HK40072688B - Combination of encapsulated phenothrin and emulsified prallethrin - Google Patents

Description

A mixture of encapsulated fenpyroxene and emulsified dextromethorphan.

Technical Field

This invention relates to a novel water-based formulation comprising two active ingredients, namely fenpyroxene and d-propyne pyroxene.

Background Technology

Currently available products are in the form of water-based emulsions or in the form of emulsifiable concentrates, which can be used in aerosols or as ready-to-use solutions of the active ingredient.

The following product compositions are available:

0.25% d-phenylephrine / 0.125% d-phenylephrine.

0.20% d-phenylephrine / 0.1% d-phenylephrine / 0.90% PBO

0.33% d-phenylephrine / 0.13% d-phenylephrine

All of these products have drawbacks, for example:

Lower residual effect;

Highly toxic;

It places a high burden on the human body;

The concentration of active ingredients is higher;

The product's full availability during use can lead to overuse.

The biodegradability of the active ingredients cannot be controlled;

High content of aromatic/aliphatic solvents;

No UV protection;

It is very sensitive to organic matter in the environment;

It changes color and has an odor.

Pyrethroid (3-phenoxyphenyl)-methyl-(1R)-cis-trans-2,2-dimethyl-3-(2-methyl-1-propenyl)-cyclopropanecarboxylate) belongs to the first-generation type I synthetic pyrethroids. Its structure is as follows:

It acts on nerve cell membranes upon contact or absorption, and during repolarization, it blocks the closure of the ion gates of sodium channels. This interrupts the transmission of nerve impulses. At low concentrations, insects become hyperactive, while at high concentrations, they become paralyzed and die.

First registered by the U.S. Environmental Protection Agency (EPA) in 1976, permethrin is available as a ready-to-use (RTU) indoor spray and carpet powder, as well as as a pressurized concentrate and emulsified concentrate, and is formulated as a dot or strip for the control of fleas and ticks on pets. In addition to permethrin, formulations for pets typically contain other active ingredients. Permethrin is also formulated for use in ultra-low volume (ULV) sprayers and indoor atomizers. Its instability to sunlight reduces residual effects, thus shortening the duration of protection.

Dextrorotatory pyrethroid (2-methyl-4-oxo-3-prop-2-en-1-yl-2,2-dimethyl-3-(2-methylprop-1-en-1-yl)-cyclopropanecarboxylate) belongs to type II pyrethroids. It is a pyrethroid that has a rapid, immediate effect (knockdown effect) on household pests. Its structure is as follows.

The most important types of formulations available are vaporizer pads (mosquito killers) and liquid vaporizers.

There are some products on the market containing permethrin and d-propargyl. However, these products do not specify residual effects, from which it can be concluded that they also have no residual effects, as residual effects are highly anticipated. The following is a list of products containing permethrin and d-propargyl found in the European Patent Office database:

-DUET ^TM Dual-action(EPA Reg.No.:1021-1795-8329)

-Raid Flying inspection(EPA Reg.No.4822-569)

-Raid Multi-insect(EPA Reg.No.4822-569)

These products have no residual effects.

Patcit 0001: US Patent US 2015237861 A discloses a formulation containing tetrahydropyrethrin, dichlorophenyl ether, and piperonyl butyl ether (see Table 2). However, as shown in Table 4 of this document, this formulation exhibits insufficient residual effect within seven days of application. Example 2C of the same document illustrates a formulation containing tetrahydropyrethrin and dichlorophenyl ether, but this formulation also showed a significant decrease in effectiveness within three months.

In US Patent 8216598 B, Patcit 0002, GAT Microcapsule Corporation describes a method for producing microcapsules. These microcapsules can be produced via in-situ emulsion polymerization, resulting in ethylene glycol-polyurea microcapsules.

Summary of the Invention

The objective of this invention is to find a formulation in which the two active ingredients, phenoxy ...

According to the present invention, the novel formulation is a suspension of encapsulated fenpyroxene and an emulsion of dextromethorphan.

Therefore, the formulation according to the present invention can be understood as an application of the patent mentioned in Patcit 0003 US Patent US 8216598 B, to obtain a more environmentally friendly product with better efficacy, longer residual effect and improved toxicological characteristics.

In this formulation, permethrin is released in a controlled manner, resulting in high efficacy against various crawling and flying insect pests such as black ants, fire ants, termites, silverfish, bedbugs, German cockroaches, American cockroaches, house spiders, mosquitoes, midges, and mosquitoes.

Currently, there are no products of this kind for insect control in which two active ingredients, namely, fenpropathrin microcapsules as a long-acting formulation and d-propargyl ester emulsion as a fast-acting formulation, are combined in a single ZW formulation. ZW is a mixture of CS (capsule suspension) and EW (emulsion, oil-in-water suspension). To date, the most similar commercially available products are registered with the European Patent Office, which consist of free, non-microcapsulated fenpropathrin and d-propargyl ester in emulsion form, but also contain piperonyl butyl ether (PBO) as an additional ingredient. Therefore, the product according to the invention has a considerable advantage: surprisingly, it exhibits a residual effect for at least 8 weeks, and even up to 12 weeks, which is unattainable from the prior art. Studies have shown that, in tests on houseflies and German cockroaches, the product according to the invention also caused complete mortality after three months.

The ratio (mass ratio) of phenoxy ...

Particularly preferred is that the permethrin is microencapsulated, with a specific particle size preferably between 1.8 μm and 3.3 μm. The particle size is determined as a volume-weighted average by laser diffraction.

It has been demonstrated that, especially when the ratio of phenoxybenzyl to d-propargyl is close to the optimal ratio of 10:1, the duration of action of this composition is at least 8 weeks. Typically, the lethal effect is fully maintained for at least twelve weeks, decreasing only after sixteen weeks. However, the toxicity to humans and other warm-blooded animals is very low, a fact crucially contributed by microencapsulation. Due to microencapsulation, the toxicity that humans and other warm-blooded animals may inhale is also lower.

By co-formulating with a UV stabilizer, stability against UV radiation can be ensured, thus guaranteeing a longer duration of action even in areas with high sun exposure. A suitable UV stabilizer is Es Calo 551.

Microencapsulation allows for optimal tuning of time-release properties. Therefore, compared to known products, fewer active ingredients can be used to perform the procedure.

Therefore, the concentrate may contain approximately 10% by weight of fenpropathrin and approximately 1% by weight of d-propargyl. This concentrate is diluted with water at a ratio of 1:99 to obtain a usable final product. This final product contains approximately 0.1% by weight of fenpropathrin and 0.01% by weight of d-propargyl. This final product is particularly suitable as an insecticide. As demonstrated below, the optimal coating amount is approximately 25 ml/ ^m² on non-porous surfaces and approximately 50 ml/ ^m² on porous surfaces.

Release rate is affected by microcapsule size, the ratio of monomer, prepolymer and three-dimensional crosslinking agent, as well as wall thickness and wall permeability.

It exhibits high storage stability, resulting in only slight degradation of the active ingredients during storage.

The active ingredients achieve compatibility through release rates, and these active ingredients are selected based on their action behavior to achieve a balance between efficacy, toxicity, and stability. This product provides two effects with a single application: rapid knockdown (paralyzing insects) and safe killing.

This invention focuses on the efficacy of these two active ingredients and improves their inherent properties through microencapsulation and emulsification in water to enhance both immediate (knockout) and residual effects. The fully tested formulation contains 0.1% fenpropathrin and 0.01% d-propynephrine. This formulation is referred to as the "final product".

When used in combination with d-propargyl, it exhibits excellent performance in controlling household insects.

Table 1

Advantages of benzebufen: Advantages of d-propargylpyrethrin: Excellent effectiveness curve Excellent immediate effect Non-corrosive Effective even with low dosage Biodegradable Biodegradable Diverse applications Diverse applications Beneficial toxicity Beneficial toxicity

There are currently 198 valid licenses for permethrin products in the United States.

In products sold in the United States and Canada, the concentration of permethrin is 0.096% in pet care sprays and 1.3% in pump-action flea sprays. The estimated duration of effect is less than two months.

The available formulations are either oil-based or water-based aerosols. Both types are often combined with synergists. In this regard, many household products containing permethrin are sold in aerosol spray cans containing highly flammable inert propellants such as propane and isobutane.

Some products, available as ready-to-use indoor sprays or as carpet powder, can be used as pressurized or emulsified concentrates. Another form of use is to apply them in dots or strips along with other active ingredients to eliminate fleas and ticks. Finally, permethrin-based products can be used with ultra-low volume sprayers and indoor sprayers.

Surface application of pesticides with residual effects remains one of the most cost-effective and versatile methods for controlling insect pests in urban and domestic environments. The surfaces on which pesticides are applied vary widely, and these surfaces are often porous. This can negatively impact the bioavailability of the pesticide. Other surfaces may be additionally chemically reactive and denature the active ingredient, thus impairing the persistence of the effect. Furthermore, pesticides applied to external surfaces are susceptible to other adverse conditions, primarily photodegradation, which significantly reduces the persistence of the effect.

In the field of insect control, the final product is a novel composition with slow to medium-speed release characteristics, in which the release rate remains constant until the active ingredient in the capsule is depleted.

Once microcapsules containing permethrin come into contact with insects, the active ingredient rapidly diffuses into the insect's lipophilic cuticle. Based on this fact, the state and biological properties of permethrin can be altered through microencapsulation.

Microencapsulated formulations protect permethrin from degradation caused by sunlight. Periodic release results in a formulation with a slow-release active ingredient. This produces better efficacy because the active ingredient is delivered at a constant and prolonged release rate.

Therefore, the final product is a complex, dual-action household insecticide. It combines the proven efficacy of microencapsulated permethrin with the superior immediate effect of d-propargylpyr. This is why the final product begins to work effectively immediately.

These active ingredients together provide a superior control mechanism because the best effects of each active ingredient are utilized to create an insecticide that achieves unique results and improves the effectiveness of insect control and user safety.

In summary, the final product was formulated using microencapsulation technology to create a product specifically for urban and residential areas, as outlined below;

- Contains highly effective ingredients;

- It continues to produce effectiveness on many surfaces, including highly porous and chemically reactive surfaces;

- Rapid, immediate effect (knockout effect) and lethality.

Furthermore, the use of microcapsules in the final product results in several significant improvements in environmental and user safety.

The final product may also have the following characteristics:

- A sustained-release formulation containing antioxidants, which, due to the action of microcapsules, has UV protection capabilities;

- Immediate and timed release, which lasts for at least eight weeks, as scientifically proven;

- Slow degradation, thus requiring very little administration to maintain a lethal dose.

Detailed Implementation

Examples of formulations according to the present invention.

The following explains how the microcapsules and emulsions necessary for producing the final product are composed. They include the following components:

Table 2

In the following five examples, the following amounts (by weight percentage) of components A through O were used respectively.

Table 3

Example 1

Production of capsule suspension (CS)

For a final product of 5kg, 1670g of capsule suspension (CS) is required. All data are expressed as a percentage by weight.

Table 4

Prior to the emulsification process, the aqueous and oil phases were placed in a 2-liter jacketed reactor at a temperature of 40°C.

In a 2-liter jacketed reactor equipped with a clawless mixer and a high-shear mixer, the aqueous phase is added at 40°C. When the clawless mixer is turned on at 1600 rpm, the oil phase is added to the aqueous phase very rapidly (~1 minute), thereby initiating the emulsification polymerization process.

After the entire oil phase was fully emulsified, the high-shear mixer was started at 4600 rpm. Emulsion polymerization ended after 4 minutes.

The capsule suspension was then transferred at 60°C to another jacketed reactor equipped with only one anchor stirrer at 36 rpm.

Stir the capsule suspension for 3 hours at 60°C until the capsules harden and form stably.

Production of water-in-oil emulsions (EW)

3330g of emulsion (EW) is required for 5kg of final product. All data are expressed as a percentage by weight.

Table 5

Propylene glycol 7.5 Zephrym PD3315 3.0 Xanthan Gum 0.6 Break Thru AF5503 0.0225 Proxel GXL 0.15 water 871.175 Prallethrin TG 1.61

In a 5-liter jacketed reactor equipped with a high-shear mixer, all components of the water-in-oil emulsion formulation, except for xanthan gum and d-propargylpyrethrin, are added.

The components were mixed using a high-shear mixer at a speed of 1200 rpm, and the solution was heated to 40°C.

After the temperature reaches 40°C, xanthan gum is added at 4600 rpm to allow it to fully form a transparent gel.

Finally, add the technical type of d-propargylpyrene heated to 40°C and stir at 4600 rpm for 4 minutes to obtain a homogeneous and stable emulsion in water (EW).

The final suspension of the capsules, mixed with an emulsion (EW), is produced to form the ZW formulation.

In a 6-liter jacketed reactor, 1670 g of capsule suspension was mixed with 3330 g of water emulsion (EW) at a speed of 36 rpm for at least 4 hours using an anchor stirrer until the suspension reached equilibrium and stabilized.

The particle size of the ZW formulation was measured using laser diffraction equipment, and the dispersion stability of the capsules in 342 ppm hard water at a ratio of 1:99 was also measured.

Example 2

Production of capsule suspension (CS)

For a final product weighing 5kg, 1670g of CS is required. All data are expressed as a percentage by weight.

Table 6

oil phase weight percentage Aqueous phase weight percentage 1R-trans-phenylephrine 31.932 Synperonic PE/F 127 2.25 TMXDI 0.450 BrijO20 0.056 ONGRONAT 2100 3.150 Zephrym PD3315 3.00 Cymel 1170 0.300 water 44.912 Radia 7117 13.500 Cycat 4040 0.45

The production method is the same as in Example 1.

Production of water-in-oil emulsions (EW)

For 5kg of final product, 3330g of emulsion (EW) is required. All data are expressed as a percentage by weight.

Table 7

The production of the water emulsion and the final suspension are carried out in accordance with Example 1.

Example 3

Production of capsule suspension (CS)

For a final product of 5kg, 1670g of capsule suspension (CS) is required. All data are expressed as a percentage by weight.

Table 8

oil phase weight percentage Aqueous phase weight percentage 1R-trans-phenylephrine 31.932 Synperonic PE/F 127 2.52 TMXDI 0.900 BrijO20 0.056 ONGRONAT 2100 4.200 Zephrym PD3315 3.0 Cymel 1170 0.75 water 41.102 Radia 7117 15.00 Cycat 4040 0.54

The production method is the same as in Example 1.

Production of water-in-oil emulsions (EW)

For 5kg of final product, 3330g of emulsion (EW) is required. All data are expressed as a percentage by weight.

Table 9

Propylene glycol 11.25 Zephrym PD3315 3.00 Xanthan Gum 0.525 Break Thru AF5503 0.0225 Proxel GXL 0.15 water 83.442 Prallethrin TG 1.61

The production of the water emulsion and the final suspension are carried out in accordance with Example 1.

Example 4

Production of capsule suspension (CS)

For a final product of 5kg, 1670g of capsule suspension (CS) is required. All data are expressed as a percentage by weight.

Table 10

oil phase Gew.-% Aqueous phase Gew.-% 1R-trans-phenylephrine 31.932 Synperonic PE/F 127 2.76 TMXDI 1.20 BrijO20 0.056 ONGRONAT 2100 4.50 Zephrym PD3315 3.0 Cymel 1170 0.90 Wasser 36.902 Radia 7117 18.00 Cycat 4040 0.75

The production method is the same as in Example 1.

Production of water-in-oil emulsions (EW)

For 5kg of final product, 3330g of emulsion (EW) is required. All data are expressed as a percentage by weight.

Table 11

Propylene glycol 13.5 Zephrym PD3315 3.52 Xanthan Gum 0.45 Break Thru AF5503 0.0225 Proxel GXL 0.15 water 807.475 Prallethrin TG 1.61

The production of the water emulsion and the final suspension are carried out in accordance with Example 1.

Example 5

Production of capsule suspension (CS)

For a final product of 5kg, 1670g of capsule suspension (CS) is required. All data are expressed as a percentage by weight.

Table 12

The production method is the same as in Example 1.

Production of water-in-oil emulsions (EW)

5kg of final product requires 3330g of emulsion (EW). All data are expressed as a percentage by weight.

Table 13

Propylene glycol 15.00 Zephrym PD3315 2.70 Xanthan Gum 0.45 Break Thru AF5503 0.0225 Proxel GXL 0.15 water 800.675 Prallethrin TG 1.61

The production of the water emulsion and the final suspension are carried out in accordance with Example 1.

Key parameters for microcapsule selection

The selection of microcapsules for stability and efficacy studies is based on the desired characteristics of the final product.

The most important characteristic is the release rate of the microcapsules, which is mainly controlled by the following factors:

1. Size of the microcapsules (in μm);

2. Degree of crosslinking (ratio of wall-forming material to crosslinking agent);

3. Wall thickness (ratio of polymer to encapsulated oil phase);

4. The mobility of the oil phase is a function of the solvent content.

Considering all four characteristics listed, each example can reference the following data:

Table 14

Medium/high particle size means a small number of particles per volume;

Low/medium particle size means that there are many particles per volume.

A higher degree of cross-linking means a lower release rate and a longer residual effect;

Moderate cross-linking means rapid release and moderate residual effectiveness;

A lower degree of cross-linking means rapid release and low residual effectiveness.

High wall thickness implies moderate diffusion rate;

Low wall thickness means high diffusion rate.

Therefore, it can be seen that the number of particles per volume is low in Examples 1 and 2; consequently, the surface area used to deliver the active ingredient is too small, resulting in low effectiveness. Thus, these examples are not suitable for further testing.

In Example 3, the higher number of particles per volume provides a larger surface area for the delivery of the active ingredient, resulting in greater effectiveness. Furthermore, the narrow particle size distribution leads to better dispersion stability. The degree of crosslinking yields a moderate release profile, with a higher proportion of wall-forming material resulting in moderate diffusion, which produces a sufficient residual effect. This example was selected for further testing.

Example 4 is similar to Example 3, but the particle size distribution is less narrow and the mobility is higher; this formulation is acceptable, but not as ideal as Example 3.

In Example 5, the number of particles per volume is moderate to high, there is moderate surface area available for delivering the active ingredient, and the residual effect is low due to the rapid release profile. Therefore, this example is not suitable for further testing.

Finally, Example 3 was selected for further testing (efficacy, toxicity).

Data on the effectiveness of the final product (without selection testing)

The concentrate has been diluted at a ratio of 1:99, making it available as a ready-to-use formulation.

Adults of different sexes were used to assess the residual effects of this final product in terms of knockdown and mortality.

Shake the product thoroughly before use. Apply 100 ml/ ^m² to carpet, concrete, and wood surfaces, and 50 ml/ ^m² to ceramic surfaces. These surfaces were stored under ambient conditions before use. For a realistic approach, the total treated area was 1 ^m² . An untreated control (without any product) was prepared in the same manner for comparison.

This is a test that forces insects to remain on the treated surface (“no-selection” test). The persistence of the effect was determined by performing the same test after 4 and 8 weeks of panel storage. Insect observation was based on the following criteria:

--Knockout effect;

--mortality rate.

A supplementary experiment was conducted in which the final product was sprayed directly onto insects, and the immediate knockdown effect and mortality rate after 24 hours were measured. In both cases, the result was 100%.

It exhibits a 100% knockdown effect on the sprayed surface.

-Day 0, 15 minutes later

- Four weeks later, 45 minutes later

-Eight weeks later, 60 minutes later

The mortality rates of the following insects were investigated on four different surfaces (concrete, wood, carpet, and tile):

Houseflies

Aedes aegypti

common Culex mosquitoes

African malaria mosquitoes

German cockroach

American cockroaches

Black Road Ants

Common wood tick, a type of shield tick

cat fleas

silverfish

bed bugs

clothes moth

House dust mites

Corner spiders, cellar spiders

head lice

The mortality rate was 100% at day 0 and after 8 weeks.

This indicates that when spraying a non-porous surface with a dosage of 50 ml/ ^m² , and when spraying a porous surface with a dosage of 100 ml/ ^m² , the results are different.

- It has a very good insecticidal effect due to its rapid knockdown effect and thorough killing rate;

- The residual effect lasts for at least eight weeks after treatment of different surfaces (tile, carpet, wood and concrete).

Effectiveness study of the final product (simulation application) - 8 weeks

Additional tests were conducted in which the insects were able to move freely, which is equivalent to real-world conditions.

According to BSI 4172 Parts 1 and 2 (1993) standards for testing portable pressurized canister insecticides, tests were conducted in four replicates in four 15 ^m³ test chambers (6 ^m² floor area). During the test periods, the temperature in the test chambers was maintained at 26 °C ± 1 °C, and the relative humidity at 70% ± 5%.

The materials used in the testing chamber are washable. Non-porous materials, such as epoxy-coated steel and ceramic tiles, are used on the walls/ceiling and floor.

To simulate an indoor scenario, polystyrene blocks and cardboard boxes were placed in the test chamber to create hiding places (refuges) and sources of water and food.

- Water source (six 25cm long water bottles, with cotton swabs);

-Food sources (four places on the floor, and two petri dishes containing dog biscuits in hidden places).

These insects can reach water and food sources without contact with pesticides. They are able to hide in many places. Only half of the area is treated, thus allowing all target organisms to choose whether or not to come into contact with the final product.

For each treatment and each replicate, insects were used as follows: 25 per species, except for the hard-to-find cellar spider, and only 5 of them were used for each replication, including the corresponding untreated control.

Control test subjects are used to examine the animals used for testing and to identify any unintended effects that the treatment or test conditions may have.

The insects were released two hours after treatment to allow sufficient time for the surface to dry.

Apply using a GLORIA 8l professional sprayer with an anti-drip nozzle. Shake the liquid vigorously between each treatment.

The dosage is 50 ml/ ^m² , and the area to be treated is half of the test chamber, for example, 3 ^m² , that is, 150 ml of product is applied to each 3 ^m² area.

The routes to the feed and water sources were not treated.

The following insects were used in the test.

Houseflies

Aedes aegypti

common Culex mosquitoes

African malaria mosquitoes

German cockroach

American cockroaches

Black Road Ants

Red imported fire ants

Yellow-legged termites

silverfish

bed bugs

Corner spiders, cellar spiders

The mortality rate was 100% at day 0 and after 8 weeks.

Under the conditions of this study (simulated application), the final product, applied at a rate of 50 ml/ ^m² , showed complete destruction within less than a week, with a mortality rate of 100%. The residual effect remained unchanged over eight weeks following treatment.

Effectiveness study of the final product (simulation application) - 12 and 16 weeks

Additional tests were conducted to evaluate the effectiveness and residual effects of the final products applied to control various insect pests.

The experiment was conducted in a laboratory testing room with materials designed for actual use (cardboard boxes = hiding places/refuges + food/water), and only half of the area was treated with the product, allowing the target organism to choose whether or not to come into contact with the product.

Effectiveness was quantified by the percentage reduction in number after 8 and 12 weeks of treatment.

The tested dosages were: 50 ml/ ^m² for non-porous surfaces (tiles) and 50 ml/ ^m² for porous surfaces (fiber cement).

The species selected for testing were houseflies and German cockroaches.

This product has been proven to be highly effective against both of these target pests with a complete kill rate (100%) over a contact period of up to 12 weeks.

Tests conducted four weeks later showed that the drug remained effective against houseflies, but had only slight effectiveness against German cockroaches.

Table 15

8 weeks 12 weeks 16 weeks Houseflies 100% 100% 100% German cockroach 100% 100% 17%

Toxicity studies of the final product

Acute oral toxicity tests were conducted in rats to determine whether the final product was toxic at a single dose. Under study conditions, the acute oral LD50 of the final product was greater than 5000 mg/kg body weight in female rats. During the study period, all animals survived, gained weight, and appeared active and healthy. Therefore, the final product is classified as GHS Hazard Group 5, meaning no symbols or warnings are required.

Acute inhalation toxicity tests were conducted using rats to determine whether the final product would be toxic in a single inhalation exposure (nasal exposure only). Under the study conditions, the LC50 of the test substance was greater than 5.03 mg/L in both male and female rats. Therefore, the final product also meets the requirements of Class 5.

All animals survived the exposure and gained weight during the test. Following exposure, all rats exhibited irregular breathing, but all recovered by day 2 and remained active and healthy for the remainder of the two-week observation period. No serious abnormalities were found upon necropsy of any animal at the end of the 14-day observation period.

Because the lethal dose of the concentrate in rats exceeded 5000 mg/kg, no acute skin toxicity test was performed.

Toxicity testing of the concentrate

Similar studies on the concentrates (10% deltamethrin and 1% d-propargyl) showed that the LD50 values were greater than 5000 mg/kg body weight in both oral and acute dermal toxicity tests. This corresponds to Category 5 of the relevant GHS hazard class, meaning no symbols or warnings are required.

In the acute oral toxicity study, mortality, severe poisoning symptoms, and behavioral changes in all animals were observed at least daily for 13 or 14 days. All animals survived, gained weight, and appeared active and healthy. No signs of severe poisoning, adverse pharmacological effects, or abnormal behavior were observed.

In the acute skin toxicity study, mortality, severe poisoning symptoms, and behavioral changes in all animals were observed at least once daily for up to 14 days. All animals survived the exposure and gained weight. No serious abnormalities were found at necropsy of any animal at the end of the 14-day observation period.

In the acute inhalation toxicity study, the values met the requirements of Category 4 in the corresponding GHS hazard class. All animals survived in the test environment. Following exposure, eight rats exhibited decreased activity; in addition, all rats exhibited irregular breathing, gait abnormalities, and tremors. However, all rats recovered by day 4 and remained active and healthy throughout the remaining 14-day observation period. Although some animals experienced weight loss or at least no weight gain on day 1, all animals gained weight during the 14-day observation period. The observed weight loss was considered to be of no toxicological significance. No serious abnormalities were found during necropsy of any animal at the end of the 14-day observation period.

Shelf life of final products and concentrates

Physical and chemical properties were determined according to OECD Good Laboratory Practice (GLP) principles and the Austrian Chemicals Act 1996. These studies were conducted using 0.375 L PET spray bottles as the final packaging material. Typical parameters such as physical state, color, odor, active ingredient content, density, pH, wet sieve residue, persistent foaming, particle size, fillability, dispersion stability, and corrosion characteristics were determined. Four samples were analyzed:

-Newly manufactured products

The product after 4 freeze/thaw cycles: 18 hours at -10±2℃ and 6 hours at 20±2℃ respectively.

Products after 7 days at -0±2℃;

- Products after 14 days at 54±2℃.

In these samples, both the final product and the concentrate remained stable with accelerated aging.

Determine the anaerobic biodegradation status of the final product

The anaerobic biodegradation of the final product was determined according to OECD 310:2014. During the test period (28 days), the samples were maintained at a temperature of 20 ± 2 °C.

Since the TIC content was below 10% at the end of the test cycle, it can be concluded that no non-biodegradation occurred. According to OECD 310:2014, the final product is therefore considered non-biodegradable under aerobic conditions.

Determine the effective dose for non-porous surfaces

The purpose of this study was to evaluate different dosages of the final product on non-porous surfaces for the control of houseflies, German cockroaches, and house spiders.

These insects were exposed to different doses, namely 12 ml/ ^m² , 25 ml/ ^m² , and

The surface was treated with 35 ml/ ^m² . A control experiment was also conducted in which the surface was treated with water.

This product was used to treat some 15cm*15cm ceramic tiles, and insects were exposed to them for one hour. Mortality rates were observed at regular intervals.

The results are as follows:

For tiles treated with water, the mortality rate was less than 5%, which made the trial valid.

The percentage of insects killed in the tiles treated with 12 ml/ ^m² was as follows:

Table 16

It can be seen that this dosage is insufficient, because not all insects were eliminated after 24 hours.

For tiles treated with 25 ml/ ^m² , the following percentages were obtained:

Table 17

Here, the dosage was sufficient: all the insects were eliminated after 24 hours.

The following percentages were obtained for the tiles treated with 35 ml/ ^m² :

Table 18

This dosage increase further improved the effect: the houseflies were completely eliminated in just 7 hours, and the dosage increase also improved the elimination of the other two insects.

Determine the effective dose for porous surfaces

The purpose of this test is to evaluate the different dosages of the final product on porous surfaces for the control of houseflies and German cockroaches.

Houseflies

German cockroach

These insects were exposed to concrete treated with different doses: 25 ml/ ^m² , 35 ml/ ^m² , and 50 ml/ ^m² . A control experiment was also conducted in which the concrete was treated with water.

Observe mortality rates at regular intervals.

The results are as follows:

For concrete treated with water, the mortality rate was less than 5%, which made the test valid.

The percentage of insects killed in the tiles treated with 25 ml/ ^m² was as follows:

Table 19

It can be seen that this dosage is insufficient, because not all insects were eliminated after 24 hours.

The following percentages were obtained for the tiles treated with 35 ml/ ^m² :

Table 20

Here, although more insects were eliminated after 24 hours, not all of them were. Therefore, this dosage was still insufficient.

The following percentages were obtained from the tiles treated with 50 ml/ ^m² :

Table 21

Here, the dosage was sufficient: all the insects were eliminated after 24 hours.

Claims (10)

1. A composition of encapsulated permethrin and emulsified dextromethorphan in water, characterized in that the mass ratio of permethrin to dextromethorphan is between 5:1 and 20:1. 2. The composition according to claim 1, wherein the mass ratio of phenylephrine to d-propynephrine is 10:1. 3. The composition according to claim 1, characterized in that the permethrin is microencapsulated. 4. The composition according to claim 3, characterized in that the specific particle size of phenylephrine is between 1.8 μm and 3.3 μm. 5. The composition according to any one of claims 1 to 4, characterized in that the composition is formulated in conjunction with an ultraviolet stabilizer. 6. The composition according to any one of claims 1 to 4, characterized in that the concentration of phenoxy ... 7. The composition according to any one of claims 1 to 4, characterized in that the concentration of phenoxy ... 8. The use of the composition according to claim 7 as an insecticide. 9. The application of the insecticide according to claim 8, characterized in that it is applied to a non-porous surface at a concentration of 20 ml/ ^m² to 60 ml/ ^m² . 10. The application of the insecticide according to claim 8, characterized in that it is applied to a porous surface at a concentration of 40 ml/ ^m² to 120 ml/ ^m² .