KR102274105B1 - Tree injection composition for controlling fire blight comprising oxolinic acid having soluble concentrate type as effective component and uses thereof - Google Patents

Abstract

The present invention relates to a composition for stem injection for controlling fire blight, including an oxolinic acid having liquid formulation as an active ingredient, and a method for controlling fire blight, including the step of stem-injecting the composition into a plant. The oxolinic acid liquid formulation according to the present invention can be usefully used to reduce the spread of domestic fire blight and damage caused thereby.

Description

A composition for tree injection for controlling fire blight and its use comprising oxolinic acid having a liquid formulation as an active ingredient, and uses thereof

The present invention relates to a composition for bestial injection for controlling fruit tree burns, comprising oxolinic acid having a soluble concentrate formulation as an active ingredient, and a method for controlling fruit tree burns using the composition.

Fruit tree burn disease, which has been pointed out that there is a high possibility that pathogens may have been introduced into Korea due to the presence of pathogens in foreign agricultural products, which have increased imports since the conclusion of the Free Trade Agreement (FTA), may restrict the import and export of related fruit trees and agricultural products to countries with the disease. In addition, in the case of endemic orchard farms, it is a plant disease that can cause a ripple effect on national agriculture and economy by causing economic losses to farms, such as removal of host plants, burial of the range of nearby occurrence areas, and orchard closures.

In the case of domestic burn disease, it was first discovered in a new pear variety in a pear orchard in Anseong in 2015, and spread to 4 provinces and 6 cities and counties in 2018. In 2019, it occurred in 180 farms nationwide and 127ha orchards were buried. Occurs in Anseong (13), Paju (1), Icheon (5), Yongin (1), Wonju (2), Jecheon (62), Chungju (76), Eumseong (7), and Cheonan (10) by city and county As the area tends to expand gradually, the number of farm households is likely to increase in the future, so countermeasures are urgently needed.

Fire blight is one of the representative bacterial plant quarantine diseases, and Erwinia amylovora has been identified as the causative bacterium, and it chars the flowers, branches, and fruits of pears or apple trees as if they were burned. It is called burn disease in Korea because it kills it. Erwinia amylobora is highly contagious because it is transmitted by insects or rain and wind and invades the host through flowers, nectar, pores, bark, and wounds. There is a characteristic that there is damage to burn diseases worldwide.

Burn disease not only spoils the harvest of the year, it can also cause long-term damage. Infection of flowers can cause fruit to dry out, reducing the current harvest and burns of young shoots reduce the likelihood of the following year's fruit opening. In the roots and trunks of many fruit tree varieties, burns can destroy large branches or even entire trees. Given the potential impact of burn disease on fruit tree harvests, a solution to this disease is urgently needed.

One of the ways to combat burn disease is to minimize the incidence of disease by horticultural practices. For example, there are ways to control the infection and spread of burn disease by reducing soil moisture and balancing fertilizer nutrients. However, this method cannot eliminate the underlying disease occurrence. Alternatively, it is possible to treat burn disease by removing infected fruit trees or blackened branches in the winter, when the pathogens have a dormant period. However, in these methods, care must be taken to sterilize the equipment to prevent the spread of disease. Also, this method cannot completely eradicate the disease because it cannot detect all small lesions or internal infections.

In addition, burn-infected fruit trees can be controlled by regular spraying of copper compounds or antibiotics. However, the use of copper compounds is often ineffective or causes fruit russeting, making it difficult to use universally. The use of antibiotics, especially streptomycin, is more effective than copper compounds and less harmful to fruits. However, since Erwinia amylobora is developing resistance to streptomycin in many states in the United States, including California, Oregon, Washington, Missouri, and Michigan, where streptomycin is used, another method is needed.

On the other hand, Korean Patent No. 2025411 discloses 'a novel bacteriophage φEaP-21 effective against fruit tree burn disease bacteria and its use', and Korean Patent No. 1954392 discloses 'Molecular marker for detecting Erwinia amylobora and its use'. Although the 'use' is disclosed, there is no description of 'a composition for bestial injection for the control of fruit tree burn disease comprising oxolinic acid having a soluble concentrate formulation as an active ingredient and its use' of the present invention. .

The present invention has been derived from the above needs, and the present inventors have developed oxolinic acid, which is hardly soluble in water or organic solvents, as a drug for bestial injection for the control of fruit tree burns. As a result of formulating in a soluble concentrate formulation using an ionic surfactant, etc., and treating the oxolinic acid solution with a stem injection into a tree affected by fruit tree burn disease, the number of branches onset of burn disease did not increase, resulting in 100% control effect By confirming that there is, the present invention was completed.

In order to solve the above problems, the present invention provides a composition for treatment for head injection for controlling fruit tree burns, comprising oxolinic acid having a soluble concentrate formulation as an active ingredient.

In addition, the present invention provides a method for controlling fruit tree burns, comprising the step of injecting the composition to a plant suspected of having a fruit tree burn disease or a plant expected to develop a fruit tree burn disease.

In the present invention, oxolinic acid, which is only a formulation in which the original particle is present in a solid phase, because of its low solubility, was formulated as a liquid formulation capable of intermittent injection. Considering the characteristics of fruit tree burns that damage trees in the form of propagating within the tissues of plants and blocking the xylem and phloem, compared to the method of treating the drug in the form of a spray for the control of fruit tree burns, the It is expected that fruit tree burn disease can be controlled more effectively by treating the oxolinic acid solution with head injection.

In order to achieve the object of the present invention, the present invention provides a composition for treatment for head injection for controlling fruit tree burns, comprising oxolinic acid having a soluble concentrate formulation as an active ingredient.

As used herein, the term "soluble concentrate (SL)" refers to a liquid formulation that is dissolved when diluted in water, and a liquid or viscous liquid, which is a formulation that is hydrated when diluted in water (suspension concentrate, SC). ) is clearly different from

As used herein, the term "trunk injection (tree injection)" is a type of medical treatment for treating tree diseases, and is a method of inserting an injection or puncturing a tree trunk so that a drug can be injected.

In the composition for treatment of bestial injection of the present invention, the liquid agent may be composed of an oxolinic acid raw agent, a solubilizer, a surfactant, a stabilizer, a cryoprotectant, and an extender, but is not limited thereto.

In addition, in the composition of the present invention, the oxolinic acid raw agent and the solubilizing agent may be used in a weight ratio of 5 to 7: 1, preferably, the oxolinic acid raw agent and the solubilizing agent may be in a weight ratio of 5.5 to 6.5: 1, more preferably Preferably, the oxolinic acid raw agent and the solubilizing agent may be used in a weight ratio of 6:1, but is not limited thereto.

In the composition for treatment of bestial injection according to an embodiment of the present invention, the oxolinic acid raw agent may be 0.1 to 20% by weight based on the total weight of the oxolinic acid liquid formulation, but is not limited thereto.

In the composition for treatment of bestial injection according to an embodiment of the present invention, the solubilizing agent may preferably be sodium hydroxide, but is not limited thereto.

In addition, in the composition for treatment of bestial injection of the present invention, the surfactant may be a nonionic surfactant, preferably a nonionic surfactant with a hydrophilic-lipophilic balance (HLB) value of 8 to 16, and more Preferably, it may be a nonionic surfactant having an HLB value of 11 to 13, but is not limited thereto. In addition, the type of the nonionic surfactant is not limited thereto, but polyoxyalkylene styrenated phenyl ether, polyoxyalkylene natural oil, polyoxyalkylene fatty alcohol ( polyoxyalkylene fatty alcohol or polyoxyalkylene fatty acid.

When an ionic surfactant is used as a surfactant when preparing an oxolinic acid liquid formulation, crystals are formed and precipitated in the oxolinic acid liquid formulation.

In the composition for treatment of bestial injection of the present invention, the surfactant may be included in an amount of 1 to 10% by weight based on the total weight of the oxolinic acid solution, preferably 3 to 7% by weight based on the total weight of the oxolinic acid solution, More preferably, it may be included in an amount of 4 to 6% by weight based on the total weight of the oxolinic acid liquid formulation, but is not limited thereto.

In addition, in the composition for treatment of bestial injection according to an embodiment of the present invention, the stabilizer may be a mixture of sorbitol (D-sorbitol) and water, and maintain dilution stability by inhibiting crystal formation upon dilution of the oxolinic acid solution function to help you do it.

In addition, in the composition for bestial injection treatment of the present invention, the cryoprotectant prevents the oxolinic acid solution from freezing at low temperatures (-5°C), and even if frozen (-10°C), when the temperature rises above 0°C, Oxol It plays a role in helping the lyric acid solution to defrost quickly.

In the composition for bestial injection treatment according to an embodiment of the present invention, the cryoprotectant may preferably be propylene glycol, but is not limited thereto, and the cryoprotectant is 5 to 5 to the total weight of the oxolinic acid solution. It may be included in an amount of 20% by weight, but is not limited thereto.

The oxolinic acid liquid formulation according to the present invention is a formulation in which oxolinic acid is completely dissolved in water, and the advantage is that it is in a form that can be injected into the trunk (tree injection).

The present invention also provides a method for controlling an orchard burn disease, comprising the step of injecting the head of the composition for treatment of a trunk injection according to the present invention to a plant suspected of having a fruit tree burn disease or a plant expected to develop a fruit tree burn disease.

Currently, the method registered and used by the Rural Development Administration for the control of fruit tree burns is to dilute the drug in water and spray it. Due to the nature of the fruit tree burn disease caused by bacterial pathogens, since they are infected by bees during the flowering period, there are not many pathogens exposed to the outside, and they multiply within the plant tissue and cause damage to trees in the form of blocking the xylem and phloem. Therefore, there is a limit to the spray type control method.

The composition according to the present invention is a liquid formulation in which oxolinic acid is completely dissolved in water, and since it is a form that can be injected into a tree, it can be effectively injected into a plant suspected of having an orchard burn disease or a plant that is expected to develop an orchard burn disease. It can treat and prevent fruit tree burn disease.

In the control method according to the present invention, the stem injection method may be treated on a plant using equipment (device) or method for stem injection known in the art, but is not limited thereto, for example, a sap injection set may be used. can The infusion injection set is easy for a user to purchase and has a large size of a syringe hole, so it is easy to inject.

In addition, the dose of the oxolinic acid liquid formulation to be treated may be appropriately selected by those skilled in the art according to the level or purpose (eg, prevention) of fruit tree burn disease of the plant to be treated.

Hereinafter, the present invention will be described in detail by way of Examples. However, the following examples only illustrate the present invention, and the content of the present invention is not limited to the following examples.

Example 1. Development of oxolinic acid formulation suitable for bestial injection

The aqueous solubility of the oxolinic acid raw material is 3.2 mg/L (25°C), and the solubility in organic solvents is known to be <10 g/kg (20°C) in hexane, xylene, or methanol, etc. have.

Due to the characteristics of oxolinic acid raw materials that are hardly soluble in water or organic solvents, soluble concentrates (SL), emulsifiable concentrates (EC), dispersible concentrates (DCs) are formulations made by dissolving the raw materials in a solvent. ), microemulsion (ME), emulsion (emulsion, oil in water, EW), and suspo-emulsion (SE) products could not be developed. wettable powder, WP), water dispersible granule (WG), suspension concentrate (SC), and oil dispersion (OD), in which the original particles are in a solid state (Rural Development Administration-National Academy of Agricultural Sciences) _Pesticide information site).

The present inventors prepared an oxolinic acid aqueous solution and an oxolinic acid liquid formulation, respectively, to develop an oxolinic acid formulation suitable for bestial injection.

1-1. Preparation of oxolinic acid suspension concentrate (SC)

The aqueous oxolinic acid liquid is dispersed by adding and dispersing the original agent, surfactant, and antifoaming agent to water, which is an extender, and then coarsely pulverized with a homogenizer, and then finely pulverized with a wet mill containing zirconia beads.微粉碎) to prepare a liquid wettable powder intermediate agent (原劑中間劑). To prepare a thickener, an anti-freezing agent, a thickener, and a preservative are added to water, which is an extender, and stirred, and the thickener is released and becomes a viscous liquid. An oxolinic acid liquid wettable powder was prepared by mixing the above original agent intermediate and a thickener.

Composition of oxolinic acid liquid wettable powder Usage Ingredients water
(%) 10% SC 20% SC Buy-in rate (%) Buy-in rate (%) original title Oxolinic acid 94.7 10.3 21.0 Surfactants Triethanol amine, compound. with poly(oxyethylene)tristyrylphenyl ether phosphate
Polyoxyethylene-polyoxypropylene copolymer
propylene glycol 2.0 2.0 Surfactants Methacrylic acid -methyl methacrylate polyethylene glycol methyl ether methacrylate copolymer
propylene glycol
Water 6.0 6.0 Surfactants Polyoxyethylene-polyoxypropylene copolymer 0.5 0.5 cryoprotectant propylene glycol 5.0 5.0 thickener Xanthan gum 0.1 0.05 antifoam Silicones and siloxanes, dimethyl 0.3 0.3 antiseptic 1,2-Benzisothiazolin-3-one 0.1 0.1 extender Water Rest Rest system 100.0 100.0

1-2. Preparation of oxolinic acid solution (soluble concentrate, SL)

The oxolinic acid liquid formulation was prepared according to the composition of Table 2 or Table 3 below. The oxolinic acid raw material with low solubility was dissolved by dissolving sodium hydroxide (NaOH), a solubilizing agent, in water first, and then the oxolinic acid raw material was added and stirred while stirring. Potassium hydroxide (KOH) can also be used as the solubilizing agent, but sodium hydroxide has more advantages in terms of corrosiveness and price, so sodium hydroxide was selected as the solubilizing agent in the present invention. As shown in the table below, when preparing a 10% solution of oxolinic acid, 1.9 g of sodium hydroxide was first dissolved in 50 ml of water, and then 10.88 g of the original oxolinic acid was added and dissolved. When preparing a 20% oxolinic acid solution, 3.7 g of sodium hydroxide was first dissolved in 40 ml of water, and then 22.18 g of the original oxolinic acid was added and dissolved. The stabilizer is a mixture of D-sorbitol and water, and a liquid product with a mixing ratio of sorbitol and water of 7:3 was used.

Composition of 10% oxolinic acid solution Usage Ingredients water
(%) buy rate
(%) remark original title Oxolinic acid 94.7 10.3 Surfactants Polyoxyalkylene styrenated phenyl ether 5.0 HLB 13 solvent Sodium hydroxide (NaOH) 1.9 stabilizator D-sorbitol
Water 10.0 cryoprotectant propylene glycol 15.0 extender Water rest system 100.0

Composition of 20% oxolinic acid solution Usage Ingredients water
(%) buy rate
(%) remark original title Oxolinic acid 94.7 21.0 Surfactants Polyoxyalkylene styrenated phenyl ether 5.0 HLB 13 solvent Sodium hydroxide (NaOH) 3.7 stabilizator D-sorbitol
Water 10.0 cryoprotectant propylene glycol 15.0 extender Water rest system 100.0

Example 2. Bestial injection experiment according to the formulation

In order to check whether the oxolinic acid liquid wettable powder (SC) and liquid formulation (SL) prepared in Example 1 can be treated with a head injection, a 10 ml tip was drilled diagonally by using a wooden drill to a depth of 3 to 4 cm. The drug was inserted into the hole and the drug was injected in an amount of 1 ml per cm of chest height, and after 30 minutes, it was judged whether the drug was injected. In relation to the control of overwater burn disease, a previously registered drug (drug A, formulation-liquid) was used as a comparative control group.

As a result, as shown in Table 4 below, commercially available oxolinic acid liquid hydrating agents (Dongbang Agro Co., Ltd., product name: Ilpum) and oxolinic acid liquid hydrating agents formulated in the present invention are not injected at all or have poor injection quality. was confirmed to be On the other hand, it was confirmed that the oxolinic acid solution formulated in the present invention and the drug A, which is a registered drug, had excellent injection.

Results of analysis on whether or not to inject the bestial injection according to the dosage form test drug LOT. NO Main ingredient content (%) Injection availability ^* Oxolinic acid SL (formulation) DBA-OA10SL-200428-01 10 ○ Oxolinic acid SL (formulation) DBA-OA10SL-200428-02 10 ○ Oxolinic acid SC (formulation) DBA-OA20SC-200318 20 × Oxolinic acid SC (formulation) DBA-OA10SC-200317 10 × Oxolinic Acid Liquid Hydrating Agent 20 × Drug A 2.3 ○ * Whether injection is possible is judged by checking the amount or precipitation of the drug remaining in the 10 ml tip.

Through the above results, it was confirmed that the oxolinic acid liquid formulation was suitable for bestial injection, and an orchard burn disease control experiment was conducted using the formulation.

Example 3. Test of control effect of oxolinic acid solution on apple burn disease

The efficacy of the drug was tested using the oxolinic acid solution confirmed that bestial injection was possible through Example 2 above. The experiment was conducted in the field of an apple farm in Anseong-si, Gyeonggi-do, where an apple burn disease occurred due to Erwinia amylovora infection as a result of the diagnosis of the Rural Development Administration. There were a few cases where the The experiment consisted of an experimental group and an untreated control group each treated with the oxolinic acid solution formulated in the present invention and the comparative control, Drug A (Table 5 and Table 6). Efficacy was evaluated by examining the number of branches with increased burn disease on the basis of stock branches after 8 days of drug treatment.

Test processing content test drug Main ingredient content (%) Dilution factor and dosage When and how to process oxolinic acid solution 10 Stock solution 0.5ml/
Diameter at breast height (cm) immediately after onset
bestial injection
(06/22) Drug A 2.3 Stock solution 0.1ml/
Diameter at breast height (cm) Stock solution 0.2ml/
Diameter at breast height (cm) unprocessed - - -

Test plot layout and area division treated water number of repetitions muzzle number medicinal effect 4 5 20 weeks

(Test group: 5 repetitions of complete randomization method, untreated group: 3 repetitions of completely random placement method)

As a result, when 0.1 ml or 0.2 ml of drug A was injected per breast height, 78.2% and 83.7% of control effects were confirmed, respectively, and when 0.5 ml of oxolinic acid solution was injected per breast height, additional burns occurred after drug treatment As the number did not increase, it showed 100% control effect (Table 7).

Control effect of oxolinic acid solution test drug Main ingredient content (%) Increased number of burn diseases after drug treatment Control (%) I II Ⅲ Ⅴ Ⅵ Average oxolinic acid solution 10
[0.5ml/diameter at breast height (cm)] 0 0 0 0 0 0 100.0 Drug A 2.3
[0.1ml/diameter at breast height (cm)] 0 0 2 2 0 0.8 78.2 2.3
[0.2ml/diameter at breast height (cm)] 0 One One One 0 0.6 83.7 unprocessed 5 2 4 - - 3.67 -

Through these results, it was predicted that the oxolinic acid solution formulated in the present invention could be usefully used for interstitial injection for the control of overwater burns.

Claims (7)

A composition for treatment of bestial injections for controlling fruit burns, comprising oxolinic acid having a soluble concentrate (SL) formulation as an active ingredient,
The liquid formulation is an oxolinic acid raw agent, sodium hydroxide, and a nonionic hydrophilic-lipophilic balance (HLB) value of 8 to 16. It consists of a surfactant, a stabilizer, an anti-freezing agent and an extender,
The oxolinic acid base agent is 0.1 to 20% by weight relative to the total weight of the liquid formulation, the oxolinic acid base agent and sodium hydroxide are in a weight ratio of 5 to 7: 1, and the nonionic surfactant is 1 to 10% by weight based on the total weight of the liquid formulation, The composition for treatment of head injection, characterized in that the stabilizer is a mixture of sorbitol and water. delete delete delete delete delete A method for controlling fruit tree burns, comprising the step of injecting the composition of claim 1 to a plant suspected of having a fruit tree burn disease or a plant expected to develop a fruit tree burn disease.