A mite-killing composition containing spirobudiclib and clofentezine

Abstract

The present invention relates to a mite killing composition containing spirobudiclib and clofentezine and a use thereof, wherein the weight percentage of the active ingredients spirobudiclib and clofentezine is 1:50-50:1. The mite killing composition can produce a relatively high synergistic effect, overcome and delay the generation of insecticide resistance, has a fast mite killing speed, a long lasting effect period, and reduces the cost of medicine. The present invention can prevent and kill plant pests, especially has an outstanding effect on harmful mites such as citrus panonychus mites, and its effect is significantly better than that of a single agent.

Description

Technical Field

[0001] The invention relates to a miticide composition, in particular to a miticide composition containing spirobudiclib and clofentezine and application thereof. Background Art

[0002] Agricultural pest mites are small, fast-growing, highly adaptable, and easy to develop drug resistance. They are important pests of fruit trees, vegetables, and agricultural and forestry crops. They mainly harm leaves, tender shoots, flower buds, and fruits, causing leaf, bud, and fruit fall, which can lead to reduced production and weakened tree vigor at the least, or even loss of harvest or death of the entire plant at the worst. In addition, many mites can also spread plant diseases, which are quite harmful. Long-term use of a single acaricide product can easily lead to drug resistance in pest mites. Therefore, it is of great significance to develop and prepare acaricide compositions to prolong the service life of acaricides and slow down the development of resistance of pest mites to single acaricide products.

[0003] The chemical name of spirobudiclofen is: 3-(2,4-dichlorophenyl)-2-oxo-1-oxaspiro[4,5]-dec-3-en-4-yl carbonate butyl ester, CAS number: 1305319-70-3, chemical structure formula:

[0004]

[0005] The mechanism of action of spirobudic acid is to inhibit fat synthesis in the body of harmful mites and block energy metabolism. It is a non-systemic acaricide that controls eggs, nymphs and female adult mites through contact and stomach poisoning. Spirobudic acid has an outstanding egg-killing effect and has good preventive effects on harmful mites at different developmental stages. It can be used in all growth stages of citrus.

[0006] The chemical name of clofentezine is: 3,6-bis(2-chlorophenyl)-1,2,4,5-tetrazine, CAS number: 74115-24-5. Clofentezine is a tetrazine acaricide, embryonic development inhibitor, mainly kills mite eggs, but also has a certain effect on young mites, but is ineffective against adult mites; therefore, the best time to use clofentezine to control mites is the early stage of mites damage. The chemical structure is:

[0007]

[0008] The combination of spirobudiclib and clofentezine can reduce the amount of pesticides used, significantly improve the acaricide effect, reduce environmental pollution, and solve the problem that mites are prone to resistance to a single acaricide. At present, the combination and application of spirobudiclib and clofentezine have not been disclosed at home and abroad. Summary of the invention

[0009] The object of the present invention is to provide a preparation and application of a mite-killing composition containing spirobudiclib and clofentezine, wherein the composition can fully utilize the significant synergistic effect produced by mixing the two active ingredients, improve the control effect, reduce the use cost, and delay the development of insect and mite resistance.

[0010] In order to achieve the above-mentioned object of the invention, the present invention provides a miticide composition containing spirobudiclib and clofentezine, wherein the miticide composition comprises active ingredients spirobudiclib and clofentezine, and the mass ratio of the active ingredients spirobudiclib to clofentezine is 1:50-50:1;

[0011] Further, the mass ratio of spirobudic acid to clofentezine is 1:10-10:1;

[0012] Further, the mass ratio of spirobudic acid dienate to clofentezine is 1:10-5:1;

[0013] Further, the mass ratio of spirobudic acid to clofentezine is 1:5-2:1;

[0014] Alternatively, further, the mass ratio of spirobudic acid to clofentezine is 1:10, 1:5, 1:2, 1:1, 2:1, 5:1, 10:1;

[0015] Furthermore, the acaricide composition contains, in addition to the active ingredient, one or more of the adjuvants, carriers, and solvents permitted by pesticides;

[0016] Furthermore, the sum of the mass of the active ingredients spirobudiclib and clofentezine accounts for 1% to 90% of the composition;

[0017] Furthermore, the sum of the mass of the active ingredients spirobudiclib and clofentezine accounts for 10%-80% of the composition;

[0018] Furthermore, the acaricidal composition can be prepared into an agriculturally acceptable dosage form;

[0019] Furthermore, the dosage forms permitted in agriculture are suspension concentrate and wettable powder;

[0020] Furthermore, the acaricidal composition is used for controlling plant pests;

[0021] Furthermore, the plant is citrus; and the pest is Panonychus mites.

[0022] The advantages of the present invention are:

[0023] 1) The insecticide combination exhibits obvious synergistic effect within a certain ratio range, and the mite killing effect after mixing is significantly better than that of a single agent;

[0024] 2) Reduce the dosage of medicine and reduce costs;

[0025] 3) Spirobudic acid diester and clofentezine have different modes and mechanisms of action. Proper mixing and application of the two components can extend the application life of the pesticide and delay the development of pesticide resistance in pest mites. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical solutions and advantages of the present invention more concise and clear, the present invention is described with the following specific embodiments, but the present invention is by no means limited to these embodiments. The embodiments described below are only preferred embodiments of the present invention, which can be used to describe the present invention and cannot be understood as limiting the scope of the present invention. It should be pointed out that any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

[0027] Preparation

[0028] Preparation Example 1: 20% spirobudic acid·clofentezine suspension (1:1)

[0029] Formula: 10.0% spiroclofen 10.0%, clofenac 1.5%, block polyether 1.5%, modified polyether 4.0%, polycarboxylate 1.5%, glycerol 5.0%, magnesium aluminum silicate 1.0%, kason 0.1%, xanthan gum 0.2%, silicone defoamer 0.5%, and deionized water to make up the balance.

[0030] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in a reactor in sequence, water is added to mix evenly, and the suspension is obtained by high-speed shearing, wet sand grinding, and finally homogenization filtration.

[0031] Preparation Example 2: 15% spirobudic acid·clofentezine suspension (1:2)

[0032] Formula: 5.0% spiroclofen, 10.0% clofenac, 1.0% block polyether, 3.0% modified polyether, 1.0% polycarboxylate, 5.0% glycerol, 0.6% magnesium aluminum silicate, 0.07% kason, 0.14% xanthan gum, 0.5% silicone defoamer, and deionized water to make up the balance.

[0033] Preparation method: Same as Preparation Example 1.

[0034] Preparation Example 3: 15% spirobudic acid·clofentezine suspension (2:1)

[0035] Formula: 10.0% spiroclofen, 5.0% clofenac, 1.5% block polyether, 2.5% modified polyether, 1.5% polycarboxylate, 4.5% glycerol, 0.5% magnesium aluminum silicate, 0.07% kason, 0.2% xanthan gum, 0.5% silicone, and deionized water to make up the balance.

[0036] Preparation method: Same as Preparation Example 1.

[0037] Preparation Example 4: 18% spirobudic acid·clofentezine wettable powder (1:5)

[0038] Formula: 3.0% spirobudic acid diester, 15.0% clofenac, 5.5% sodium naphthalenesulfonate formaldehyde condensate sodium salt, 5.0% sodium lignin sulfonate, 3.5% sodium butylnaphthalenesulfonate, 5.5% white carbon black, and kaolin to make up the balance.

[0039] Preparation method: According to the formula ratio of the example, the active ingredients spirobudic acid diester and clofentezine are added to the carrier, and a surfactant and other functional additives are added thereto, mixed, and then air flow crushed and mixed again to obtain a wettable powder.

[0040] Preparation Example 5: 24% spirobudic acid·clofentezine wettable powder (5:1)

[0041] Formula: 20.0% spirobudic acid diester, 4.0% clofenac, 5.0% sodium naphthalenesulfonate formaldehyde condensate sodium salt, 5.0% sodium lignin sulfonate, 3.0% sodium butyl naphthalenesulfonate, 5.0% white carbon black, and kaolin to make up the balance.

[0042] Preparation method: Same as Preparation Example 4.

[0043] Preparation Example 6: 22% spirobudic acid·clofentezine wettable powder (10:1)

[0044] Formula: 20.0% spirobudic acid diester, 2.0% clofenac, 8.0% sodium naphthalenesulfonate formaldehyde condensate sodium salt, 5.0% sodium lignin sulfonate, 3.5% sodium butylnaphthalenesulfonate, 10.0% white carbon black, and kaolin to make up the balance.

[0045] Preparation method: Same as Preparation Example 4.

[0046] Indoor activity

[0047] Indoor Example 1: Indoor joint action test of spirobudiclib and clofentezine combination on Panonychus mites

[0048] Test basis: NY / T1154.5-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Insecticides Part 5: Ovicidal Activity Test Immersion Method", NY / T1154.7-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Insecticides Part 7: Determination of Combined Action of Mixtures".

[0049] Test target: Panonychus citri McGregor, also known as citrus red spider. Adults, juveniles and young mites use their mouthparts to pierce the host leaves, green branches and fruit skins to suck juice, with leaves being the most seriously damaged. The damaged leaves show numerous small grayish-white spots. In severe cases, the entire leaf loses its green color and turns grayish-white, causing a large amount of leaf fall, affecting tree vigor and yield. Adults, juveniles and young mites all like to live in groups on the main veins, side veins and leaf edges on the back of leaves to cause damage.

[0050] Egg card making: Cut off the broad bean leaves with stalks, insert them into an ampoule bottle with water, and add a certain amount of adult mites. After the adult mites lay eggs for 24 hours, remove the adult mites. The number of eggs on each leaf should be no less than 50, and set aside.

[0051] Test agents: 95% spirobudic acid TC and 95% clofentezine TC, both provided by the Group’s R&D Center.

[0052] Preparation of medicine: dissolve the original medicine in DMF, and then dilute it with an aqueous solution containing 0.1% Tween 80. Dilute it into 5 series of mass concentrations, and the amount of medicine solution for each concentration shall not be less than 50 ml.

[0053] Chemical treatment: After the prepared egg cards are immersed in the chemical solution for 10 seconds, they are transferred to normal conditions (25±5℃, 16h light / d) for culture. The experiment is repeated 4 times, and a blank control is set up. After all the controls are hatched, an investigation is conducted, and the number of hatched eggs and unhatched eggs in each treatment is recorded respectively.

[0054] Calculation formula:

[0055] Hatching inhibition rate % = (number of unhatched eggs / total number of eggs treated) × 100

[0056] Corrected hatching inhibition rate % = (hatching inhibition rate of treatment area - hatching inhibition rate of control area) / (1 - hatching inhibition rate of control area) × 100

[0057] If the hatching inhibition rate in the control area is less than 5%, no correction is required; if the hatching inhibition rate in the control area is between 5% and 20%, correction is required; if the hatching inhibition rate in the control area is greater than 20%, the test needs to be repeated.

[0058] The measured toxicity index (ATI) of the mixture = (LC of the standard agent) 50 / LC of mixture 50 )×100

[0059] Theoretical toxicity index (TTI) of mixture = toxicity index of agent A × percentage of agent A in the mixture + toxicity index of agent B × percentage of agent B in the mixture

[0060] Co-toxicity coefficient (CTC) = (Actual toxicity index (ATI) of mixture / Theoretical toxicity index (TTI) of mixture) × 100

[0061] Evaluation method: CTC ≥ 120 of the compound agent shows synergistic effect; CTC ≤ 80 shows antagonistic effect, and CTC between 80-120 shows additive effect.

[0062] The test results were statistically analyzed using DSP data processing software.

[0063] The test results are shown in Table 1:

[0064] Table 1 Combined effects of spiroclofen and clofentezine on Panonychus citri

[0065]

[0066] The combined toxicity determination of spirobudiclib and clofenazine is shown in Table 1. It can be seen from Table 1 that the co-toxicity coefficients of the mixtures of spirobudiclib and clofenazine in the ratios of 1:10, 1:5, 1:2, 1:1, 2:1, 5:1, and 10:1 are 153.697, 170.046, 181.623, 248.177, 170.404, 158.269, and 131.954, respectively. Therefore, the mixed pair of the two agents of the present invention has a synergistic effect on citrus mites, wherein the co-toxicity coefficients are all greater than 150 at the ratios of 1:10, 1:5, 1:2, 1:1, 2:1, and 5:1, showing significant synergy, and the co-toxicity coefficient is the largest when the ratio is 1:1, that is, the synergistic effect is most obvious.

[0067] Field control effect

[0068] Test method: The test was carried out in the citrus orchard in Daciyan Town, Jiande City. The test agents were 20% spirobudiclofen·clofentezine suspension (1:1), 15% spirobudiclofen·clofentezine suspension (1:2), 15% spirobudiclofen·clofentezine suspension (2:1), 18% spirobudiclofen·clofentezine wettable powder (1:5), 24% spirobudiclofen·clofentezine wettable powder (5:1), 22% spirobudiclofen·clofentezine wettable powder (10:1), 24% spirobudiclofen suspension, and 50% clofentezine suspension. The dosage is shown in Table 2. Each treatment plot was arranged in a random block group, with 2 citrus trees in each plot, 4 replicates for each treatment, and a clear water control.

[0069] Application time: The test was carried out at the early stage of the occurrence of citrus mites.

[0070] Survey time: Survey the insect population base before applying the pesticide, and survey the number of mites once every 3 days, 7 days, and 28 days after applying the pesticide, for a total of 4 surveys.

[0071] Survey method: Mark the tender shoots in five directions (east, south, west, north and center) in each plot, and survey the number of active mites (the sum of young mites, nymphs and adult mites) on 30 damaged leaves in each plot.

[0072] Efficacy calculation formula:

[0073] Control effect % = [1-(number of mites in the control area before treatment × number of mites in the treatment area after treatment) / (number of mites in the control area after treatment × number of mites in the treatment area before treatment)] × 100

[0074] Table 2 Field efficacy of spiroclofen and clofentezine mixed to control Panonychus citri

[0075]

[0076] The test results show that the control effect of the mixture of spirobudiclib and clofentezine was better than that of single agent at 3, 7 and 28 days after application. The control effect of the mixture of spirobudiclib and clofentezine was greater than 90% at 28 days after application. No phytotoxicity was found in any treatment during the test, so it can be used in production.

Claims

1. A mite-killing composition containing spirobudiclib and clofentezine, characterized in that: The acaricidal composition comprises active ingredients of spirobudiclib and clofentezine, and the mass ratio of the active ingredients of spirobudiclib to clofentezine is 1:10-10:

1.

2. The acaricidal composition according to claim 1, characterized in that The mass ratio of spirobudic acid to clofentezine is 1:5-2:

1.

3. The acaricidal composition according to claim 1, characterized in that: The acaricide composition contains not only active ingredients but also one or more auxiliary agents, carriers and solvents permitted by pesticides.

4. The acaricidal composition according to claim 1, characterized in that: The sum of the masses of the active ingredients spirobudiclib and clofentezine accounts for 1% to 90% of the composition.

5. The acaricidal composition according to claim 1, characterized in that: The sum of the masses of the active ingredients spirobudiclib and clofentezine accounts for 10%-80% of the composition.

6. The acaricidal composition according to claim 1, characterized in that: The acaricidal composition can be prepared into a dosage form permitted in agriculture.

7. The acaricidal composition according to claim 6, characterized in that: The dosage forms permitted in agriculture are suspension concentrate and wettable powder.

8. Use of the acaricidal composition according to any one of claims 1 to 7 for controlling plant pests.

9. The use according to claim 8, characterized in that The plant pest is Panonychus citri McGregor.

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