CN106035348A - Bactericidal composition containing SYP-Z048 and triflumizole - Google Patents

Abstract

The invention discloses a bactericidal composition containing pyridoxazole and fluconazole, which belongs to the technical field of pesticide compositions. The active ingredients of the present invention are pyridoxazole and fluconazole, and the ratio of pyridoxazole and flucloconazole is 1-40:40-1. The compound fungicide with pyridoxazole and flubuconazole as active ingredients of the present invention has obvious synergistic effect, prolongs the effective period, expands the scope of application of the product, reduces the number of times of use of the medicament, and delays disease resistance. The emergence of medicinal properties improves the control effect and reduces the cost of farmers' medication.

Description

A kind of bactericidal composition containing pyridoxazole and fluconazole

technical field

The invention relates to the technical field of pesticide compositions, in particular to a fungicidal composition whose active ingredients are pyridoxazole and fluclopyrazole.

Background technique

At present, the application of chemical agents is the most effective means to prevent and control agricultural diseases, but the long-term continuous application of a large number of single fungicides can easily induce the resistance of bacteria. Reasonable chemical fungicide compounding or mixing can expand the bactericidal spectrum, reduce the dosage Improve control effect, reduce phytotoxicity, reduce residue, delay the occurrence and development of fungal drug resistance and drug resistance, etc. Therefore, fungicide compounding is one of the most effective methods to solve the above problems.

The pathogens of capsicum anthracnose are A. capsici and A. fruit rot, which belong to the subphylum Deuteromycetes. The cause of the disease spreads quickly and is difficult to control. It has become the key point and difficulty in the prevention and control of pepper production. However, the existing pesticides for sterilization The control effect of pesticides on pepper anthracnose is not good, the application amount is large and the frequency of spraying is many, which increases the cost and has a serious impact on the environment. Therefore, it is urgent to develop high-efficiency pesticides in production.

Contents of the invention

In order to make up for the above deficiencies and solve the problems of the existing fungicides for the prevention and treatment of pepper anthracnose, such as poor control effect, large amount of application, and many times of application, the invention provides a bactericidal combination containing pyridoxazole and flufenazole The composition can be used to prevent and control various diseases of cereals, melons, fruit trees, vegetables, etc., and the effect on the prevention and treatment of pepper anthracnose is particularly outstanding.

Technical scheme of the present invention is:

A bactericidal composition containing pyridoxazole and fluconazole, the active ingredients are pyridoxazole and fluconazole, and the ratio of pyridoxazole to flucloconazole is 1-40:40-1.

As a preferred solution, the ratio of pyridoxazole to fluconazole is 1-10:10-1. Within this ratio range, the synergistic effect of controlling capsicum anthracnose is more obvious after the combination of pyridoxazole and flufenazole.

As a preferred solution, the ratio of pyridoxazole to fluconazole is 1-2:1-6. Within this ratio and within this range, the synergistic effect of controlling capsicum anthracnose is more obvious after the combination of pyridoxazole and flufenazole.

Further, the ratio of pyridoxazole and fluconazole is 1:4. At this ratio, the synergistic effect of controlling capsicum anthracnose is the most obvious after the combination of pyridoxazole and flufenazole.

As a preferred solution, its dosage form is emulsifiable concentrate, water emulsion, microemulsion, microcapsule and microcapsule suspoemulsion. It has been verified that when the bactericidal composition containing pyridoxazole and fluconazole of the present invention is in the form of emulsifiable concentrate, water emulsion, microemulsion, microcapsule and microcapsule suspoemulsion, the drug effect of preventing and treating capsicum anthracnose is better.

Further, its dosage form is microcapsule suspoemulsion. It has been verified that when the dosage form of the bactericidal composition of the present invention is microcapsule suspoemulsion, the efficacy of preventing and treating pepper anthracnose is the best.

As a preferred solution, the mass fraction of pyridoxazole and fluconazole in the fungicidal composition is 1%-80%.

As a preferred version, the microcapsule suspoemulsion is obtained by uniformly mixing pyridoxazole aqueous emulsion with fluclofenazole microcapsules using urea-formaldehyde resin as the wall material; Pyridoxazole microcapsules are uniformly mixed. The two microcapsule suspoemulsions have good control effects on pepper anthracnose.

Further, the microcapsule suspoemulsion is obtained by uniformly mixing pyridoxazole aqueous emulsion and fluclofenazole microcapsules with urea-formaldehyde resin as the wall material. The microcapsule suspoemulsion has the best control effect on capsicum anthracnose.

The bactericidal composition containing pyridoxazole and fluconazole is used in the prevention and treatment of capsicum anthracnose.

Among the active ingredients of the bactericidal composition containing pyridoxazole and fluconazole of the present invention:

Pyridoxazole was created by Shenyang Research Institute of Chemical Industry. It belongs to sterol synthesis inhibitor fungicides. Chemical name: N-methyl-3-(4-chloro)phenyl-5-methyl-5-pyridine-3-methyl Oxazoline, which has broad-spectrum bactericidal activity, has protective and therapeutic effects and good systemic properties, and can be used to prevent and treat various diseases.

Flufenazole belongs to imidazole fungicides, chemical name: (E)-N-(1-imidazol-1-yl-2-propoxyethylene)-4-chloro-2-trifluoromethylaniline, which has The functions of systemic absorption, protection, treatment and eradication are mainly used for various diseases of cereals, vegetables, fruit trees and other crops.

Combining the active ingredients of different pesticides into pesticides is an effective and fast way to develop and develop new pesticides. After different varieties of pesticides are mixed, they usually show three types: additive effect, synergistic effect and antagonistic effect. However, the specific role cannot be predicted, and can only be understood through a large number of experiments. Compounding and synergizing is an important means of comprehensive prevention and control.

The bactericidal composition containing pyridoxazole and fluconazole of the present invention uses pyridoxazole and fluclofenazole as active ingredients, and the combination of the two according to a certain ratio has obvious synergistic effect on pepper anthracnose and the like. Rather than simple addition of the two drugs, joint toxicity was specifically used for indoor bioassays.

Indoor Toxicity Determination of Pyridoxazole and Flufenazole in Different Proportions of Capsicum Anthracnose Bacteria

Test drug

95% pyridoxazole technical product was provided by Shenyang Chemical Industry Research Institute, and 95% fluconazole technical product was provided by Shanghai Shengnong Biochemical Products Co., Ltd.

experiment method

Pharmacy configuration

Dissolve the original drug with acetone first, and mix the appropriate amount of the two original drugs into different proportions according to the results of the preliminary experiment, and then use acetone to dilute each treatment into several concentration gradients for use.

indoor bioassay

Refer to the "Pesticide Indoor Bioassay Test Guidelines for Fungicides", use the mycelium growth rate method indoors to measure the toxicity of different ratios to the strains, measure the colony diameter with the cross method after 6 days, and calculate the net growth and bacterial counts of each treatment. silk growth inhibition rate.

Net growth (mm) = measured colony diameter -8

The mycelia growth inhibition rate was converted into a probability value (y), and the concentration of the medicinal solution (ug/mL) was converted into a logarithmic value (x), and the regression equation of toxicity (y=a+bx) was obtained by the least square method, and by This calculates the _EC50 value for each agent. At the same time, according to the Wadley method, the synergistic ratio (SR) of the combination of two drugs with different ratios was calculated. SR<0.5 was regarded as antagonistic effect, 0.5≤SR≤1.5 was regarded as additive effect, and SR>1.5 was regarded as synergistic effect. Calculated as follows:

Wherein: a and b are respectively the proportions of the active ingredients pyridoxazole and fluconazole in the combination;

A is pyridoxazole; B is fluconazole

Indoor Toxicity Test Result and Analysis

Indoor toxicity assay results are shown in Table 1;

Table 1 Indoor toxicity test results

It can be seen from Table 1 that the EC ₅₀ of pyridoxazole and flucloxanil against Capsicum anthracnose are 0.1127 mg/L and 0.6749 mg/L, respectively. When the ratio of pyridoxazole and fluclofenazole is 1:10～10:1, the synergistic ratio SR is greater than 1.5, indicating that the mixture of pyridoxazole and fluclofenazole in the range of 1:10～10:1 The synergistic effect was obvious, especially when the ratio of the two was between 1:2 and 1:6, the synergistic effect was more prominent, and the joint toxicity was the highest when the ratio of the two was 1:4.

The beneficial effects of the present invention are:

The compound fungicide with pyridoxazole and flubuconazole as active ingredients of the present invention has obvious synergistic effect, prolongs the effective period, expands the scope of application of the product, reduces the number of times of use of the medicament, and delays disease resistance. The emergence of medicinal properties improves the control effect and reduces the cost of farmers' medication.

detailed description

Formulation example

Example 1 15% pyridoxazole·fluconazole emulsifiable concentrate

5.26g 95% pyridoxazole technical substance, 10.53g 95% flufenazole technical substance, 6g calcium dodecylbenzene sulfonate, 7g phenethylphenol polyoxyethylene ether, solubilizer oil to make up to 100g.

Example 2 15% pyridoxazole·fluconazole emulsifiable concentrate

3.16g 95% pyridoxazole technical substance, 12.63g 95% flufenazole technical substance, 6g calcium dodecylbenzene sulfonate, 7g phenethylphenol polyoxyethylene ether, solubilizer oil to make up to 100g.

Example 3 14% pyridoxazole·fluconazole emulsifiable concentrate

2. 11g 95% pyridoxazole technical substance, 12.63g 95% flufenazole technical substance, 6g calcium dodecylbenzene sulfonate, 7g phenethylphenol polyoxyethylene ether, solubilizer oil to make up to 100g.

Example 4 15% pyridoxazole·fluconazole aqueous emulsion

3.16g 95% pyridoxazole technical product, 12.63g 95% flufenazole technical product, 20g solvent naphtha 150#, 6g phenylethylphenol polyoxyethylene polyoxypropylene ether, 2g fatty alcohol polyoxyethylene ether, 1g castor Sesame oil polyoxyethylene ether, 0.1g n-butanol, 2g ethylene glycol, and water make up to 100g.

Example 5 15% pyridoxazole·fluconazole microemulsion

3.16g 95% pyridoxazole technical drug, 12.63g 95% flufenazole technical drug, 10g mineral spirits 150#, 5g N,N-dimethylformamide, 9g phenylethylphenol polyoxyethylene polyoxypropylene ether , 6g calcium dodecylbenzenesulfonate, 0.1g n-butanol, and water are added to 100g.

Example 6 15% pyridoxazole · flufenazole microcapsule suspension

The present embodiment prepares the microcapsule suspension according to the following method, and the specific steps are as follows:

Add urea and formaldehyde into a three-necked flask equipped with a thermometer and a stirring device, the molar ratio is 1:2.0, after dissolving, add deionized water twice the weight of formaldehyde and urea, adjust the pH value to 8.5 with triethanolamine, and raise the temperature to 70 ℃, stirring at low speed for 1 hour to obtain an aqueous solution of urea-formaldehyde resin prepolymer.

Under normal temperature, 3.16g 95% pyridoxazole original drug and 12.63g 95% fluclofenazole original drug were completely dissolved in 15g solvent naphtha 150#, and 18g of the above-mentioned urea-formaldehyde resin prepolymer aqueous solution, 14g 5% polyoxymethylene resin were added while stirring. Sodium acrylate aqueous solution, 10g water, 10000 rpm high-speed shearing to form a stable O/W emulsion; reduce the rotation speed to 400 rpm, add 1M hydrochloric acid in 5 batches within 60 minutes to adjust the pH value of the system to 2.0, polycondensation reaction for 1 hour Afterwards, the temperature was raised to 60°C to solidify the capsule wall for 1 hour, and then sodium hydroxide was added to adjust the pH value to 7.0, 2.5g Tween-80 and 1.5g sodium lignosulfonate were added, and 15% mass fraction of 1% xanthan gum was added Solution, 2g of ethylene glycol, 0.1g of organosilicon defoamer, add water to make up to 100g to obtain 15% pyridoxazole · flufenazole microcapsule suspension.

Example 7 15% Pyridoxazole · Flufenazole Microcapsule Suspoemulsion

This embodiment prepares 18% flucloconazole microcapsule suspension according to the following method, and the specific steps are as follows:

Add urea and formaldehyde into a three-necked flask equipped with a thermometer and a stirring device, the molar ratio is 1:2.0, after dissolving, add deionized water twice the weight of formaldehyde and urea, adjust the pH value to 8.5 with triethanolamine, and raise the temperature to 70 ℃, stirring at low speed for 1 hour to obtain an aqueous solution of urea-formaldehyde resin prepolymer.

Dissolve 18.95g of 95% fluclofenazole technical substance completely in 15g of solvent naphtha 150# at normal temperature, add 18g of the above-mentioned urea-formaldehyde resin prepolymer aqueous solution, 14g of 5% sodium polyacrylate aqueous solution, 10g of water while stirring, 10000 rpm High-speed shearing forms a stable O/W emulsion; reduce the speed to 400 rpm, add 1M hydrochloric acid in 5 batches within 60 minutes to adjust the pH value of the system to 2.0, and polycondense for 1 hour; then raise the temperature to 60°C to solidify the capsule wall 1 After 1 hour, add sodium hydroxide to adjust the pH value to 7.0, add 2.5g Tween-80 and 1.5g sodium lignosulfonate, then add 15g of 1% xanthan gum aqueous solution, 2g ethylene glycol, 0.1g organic silicon defoamer, Add water to make up to 100g to obtain 18% flucloconazole microcapsule suspension.

Prepare 9% pyridoxazole water emulsion according to the preparation method of water emulsion, formula is as follows: 9.47g 95% pyridoxazole former medicine, 20g solvent naphtha 150#, phenylethylphenol polyoxyethylene polyoxypropylene ether 6g, fat Alcohol polyoxyethylene ether 2g, castor oil polyoxyethylene ether 1g, n-butanol 0.1g, ethylene glycol 2g, xanthan gum 0.1g, water to 100g.

Mix 9% pyridoxazole aqueous emulsion and 18% flufenazole microcapsule suspension at a ratio of 1:2, cut at 10,000 rpm for 10 minutes, and prepare 15% pyridoxazole·flufenazole microcapsules Suspoemulsion.

Example 8 15% Pyridoxazole · Flufenazole Microcapsule Suspoemulsion

This embodiment prepares 9% pyridoxazole microcapsule suspension according to the following method, and the specific steps are as follows:

Add urea and formaldehyde into a three-necked flask equipped with a thermometer and a stirring device, the molar ratio is 1:2.0, after dissolving, add deionized water twice the weight of formaldehyde and urea, adjust the pH value to 8.5 with triethanolamine, and raise the temperature to 70 ℃, stirring at low speed for 1 hour to obtain an aqueous solution of urea-formaldehyde resin prepolymer.

Under normal temperature, 9.47g 95% pyridoxazole former drug is completely dissolved in 15g solvent naphtha 150#, add 16g above-mentioned urea-formaldehyde resin prepolymer aqueous solution, 14g 5% sodium polyacrylate aqueous solution, 10g water while stirring, 10000 rpm Form a stable O/W emulsion by high-speed shearing; reduce the speed to 400 rpm, add 1M hydrochloric acid in 5 batches within 60 minutes to adjust the pH value of the system to 2.0, and polycondense for 1 hour; then raise the temperature to 60°C to solidify the capsule wall After 1 hour, add sodium hydroxide to adjust the pH value to 7.0, add 2.5g Tween-80 and 1.5g sodium lignosulfonate, then add 15g of 1% xanthan gum aqueous solution, 2g of ethylene glycol, and 0.1g of silicone defoamer , add water to make up to 100g, namely obtain 9% pyridoxazole microcapsule suspension.

According to the preparation method of water emulsion, prepare 18% fluconazole water emulsion, the formula is as follows: 18.95g fluconazole, 20g solvent naphtha 150#, phenylethylphenol polyoxyethylene polyoxypropylene ether 6g, fatty alcohol polyoxyethylene ether 2g , castor oil polyoxyethylene ether 1g, n-butanol 0.1g, ethylene glycol 2g, and water to make up to 100g.

Mix 9% pyridoxazole microcapsule suspension and 18% fluclofenazole aqueous emulsion at a ratio of 1:2, cut at 10,000 rpm for 10 minutes, and prepare 15% pyridoxazole · fluclofenazole microcapsules Suspoemulsion.

Field experiment to control pepper anthracnose

experiment method

The experiment was conducted in the chili planting area of Jining City, Shandong Province. In the experiment, each treatment was repeated 4 times, and the random block design was used. The area of the plot was 40m ² , and 5 points were investigated in each plot, and 10 pepper fruits were investigated in each point, and the incidence was recorded by the classification method. degree, the grading standards are as follows:

Grade 0: no lesions;

Level 1: The lesion area accounts for less than 2% of the whole pepper fruit area;

Level 3: The lesion area accounts for less than 3%-8% of the whole pepper fruit area;

Level 5: The lesion area accounts for less than 9%-15% of the whole pepper fruit area;

Level 7: The lesion area accounts for less than 16%-25% of the whole pepper fruit area;

Grade 9: The lesion area accounts for more than 25% of the whole pepper fruit area.

Survey time and frequency

The test was investigated 4 times, before spraying, 7d after the first spraying, and 7d and 14d after the second spraying, and the disease index and control effect were calculated.

Drug efficacy calculation method

Diseased fruit rate (%) = number of diseased fruits/total number of investigated fruits × 100

Disease index = ∑ (number of diseased fruits at all levels × relative level value) / (total number of investigated fruits × 9) × 100

Control effect (%)=[(1-pre-medication condition index of blank control area×treatment area post-drug condition index)/(blank control area post-drug condition index×treatment area pre-drug condition index)]×100

Table 2 shows the field control effects of the same dosage form and different ratios on pepper anthracnose.

Table 2 The field control effect of the same dosage form and different ratios on pepper anthracnose

It can be seen from Table 2 that different proportions of the same dosage forms of mixed medicines were tested according to different dosages. : Under the compound ratio of 4, its preventive effect is all better than single agent and other compound ratios and the preventive effect increases progressively with the increase of dosage.

The field control effects of different formulations with the same ratio on pepper anthracnose are shown in Table 3.

Table 3 Field control effect of different formulations with the same ratio on pepper anthracnose

As can be seen from Table 3, when the two active ingredient ratios and dosages are the same, there are differences in the control effects of different formulations, and the control effect of Example 7 is better than other examples.

In summary, after the present invention mixes pyridoxazole and flufenazole, the two have a synergistic effect on pepper anthracnose within a certain ratio range, and are safe to their target crops; when the dosage forms are different, the medicament There are differences in the prevention and treatment effect, and when the dosage form is the microcapsule suspoemulsion of example 7 in the present invention, the prevention and treatment effect to capsicum anthracnose is better than other several dosage forms. The invention and popularization of the compound preparation are helpful to the prevention and treatment of pepper anthracnose, reduce the use of pesticides, and have very important value to agricultural production.

Claims (10)

1. A bactericidal composition containing pyridoxazole and fluconazole, characterized in that: the active ingredients are pyridoxazole and fluconazole, and the ratio of pyridoxazole and flucloconazole is 1 ~ 40:40 ~1. 2. The bactericidal composition containing pyridoxazole and fluconazole as claimed in claim 1, characterized in that: the ratio of pyridoxazole and flucloconazole is 1-10:10-1. 3. The fungicidal composition containing pyridoxazole and flucloxanil according to claim 1 or 2, wherein the ratio of pyridoxazole to flucloxanil is 1~2:1~6. 4. The bactericidal composition containing pyridoxazole and fluconazole as claimed in claim 3, characterized in that: the ratio of pyridoxazole and fluconazole is 1:4. 5. The bactericidal composition containing pyridoxazole and fluconazole as claimed in claim 1, characterized in that: its dosage form is emulsifiable concentrate, water emulsion, microemulsion, microcapsule and microcapsule suspoemulsion. 6. The bactericidal composition containing pyridoxazole and fluconazole as claimed in claim 5, characterized in that: its dosage form is microcapsule suspoemulsion. 7. as claimed in claim 5 or 6, the bactericidal composition containing pyridoxazole and fluconazole is characterized in that: the massfraction of pyridoxazole and fluconazole in the bactericidal composition is 1%- 80%. 8. as claimed in claim 5 or 6, the bactericidal composition containing pyridoxazole and fluconazole is characterized in that: the microcapsule suspoemulsion is composed of pyridoxazole aqueous emulsion and fluorine with urea-formaldehyde resin as wall material. Obenazole microcapsules are uniformly mixed; or obtained by uniformly mixing fluconazole aqueous emulsion and pyridoxazole microcapsules with urea-formaldehyde resin as the wall material. 9. as claimed in claim 8, the bactericidal composition containing pyridoxazole and flufenazole is characterized in that: said microcapsule suspoemulsion is composed of pyridoxazole aqueous emulsion and fluclofenazole with urea-formaldehyde resin as wall material. The microcapsules are uniformly mixed. 10. as claimed in claim 1, the bactericidal composition containing pyridoxazole and fluconazole is used in the prevention and treatment of capsicum anthracnose.