KR20030037989A - Insecticidal compositions containing cyromazine and deltamethrin as an effective ingredient - Google Patents

Abstract

PURPOSE: Provided is an insecticide composition containing, as an ingredient, cyromazine and deltamethrin which removes the larva and imago of insect pests, thereby effectively killing mosquitos and flies. CONSTITUTION: The insecticide composition contains 0.1 to 20% by weight of cyromazine of the formula(1), 0.1 to 20% by weight of deltamethrin of the formula(2), 0.1 to 99% by weight of a carrier and 0.1 to 10% by weight of a surfactant. The mixing ratio of cyromazine and deltamethrin is 1:1 to 1:10. The composition is directly sprayed on a livable habitat for insect pests in an amount of 10 to 50mg/m¬2 or added to animal feeds or animal excrement.

Description

Insecticide composition containing cyro-margin and deltamethrin as active ingredient {INSECTICIDAL COMPOSITIONS CONTAINING CYROMAZINE AND DELTAMETHRIN AS AN EFFECTIVE INGREDIENT}

The present invention between the margin (cyromazine) and deltamethrin (deltamethrin) the present invention relates to pesticide compositions, as an active ingredient, in particular larvae relief agent to to Jane adult relief and margin from 0.1 to 10% between the represented by the general formula (1) formula (2) The present invention relates to a pesticide composition prepared by mixing 0.1 to 99% of a carrier and 0.1 to 10% of a surfactant with a suitable excipient in 0.1 to 10% of deltamethrin, and a method of controlling pests using the same.

<Formula 1>

<Formula 2>

Insecticides generally consist of a composition containing one pesticidal active ingredient and a composition containing two or more pesticidal active ingredients. In the case of containing one pesticide component shows a single efficacy, the pesticide prepared by using two or more components has been widely used because it shows an excellent efficacy than a single agent. However, such a mixed agent generally has a problem in stability because the active ingredient can be decomposed when a long time after the preparation.

Cyromazine (C ₆ H ₁₀ N ₆ , molecular weight 166.19) is a triazine-based chitin synthesis inhibitor developed by Ciba-Geigy (Switzerland, now merged with Novartis). CGA-19255, CGA-34296 and CGA-72662 are known. CGA-72662 (cyromazine; N-cyclopropyl-1,3,5-triazine-2,4,6-triamine), first discovered in 1978, is CGA-19255 (azidotriazine; 6-azido-N-cyclopropyl-N'-ethyl -1,3,5-triazine-2,4-diamine was metabolized by two steps of azide reduction and N-deethylation. Has the strongest toxicity.

Cyroma margins have been used to control flies and maggots by treating them with feces or feed, as they are effective against bicot pests. In particular, when flies are severely added to the laying hen's feed during the summer months, flies can be discharged into the poultry to kill maggots present in the minute, thereby preventing flies from occurring. The substance is currently marketed worldwide by Novartis Corporation under the trade name Larvadex, approved by the US Food and Drug Administration (FDA) and the Environmental Protection Agency (EPA) for use in poultry feed. It is used in various animal breeding methods, such as spraying and a bath.

Deltamethrin (C ₂₂ H ₁₉ Br ₂ NO ₃ , Molecular Weight 505.2) is a pyrethroid insecticide, a photostable insecticide commercially produced since 1982 synthesized by Elliott in 1974. (Flavio et al., 1999, J Agric Food Chem, 47, 174-176). Pyrethroid insecticides are divided into two types: insecticides of type I (Allethrin, tetramehtrin, resmethrin) without cyano groups in the carboxyl alpha position and cyano groups in the carboxyl alpha position. Type II (Cypermethrin, deltamethrin) is divided into insecticides. Among them, deltamethrin is known to have 10 times or more excellent insecticidality compared to the first generation pyrethroid such as Permethrin (Flavio et al., 1999, J Agric Food Chem, 47, 174-176).

As described above, cyromargin is a pesticide for controlling larvae by suppressing larvae, and pyrethroid-type insecticides such as deltamethrin are insecticides for controlling adults, and two components are widely used in various fields. However, only exterminating larvae and adults of pests poses a limit to the fundamental control of pests.

The present inventors have completed the present invention by developing a pesticide composition that can control not only the larvae of insects but also the adult by mixing the appropriate excipients containing cyromargin and deltamethrin as an active ingredient.

It is an object of the present invention to provide an insecticide composition which can effectively control both adult and larvae of pests.

1 is a comparison of the sustained insecticidal effect on the housefly adult of the single formulation containing only deltamethrin and the mixed formulation containing deltamethrin and cyro-margin,

a: deltamethrin alone

b: Deltamethrin + Cyromargin Mixture

FIG. 2 compares the sustained insecticidal effects of adult adult red-colliders of a single formulation containing only deltamethrin and a mixed formulation containing deltamethrin and cyromargin.

a: deltamethrin alone

b: Deltamethrin + Cyromargin Mixture

In order to achieve the above object, the present invention provides a pesticide composition prepared by mixing the siroma margin and deltamethrin as an active ingredient and a suitable excipient thereto.

In addition, the present invention provides a method for simultaneously controlling the adult and larvae of pests using the pesticide composition.

Hereinafter, the present invention will be described in detail.

The present invention provides a pesticide composition prepared by mixing cyromargin and deltamethrin as an active ingredient and a suitable excipient thereto.

The pesticide composition of the present invention comprises 0.1-20% of cyromargin, 0.1-20% of deltamethrin, 0.1-99% of carrier and 0.1-10% of surfactant with suitable excipients.

The mixture ratio of deltamethrin and cyromargin may be in the range of 1: 1 to 1:10 by weight.

The carrier in the composition according to the present invention may be any material as long as it facilitates application of the active ingredient to the desired site, or facilitates storage, or facilitates transport or manipulation. The carrier is usually a gas, but may be liquid or solid, including materials compressed to form a liquid, and any carrier commonly used to form the pesticide composition may be used.

Suitable solid carriers include natural and synthetic clays and silicates such as natural silica such as diatomaceous earth; Magnesium silicates such as talc; Magnesium aluminum silicates such as etherpulzite and vermiculite; Aluminum silicates such as kaolinite, montmorillonite and mica; Calcium carbonate; Calcium sulfate; Ammonium sulfate; Synthetic hydrated silicon oxides and synthetic calcium or aluminum silicates; Elements such as carbon and sulfur; Natural and synthetic resins such as coumarone resins, polyvinyl chloride and styrene polymers and copolymers; Solid polychlorophenols; bitumen; Waxes; And solid pesticides such as superphosphates.

Suitable liquid carriers include water; Alcohols such as isopropanol and glycols; Ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone and cyclohexanone; Ethers; Aromatic or araliphatic hydrocarbons such as benzene, toluene and xylene; Pertrolium fractions such as kerosine and light mineral oils; Chlorinated hydrocarbons such as carbon tetrachloride, perchloroethylene and trichloroethane; and the like.

Pesticide compositions of the present invention are often formulated and distributed in concentrated form and can be diluted by the user prior to use. The presence of a small amount of carrier, a surfactant, facilitates this dilution process. Therefore, at least one of the carriers used in the composition according to the invention is preferably a surfactant. For example, the composition may contain at least two carriers, at least one of which is a surfactant.

The surfactant may be an emulsifier, dispersant or moisturizer and the surfactant may be ionic or nonionic. Examples of suitable surfactants include sodium or calcium salts of polyacrylic acid and lignin sulfonic acid; Condensation products of fatty acids or aliphatic amines or amides containing at least 12 carbon atoms in a molecule with ethylene oxide and / or propylene oxide; Fatty acid esters of glycerol, sorbitan, sucrose or pentaerythritol; Ethylene oxide and / or propylene oxide and their condensates; fatty alcohols or alkyl phenols such as condensation products of p-octylphenol or p-octylcresol with ethylene oxide and / or propylene oxide; Sulfates or sulfonates of these condensation products; Alkali or alkaline earth metal salts of sulfuric acid or sulfonic acid esters containing at least 10 carbon atoms in the molecule, preferably sodium salts such as sodium lauryl sulfate, secondary alkyl sodium sulfate, sodium salts of sulfonated castor oil, and dodecylbenzene sulfo Sodium alkylarylsulfonates such as nates; And polymers of ethylene oxide and copolymers of ethylene oxide and propylene oxide.

The compositions of the present invention may be formulated, for example, as wettable powders, dusts, granules, solutions, emulsifiable concentrates, emulsions, emulsion concentrates, suspension concentrates and wetting agents, aerosols.

The composition of the present invention may also contain a mixture of other compounds having other herbicidal, pesticidal or fungicidal properties, for example.

Insecticide composition of the present invention has an improved insecticidal effect that is effective for the control of the larvae as well as the larvae of insects by containing the cyro margin and deltamethrin as an active ingredient.

As a result of investigating the insecticidal properties of the formulation of the pesticide composition of the present invention, the formulation containing both cyromargin and deltamethrin at the same time than the formulation containing only the cyromarine or deltamethrin alone showed improved insecticidal activity for both the adult and the larvae of the pest. It was. Therefore, the insecticide composition containing the cyromargin and the deltamethrin of the present invention as an active ingredient exhibits a very effective insecticidal effect not only for the flies and mosquitoes but also for the larvae, and thus may be useful for controlling flies and mosquitoes.

In addition, the present invention provides a method for simultaneously controlling the adult and larvae of pests using the pesticide composition.

The insecticide composition of the cyclomargin and deltamethrin mixed formulations of the present invention can be effectively used for the control of double-pest pests. Specifically, flies such as house flies, cow flies, moth flies, tsetse flies and red mosquitoes such as chicken mosquitoes It can be useful for controlling both adult and larvae of pests such as mites, fleas, and the like.

Insecticide composition of the present invention can be directly sprayed on the habitat of the pest or added to the feces or feed of livestock to control flies or maggots, especially when added to laying hens for long-term administration is discharged as a poultry killing maggots present in the minutes The occurrence of flies can be prevented at the source. In addition to the method of addition in the feed can be controlled at the same time the adult and larvae of pests by spraying, bathing around the barn. At this time, the effective amount of the pesticide composition to be sprayed may vary depending on the type of pests or adults or larvae, but in general, when flies extermination, the pesticide composition of the present invention is mixed with 20 l of water and sprayed evenly over an area of 360 m 2. In mosquito control, it is preferable to mix 100 ml of the pesticide composition of the present invention to 40 l of water and spray evenly over an area of 720 m 2, so that the final spraying concentration is 10 to 50 mg / m 2.

Hereinafter, the present invention will be described in detail by way of examples.

However, the following examples are merely to illustrate the invention, but the content of the present invention is not limited to the following examples.

Example 1 Preparation of Pesticide Formulations

2.65 g of cyro-margin (LG Chem, Korea) was mixed with 7.96 g of deltamethrin (LG Chem, Korea), followed by 79 ml of purified water and NK-PG 8.0 g (Coseal, Korea) as a cryoprotectant, NK as a preservative. -Betacide 0.2 g (Coseal Co., Ltd.) and NK-TSP120 1.0 g (Coseal Co., Ltd.) as an emulsifier were added to prepare a mixed formulation containing both cyro-margin and deltamethrin at the same time. As a comparative formulation, a single formulation containing only cyromargin or deltamethrin was used, which was prepared by dissolving the original agent of the pesticide in acetone according to the concentration and diluting each concentration.

<Example 2> Direct insecticidal effect using the spray tower

Using a rotary spray tower (Japan KK Mizuha Ewha Co., Ltd.) was compared the insecticidal power of the deltamethrin prepared in Example 1 and the sole formulation containing only each of the active ingredients of the formulation formulation. The test insects used in the experiment were Musca domestica and small red colony ( Culex pipiens pallens ), which were sold by the National Institutes of Health in 1986 and are used to date, and are susceptible to insecticides. Insecticides The direct pesticidal effects of individual and mixed formulations were investigated in order to compare the insecticidal rates of single and mixed formulations.

In order to investigate the insecticide spraying rate directly, inoculate 20 adult insects of small flies and small red domestic mosquitoes into plastic cups with a lower diameter of 5.5 × upper diameter of 7.5 × 6.5 cm in height. It was.

(2-1) Direct Spray Insecticidal Effects on Housefly Adults

In order to investigate the insecticidal effect in the direct spraying on housefly adults, a direct spray treatment effect experiment was conducted using a rotary spray tower. The samples used in the experiments were divided into a single dose group of deltamethrin or cyromarine, and a combination dose group of deltamethrin and cyromarine.

As shown in Table 1 below , as a result of spraying on housefly adults, the treatment of cyromarine alone showed no insecticidal effect on housefly adults, whereas the treatment of deltamethrin alone showed some insecticidal effects on housefly adults. It was. However, the insecticidal effect of the deltamethrin alone formulation was very low compared to the insecticidal effect of the deltamethrin and cyro-margin formulations.

Deltamethrin Cyro Margin Deltamethrin + Cyromargin Treatment concentration (ppm) Insecticide Rate (%) Treatment concentration (ppm) Insecticide Rate (%) Treatment Concentration (ppm) Insecticide Rate (%) 250.0 83.7 750.0 0.0 250 + 750 98.3 125.0 68.3 375.0 1.7 125 + 375 81.3 62.5 35.0 187.5 3.3 62.5 + 187.5 70.3 31.3 13.0 93.8 1.7 31.3 + 93.8 59.7 15.6 4.7 46.9 0.0 15.6 + 46.9 39.3 Control 3.3 - 0.0 - 0.0

(2-2) Direct Spraying Insecticidal Effects on Small Red Mosquitoes

In order to investigate the insecticidal effect when spraying the small red collecting device, a direct spray treatment effect experiment was conducted using the rotary spray tower in the same manner as described above. In the case of a small red collecting device, after inoculating 20 test insects inside a plastic cup with a mesh attached to the upper part, a sample treated with deltamethrin and cyromarin alone using a spray tower, and deltamethrin and cyromargin The pesticides of the samples treated by mixing were compared. Each sample was treated with 3 repetitions of 3 ml for each concentration and the insecticide rate after 24 hours was examined.

As a result of spraying tower spraying on small red colonic adults, as shown in Table 2 , the treatment with cyromarine alone showed very slight insecticidal effects on adult mosquitoes. On the other hand, the deltamethrin alone treatment was superior to the mosquitoes compared to the cyclomargin alone treatment, but this was also very low compared to the insecticide ratio of the deltamethrin and the cyclomargin mixture formulation.

Deltamethrin Cyro Margin Deltamethrin + Cyromargin Treatment concentration (ppm) Insecticide Rate (%) Treatment concentration (ppm) Insecticide Rate (%) Treatment Concentration (ppm) Insecticide Rate (%) 250.0 98.0 750.0 2.0 250.0 + 750.0 100.0 125.0 60.0 375.0 3.0 125.0 + 375.0 100.0 62.5 54.0 187.5 5.0 62.5 + 187.5 100.0 31.3 33.0 93.8 3.0 31.3 + 93.8 100.0 15.6 18.0 46.9 0.0 15.6 + 46.9 98.0 Control 5.0 - 3.0 - 2.0

From the above results, it can be seen that when the direct spraying using the spray tower, the treatment of cyromarin alone showed little insecticidal effect against flies and mosquitoes, because the cyromargin was a pesticide showing an insecticidal effect by inhibiting the larval peeling. . In addition, it was confirmed that administration of a combination formulation of cyro-margin and deltamethrin showed a better insecticidal effect than deltamethrin, which is known to control adult insect pests alone.

Example 3 Residual Contact Insecticidal Effect Using a Small Duster

In order to investigate the persistence of the insecticidal activity due to the residual contact effect after the spraying of the insecticide, the test was performed for housefly and small red colony adult using a small sprayer. Divided into a single group of deltamethrin or cyromarine and a combination group of deltamethrin and cyromarine, and the pesticides were sprayed into the home using a nebulizer (approximately 2.5 ml / cup) in 10 sets of each concentration. After spraying three times in an ice cream cup, the cups were stored at room temperature. Inoculations of flies and mosquitoes were carried out at intervals of 3 to 4 days from day 1, and the insecticidal rate for 24 hours after inoculation by residual contact was investigated.

(3-1) Pesticide Insecticidal Effects on Housefly Adults

As shown in Table 3 below , the deltamethrin single-administered group exhibited 100% insecticidal rate at a concentration of 500 ppm for housefly adults, but the insecticidal rate rapidly decreased with increasing dilution factor. In addition, the single siroma margin group also had a low insecticidal ability against housefly adults. However, it was confirmed that the insecticidal rate was excellently maintained even when the dilution rate was increased in the combined administration group in which cyromargin and deltamethrin were administered.

Deltamethrin Cyro Margin Deltamethrin + Cyromargin Treatment concentration (ppm) Insecticide Rate (%) Treatment concentration (ppm) Insecticide Rate (%) Treatment Concentration (ppm) Insecticide Rate (%) 500 100.0 1500.0 2.0 500 + 1500 100.0 250.0 87.0 750.0 0.0 250 + 750 100.0 125.0 83.0 375.0 3.0 125 + 375 100.0 62.5 47.0 188.0 2.0 62.5 + 188.0 100.0 31.3 40.0 94.0 0.0 31.3 + 94.0 100.0 15.6 17.0 47.0 0.0 15.6 + 47.0 97.0 8.0 13.0 23.0 0.0 8.0 + 23.0 95.0 Control 0.0 - 0.0 - 0.0

(3-2) Pesticide Contact Insecticidal Effects on Small Red Mosquitoes

As shown in Table 4 below , the insecticidal effect was very insignificant in the group treated with cyromargin alone, while the insecticidal effect was exhibited to some extent in the deltamethrin alone group. However, this was also very low compared to the insecticidal effect of the combination group administered with a mixture of cyro margin and deltamethrin.

Deltamethrin Cyro Margin Deltamethrin + Cyromargin Treatment concentration (ppm) Insecticide Rate (%) Treatment concentration (ppm) Insecticide Rate (%) Treatment Concentration (ppm) Insecticide Rate (%) 500 100.0 1500.0 7.0 500 + 1500 100.0 250.0 85.0 750.0 3.0 250 + 750 100.0 125.0 76.0 375.0 0.0 125 + 375 100.0 62.5 37.0 188.0 0.0 62.5 + 188.0 100.0 31.3 13.0 94.0 3.0 31.3 + 94.0 100.0 15.6 7.0 47.0 0.0 15.6 + 47.0 100.0 8.0 5.0 23.0 0.0 8.0 + 23.0 95.0 Control 0.0 - 0.0 - 0.0

Example 4 Long-term Persistence Evaluation of Insecticidal Rate

Long-term sustainability assessments were performed to evaluate the persistence of the insecticidal properties of deltamethrin alone and a combination of cyro-margin and deltamethrin. Treatment levels were treated with 125 + 375 ppm (1 / 200-fold dilution) of deltamethrin and cyro-margin for mixed formulations and 125 ppm of deltamethrin. The treatment was sprayed in 10 sets of plastic cups for each concentration to the extent that the chemical liquid was sufficiently flowed (approximately 2.5 ml / cup) using a household nebulizer with three times of treatment and stored at room temperature. Inoculations of housefly and small red colony adult were made at intervals of 3 to 4 days from 1 day after treatment, and the insecticidal rate of 24 hours after inoculation by residual contact was investigated.

(4-1) Long-term Persistence Evaluation of Insecticidal Effects on Housefly Adults

Figure 1 shows the insecticide change of the housefly adult due to the residual contact effect after the spraying of the request sample using a household sprayer. In the deltamethrin alone group, the insecticide rate was 80% at the time of inoculation and decreased to 15% after 30 days. However, when a combination formulation of deltamethrin and cyro margin was administered, the insecticide rate was 95% or more until 15 days, and thereafter, the pesticide rate was maintained at about 90 to 95% by about 26 days.

(4-2) Long-term Persistence Assessment of Insecticidal Effects on Adult Adults

Figure 2 shows the insecticidal rate due to the residual contact of each sample for the small red colony adult. The treatment concentration was 125 + 375 ppm (1 / 200-fold dilution) of the deltamethrin and cyro-margin in the mixed formulation, and diluted to 125 ppm in the deltamethrin alone administration group. As a result, as in the case of the adult housefly, the mixed insecticide exhibited an excellent insecticide sustaining effect of about 90% for about one month. However, the insecticidal effect of the deltamethrin alone group was significantly lower than that of the mixed formulation, showing a lower insecticidal rate of 25% or less after about a month after treatment.

Example 5 Insecticidal Effects on Housefly Larvae

To investigate the insecticidal activity against housefly larvae, the effect of siroma, one of the samples and components on 3, 5 and 7 day larvae (represented as 3, 5 and 7 days, respectively) after hatching in eggs Was investigated. 10 g of housefly larvae feed (prepared by adding fermented yeast extract 5% to furina meat feed) was added to the plastic cup, and 0.5 ml of each prepared concentration was treated and mixed evenly. After incubation, 3, 5 and 7 days old housefly larvae were inoculated in four replicates of 20 mice in each cup treated with the medicament, and the number of hatching to adults was examined, and the results are shown in Tables 5 to 7 below.

Cyromargin alone group Deltamethrin + Cyromazine Combination Group Treatment concentration (ppm) Insecticide Rate (%) Treatment Concentration (ppm) Insecticide Rate (%) 375.0 100.0 125 + 375 100.0 125.0 95.0 42 + 125 100.0 42.0 86.0 14 + 42 100.0 14.0 72.0 4.7 + 14 100.0 5.0 68.0 1.7 + 5 100.0 Control 13.0 Control 19

Cyromargin alone group Deltamethrin + Cyromazine Combination Group Treatment concentration (ppm) Insecticide Rate (%) Treatment Concentration (ppm) Insecticide Rate (%) 375.0 100.0 125 + 375 100.0 125.0 82.0 42 + 125 100.0 42.0 74.0 14 + 42 100.0 14.0 62.0 4.7 + 14 95.0 5.0 59.0 1.7 + 5 72.0 Control 7.0 Control 9.0

Cyromargin alone group Deltamethrin + Cyromazine Combination Group Treatment concentration (ppm) Insecticide Rate (%) Treatment Concentration (ppm) Insecticide Rate (%) 375.0 78.0 125 + 375 100.0 125.0 48.0 42 + 125 90.0 42.0 37.0 14 + 42 74.0 14.0 25.0 4.7 + 14 68.0 5.0 14.0 1.7 + 5 50.0 Control 6.0 Control 4.0

As shown in Table 5 to Table 7 , in the experiments for the three-day-old housefly larvae, in the case of the combination formulation of cyro-margin and deltamethrin, a low concentration of deltamethrin 1.7 ppm + cyro-margin 5 ppm (16,200-fold dilution factor) In addition, the insecticidal effect of 100%, while in the case of the cyro-margin alone group, the insecticidal rate was reduced to 68% at 5 ppm showed excellent insecticidal effect in the mixed formulation. The mixed formulation treatment of 5 day old housefly larvae showed 72% insecticidal effect even at low concentrations (16,200-fold dilution) of deltamethrin 1.7 ppm + cyro-margin at 5 ppm. The pesticide rate was less than 59% in Esau. Experiments on 7-day-old housefly larvae showed a 100% insecticidal rate at the concentration of 125 ppm of deltamethrin + 375 ppm (200-fold dilution) of the mixed formulation, and a low insecticide rate in the cyro-margin alone group. It was.

From the above results, it can be seen that administration of a combination formulation of cyro-margin and deltamethrin is superior to larval margin alone, and the insecticidal effect is superior to younger larvae.

Example 5 Checking Stability of Mixed Formulations

Mixed formulation pesticides prepared using two or more pesticides exhibit better insecticidal properties than a single formulation, but the active ingredient may decompose over time, causing stability problems. The stability of the formulation was investigated as follows.

Insecticides formulated with cyro-margin and deltamethrin were selected from each of the other three lots and stored at room temperature for 24 months, each at 3, 6, 9, 12, 18 and 24 months of testing. The change in the content of the active ingredient was observed.

<5-1> Determination of the content of deltamethrin

In order to prepare the sample solution, the mixed formulation of the present invention collected at each time was precisely measured in an amount corresponding to 26.5 mg of deltamethrin, placed in a 100 ml flask, and dissolved in an appropriate amount of methanol. 100 ml was adjusted. 10 ml of the solution was taken into a 100 ml volumetric flask, and methanol was added to accurately adjust the final volume to 100 ml.

The standard solution was prepared by the same method as the test solution by precisely weighing 26.5 mg of the deltamethrin standard.

The content of deltamethrin in the sample solution and the standard solution prepared as described above was measured in accordance with the following instrument conditions according to the Pharmacopoeia General Test Method Liquid Chromatography Method (Korean Amendment No. 7, Rev. 967-968). Got. The deltamethrin content in the sample solution measured from this is shown in Table 8 below.

Column: -Bondapak C18 (3.9 300 mm) and equivalent

Mobile phase: acetonitrile: water = 80: 20

Detector: UV absorbance photometer (wavelength: 230 nm)

Flow rate: 1.0 ml / min

Injection volume: 20 μl

Amount of deltamethrin (C ₂₂ H ₁₉ Br ₂ NO ₃ : 505.2) (mg) = amount of standard taken (mg) x Ru / Rs

Where Ru is the peak area of the sample solution and Rs is the peak area of the standard solution.

<5-2> Determination of Cyclomargin Content

In order to prepare the sample solution, the mixed formulation of the present invention collected at each time period was precisely measured in an amount corresponding to 79.6 mg of siro margin, and placed in a 100 ml flask, and then dissolved in an appropriate amount of methanol. Adjusted to ml. 10 ml of the solution was taken into a 100 ml volumetric flask, and methanol was added to accurately adjust the final volume to 100 ml, which was then filtered and used as a sample solution.

The standard solution was prepared in the same manner as the above test solution by precisely weighing 79.6 mg of the cyclomargin standard.

The content of the cyclomargin in the sample solution and the standard solution prepared as described above was measured in accordance with the following instrument conditions according to the Pharmacopoeia General Test Method liquid chromatography method to obtain respective peak areas Ru and Rs. Cyclomargin content in the sample solution measured from it is shown in Table 9 below.

Column: -Bondapak C18 (3.9 300 mm) and equivalent

Mobile phase: Acetonitrile: Water: Trifluoroacetic acid = 3: 97: 0.1

Detector: UV absorbance photometer (wavelength: 240 nm)

Flow rate: 1.0 ml / min

Injection volume: 20 μl

Amount of Cyromargin (C ₆ H ₁₀ N ₆ , 166.19) (mg) = Standard Intake Amount (mg) x Ru / Rs

Where Ru is the peak area of the sample solution and Rs is the peak area of the standard solution.

Changes in Deltamethrin Content in Mixed Formulations Retention period Lot A B C Exam start date 100.1 100.0 99.7 100.2 100.1 100.0 99.9 100.0 100.2 Average 100.1 100.0 100.0 3 months 100.1 100.1 99.8 99.9 100.3 100.0 99.9 100.0 100.0 Average 100.0 100.1 99.9 6 months 99.7 99.4 99.6 99.4 99.3 99.5 99.4 99.8 99.2 Average 99.5 99.5 99.4 9 months 99.2 99.1 99.2 98.9 98.9 99.0 99.1 99.0 99.0 Average 99.1 99.0 99.1 12 months 96.2 96.5 99.5 99.4 97.6 99.3 98.8 100.6 99.6 Average 98.1 98.2 99.5 18 months 96.8 98.2 94.6 98.8 99.5 97.6 99.5 99.3 98.9 Average 98.4 99.0 97.0 24 months 98.0 94.6 95.2 97.7 95.8 94.1 97.6 96.5 96.5 Average 97.8 95.6 95.3

Variation of Cyclomargin in Mixed Formulations Retention period Lot A B C Exam start date 99.3 100.3 100.2 99.0 100.4 100.1 100.2 100.9 95.7 Average 99.5 100.5 98.7 3 months 100.2 99.6 99.6 100.7 100.1 99.5 99.7 100.0 100.5 Average 100.2 99.9 99.9 6 months 100.3 99.8 100.0 102.1 100.7 100.3 101.2 99.7 100.5 Average 101.2 100.1 100.3 9 months 101.3 99.1 99.0 99.9 101.0 98.9 99.9 100.1 100.1 Average 100.4 100.1 99.3 12 months 98.7 99.1 99.9 99.5 99.4 98.6 98.5 99.5 98.5 Average 98.9 99.3 99.0 18 months 97.3 97.0 97.0 96.7 97.2 97.1 96.8 97.1 97.6 Average 96.9 97.1 97.2 24 months 94.6 95.4 95.3 95.0 95.8 94.5 95.2 95.0 95.8 Average 94.9 95.4 95.2

As shown in Table 8 and Table 9 , it can be seen that the cyclomarin and deltamethrin mixed formulations of the present invention are very stable without change in the content of the active ingredient even when stored at room temperature for 24 months.

As described above, the pesticide composition comprising the cyromargin and the deltamethrin of the present invention can be used for the control of flies and mosquitoes because the insect pest and the adult can be removed at the same time.

Claims (5)

Insecticide composition containing cyroma margin and deltamethrin as active ingredients. The insecticide composition according to claim 1, wherein the mixing ratio of deltamethrin and cyromargin is 1: 1 to 1:10. The pesticide composition of claim 1 comprising between 0.1 and 20% cyclomargin, 0.1 to 20% deltamethrin, 0.1 to 99% carrier and 0.1 to 10% surfactant. A method of simultaneously controlling the adult and the larvae of the pest by spraying the pesticide composition of claim 1 directly to the habitat of the pest or added to the feed or feces of livestock. The method according to claim 4, wherein the spraying amount of the pesticide composition is 10 to 50 mg / m 2.