and stirred for 3 to 5 hours and then dried. A method for producing a masterbatch for antibacterial and rodent avoidance, characterized in that it is manufactured by
17. According to claim 13, wherein the supporting step is a mixture of 60 to 70 parts by weight of the carrier mixture prepared through the carrier mixture preparation step with 100 parts by weight of the perilla extract and/or the prepared antibacterial composition prepared through the extract/composition preparation step And after stirring for 5 to 7 hours, the method for producing a masterbatch for antibacterial and rodent repellent, characterized in that made by filtration and drying.
18. The antibacterial and rodent according to claim 13, wherein the raw material mixing step is made by mixing 0.5 to 5 parts by weight of the carrier mixture on which the perilla extract and/or the antibacterial composition are supported through the supporting step with 100 parts by weight of the resin mixture. Method for producing a masterbatch for avoidance.
19. The method of claim 13 or 18, wherein the resin mixture comprises 100 parts by weight of linear low-density polyethylene and 10 to 50 parts by weight of ethylene vinyl acetate.

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