Insecticidal microemulsion composition

Abstract

The insecticidal microemulsion composition compounded by flonicamid and spinetoram provided by the invention can be used for preventing and treating various pests such as aphids, leafhoppers, plant hoppers, thrips and the like, and has a special effect on preventing and treating eggplant thrips. According to the composition disclosed by the invention, the polyether modified organic silicon is added as a synergist, so that the pesticide effect of the flonicamid and spinetoram compound microemulsion can be obviously improved. The polyether modified organic silicon can also reduce the lasting foamability of the pesticide, so that the effect of the pesticide is prevented from being reduced due to foamability of the pesticide liquid.

Description

Technical Field

[0001] The present invention relates to the field of pesticide preparations, and in particular to an insecticide microemulsion composition of flonicamid and spinetoram. Background Art

[0002] At present, pests and diseases are one of the main reasons affecting crop yields. In agricultural production practice, the application of chemical agents is still the most effective means of preventing and controlling crop diseases and pests. However, the use of chemical agents to control crop diseases and pests can easily have a serious impact on the ecological environment: on the one hand, the large-scale application of chemical agents can easily cause agent residues and cause serious pollution to the air, water and soil; on the other hand, the long-term high-dose application of a single chemical agent can easily cause plant pathogenic microorganisms, pests and other target organisms to develop resistance, and will also affect the survival of natural enemies. Several technical means can be used to alleviate or overcome the above problems, such as using green and environmentally friendly pesticide formulations, reducing the use of toxic volatile organic solvents, and extending the effective period; reasonable pesticide compounding, expanding the control spectrum, and improving the control effect, thereby reducing the amount of medicine used, reducing pesticide residues, and delaying the occurrence and development of target biological resistance.

[0003] Therefore, developing pesticide compound formulations with excellent pest and disease control effects and green and environmentally friendly characteristics remains the main task facing technicians in the pesticide field in the long term.

[0004] Fluphenacamide, also known as fl on i cami d in English, is a nicotinamide insecticide developed by Ishihara Sangyo Co., Ltd. of Japan. Its structural formula is as follows:

[0005]

[0006] The molecular formula of flonicamid is C9H6F3N3O, the relative molecular weight is 229.2, and the chemical name is N-cyanomethyl-4-(trifluoromethyl) nicotinamide. It is soluble in water and easily soluble in organic solvents such as methanol and acetone. Fluonicamid works by hindering the sucking action of pests. After the pests ingest the agent, they stop sucking quickly and eventually die of starvation. It is effective against various piercing-sucking mouthparts pests and has good penetration. Fluonicamid can be formulated into water-dispersible granules, suspensions and other dosage forms.

[0007] Spinetoram, also known as spinetoram in English, is a macrolide compound developed by Dow AgroSciences (now Corteva) in the United States. Its structural formula is as follows:

[0008]

[0009] Spinetoram is mainly composed of spinetoram-J (spinetoram-J, 75.5%, molecular formula C 42 H69 NO 10 ) and ethyl spinosad-L (spinetoram-L, 20.7%, molecular formula C 43 H 69 NO 10 ) are a mixture of two compounds, the two have similar physical and chemical properties, are insoluble in water, and are easily soluble in organic solvents such as methanol, ethyl acetate, and xylene. Ethyl spinetoram stimulates the central nervous system of the pests, causing non-functional muscle contraction and tremor failure. The pests suffer from neuromuscular fatigue and eventually die due to long-term excessive excitement. It has stomach poison and contact killing effects, and can be used to control Lepidoptera pests such as Plutella xylostella, Spodoptera exigua, and Rice Leaf Roller, and can also be used to control Thysanoptera pests such as thrips. Ethyl spinetoram can be formulated into water-dispersible granules, suspensions, etc.

[0010] Microemulsion is an environmentally friendly formulation developed by replacing part or all of the organic solvent in emulsifiable concentrate with water. With the help of emulsifiers, liquid pesticides are evenly dispersed in water to form a transparent or translucent O / W state. Microemulsions use a high amount of surfactants, which can easily lead to poor low-temperature stability. If the formulation components are not properly matched, the emulsion is also prone to instability. When used in the field, the diluent will produce suspended matter or precipitate crystals, affecting the deposition and adhesion of the liquid on the target, or clogging the nozzle.

[0011] Eggplant thrips are small and reproduce quickly. They can occur multiple times a year and overlap generations. They can lay eggs in stems, leaves and flowers. Adults and nymphs suck the juice of heart leaves, tender stems and young fruits, and also harm flowers, causing the heart leaves to fail to unfold, tender buds to curl, poor flower pollination and many deformed fruits. Thrips often hide on the back of leaves and in flowers, and are well concealed. General pesticides have poor control effects.

[0012] Chinese patent application CN201310524629.1 discloses an insecticidal composition of spinetoram and flonicamid, and also discloses a variety of formulations including microemulsions and their preparation methods. However, the application only lists the types and content ranges of adjuvants used in various formulations, and does not specifically disclose the formula of any formulation. The specific formula and related quality indicators of any formulation are not given in the examples, and there is no field control efficacy data of the microemulsion of spinetoram and flonicamid.

[0013] Therefore, there is still a need to develop pesticide formulation products combining flonicamid and spinetoram to meet the needs of controlling eggplant thrips. Summary of the invention

[0014] The present invention provides a microemulsion composition of flonicamid and spinetoram, which comprises the following components in terms of mass percentage:

[0015] Fluphenacamide 3-30%, spinetoram 2-6%, emulsifier 13-18%, synergist 2-6%, organic solvent 43-47%, water to make up 100%.

[0016] Preferably, the ratio of flonicamid to spinetoram is 5:1-1:2.

[0017] Preferably, the emulsifier is one or more of agricultural milk series, calcium dodecylbenzene sulfonate, tristyrylphenol polyoxyethylene ether ammonium sulfate, castor oil polyoxyethylene ether phosphate, isomeric tridecanol polyoxyethylene ether, and nonylphenol polyoxyethylene ether.

[0018] Preferably, the synergist is polyether-modified silicone.

[0019] Preferably, the organic solvent is one or more of toluene, xylene, ethyl acetate, butyl acetate, N-formylmorpholine, N,N-dimethyldecylamide, and N-methylpyrrolidone.

[0020] The insecticide microemulsion composition of the present invention is prepared by the following method:

[0021] First, dissolve flonicamid and spinetoram in an organic solvent and stir evenly; then add an emulsifier and a synergist to form an emulsion; finally, add water to make a finished product and test it.

[0022] By adopting the above technical solution, the present invention has the following beneficial effects:

[0023] (1) The insecticidal microemulsion composition of the present invention can be used to control various pests such as aphids, leafhoppers, planthoppers, thrips, etc., and is particularly effective in controlling eggplant thrips. Eggplant thrips have overlapping generations and are good at hiding. Both flonicamid and spinetoram have stomach poisoning and contact killing effects, and have systemic effects, and have various modes of action. They can better solve the problem that eggplant thrips are well hidden and difficult to reach with drugs, thereby effectively controlling them.

[0024] (2) The present invention adds polyether-modified silicone as a synergist, which can significantly improve the efficacy of the composite microemulsion of flunicrocin and spinetoram. In the prior art, there are many pesticide synergistic adjuvants, but not all pesticide active ingredients or formulations are applicable. The present invention specifically selects polyether-modified silicone, which can significantly improve the insecticidal effect of flunicrocin and spinetoram. Surprisingly, it was found that polyether-modified silicone can also reduce the persistent foaming of the agent. If the liquid foams too much, it will increase the difficulty of the pesticide spraying operation and affect the normal operation of the spraying equipment, such as clogging the nozzle, etc. It will also affect the coverage and adhesion ability of the pesticide, resulting in the inability of the liquid to adhere evenly to the crops or pests, thereby reducing the effectiveness of the pesticide. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 The preparation process flow chart of the insecticide microemulsion composition of the present invention is DETAILED DESCRIPTION

[0026] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] Example 1: 20% Fluphenacamide·Spinetoram Microemulsion

[0028] The present invention is further explained below in conjunction with specific implementation modes.

[0029]

[0030]

[0031] The preparation method is as follows:

[0032] Mix flonicamid, spinetoram, butyl acetate, N-formylmorpholine and N,N-dimethyldecylamide and stir evenly.

[0033] Calcium dodecylbenzene sulfonate, tristyrylphenol polyoxyethylene ether ammonium sulfate, isomeric tridecanol polyoxyethylene ether and polyether modified silicone are added to form an emulsion.

[0034] Add water to make the finished product.

[0035] Comparative Example 1:

[0036] The product of Comparative Example 1 was prepared according to the formula and preparation method of Example 1, except that modified soybean oil (Fengbei) was added as a synergist.

[0037] Comparative Example 2:

[0038] The product of Comparative Example 2 was prepared according to the formula and preparation method of Example 1, except that no polyether-modified silicone was added.

[0039] Several batches of the products of the embodiments and comparative examples were prepared and quality indicators were tested. The relevant data are shown in the following table:

[0040]

[0041]

[0042] In Comparative Examples 1 and 2, polyether-modified silicone was not added, which had an impact on the persistent foaming property and did not meet the requirement of ≤ 50 mL. There were no obvious differences in other quality indicators. Without being bound by any theory, the inventor believes that polyether-modified silicone may play a certain defoaming role.

[0043] Example 2: Bioassay experiment

[0044] Referring to the bioassay standard method NY / T1154.1-2006, the drop method was used: Thrips on eggplant leaves were collected and placed in a glass tube for standby. After anesthetizing the eggplant thrips with ether, thrips with the same instar were selected and placed in a petri dish. The thrips in the dish were dropped with a micropipette, 0.1 μL per thrips. After the treatment, they were put into fresh eggplant leaves for feeding. 20 thrips were dropped for each treatment, with 4 replicates set, and a treatment with the corresponding organic solvent without the medicament was set as a control.

[0045] One day later, the experimental data were statistically analyzed, and the mortality rate (%) and corrected mortality rate (%) were calculated. If the control mortality rate < 5%, no correction was needed; if the control mortality rate was between 5% - 20%, correction was needed; if the control mortality rate > 20%, the experiment needed to be redone. Taking the logarithm of the medicament concentration (mg / L) as the independent variable x and the probit value of the corrected mortality rate as the dependent variable y, the virulence regression equations were established respectively, and the EC50 of the single agent and each mixture ratio mixture and the co-toxicity coefficient of the mixture were calculated using DPS software. The co-toxicity coefficient method (CTC) was used to evaluate the interaction of the mixed use of medicaments, that is, CTC ≤ 80 was antagonistic effect, 80 < CTC < 120 was additive effect, and CTC ≥ 120 was synergistic effect.

[0046] The experimental data are shown in the following table

[0047] EC50 ATI TTI CTC Spinetoram 0.248 100 Fluphenacamide 1.758 14.11 2:1 0.259 95.75 71.37 134.17 1:1 0.284 87.32 57.05 153.06 1:2 0.397 62.47 42.74 146.17 1:3 0.506 49.01 35.58 137.75 1:4 0.532 46.62 31.29 149.00 1:5 0.620 40.00 28.42 140.73

[0048] It can be seen that when the ratio of flonicamid to spinetoram is in the range of 5:1 - 1:2, the co-toxicity coefficient is greater than 120, and a synergistic effect can be produced.

[0049] Example 3: Field experiment

[0050] Experimental time and location: In mid-March, it was carried out in a vegetable base greenhouse in Shouguang City, Shandong Province.

[0051] Test medicaments: The 20% flonicamid·spinetoram microemulsion prepared in Example 1 of this application, the control medicaments in Comparative Examples 1 and 2, and a water control.

[0052] Experimental method: A total of 12 plots were set, arranged in a randomized block design, and the plot area was 20 m 2Example 1, Comparative Examples 1 and 2, and clear water control were repeated 3 times each. The agent was sprayed by 30 ml of microemulsion diluted with 50 kg of water per mu, and sprayed on eggplant plants. The insect population base of eggplant thrips was counted before application, 1 day after application, and 3 days after application, and the control effect was calculated. The calculation formula is as follows:

[0053]

[0054] Experimental results:

[0055]

[0056] It can be seen from the above experimental data that the sample of Example 1 of the present application has a good preventive effect on eggplant thrips, reaching more than 75% one day after the drug, and up to nearly 90% three days after the drug. There is no obvious difference in the preventive effect of Comparative Examples 1 and 2, both of which are around 65%. Although the synergist modified soybean oil is added to Comparative Example 1, it has no effect on the microemulsion of the present application. It is worth mentioning that the agents of Comparative Examples 1 and 2 produce more foam when diluted with water, and it does not subside for a long time. In the later stage of spraying, the nozzle will be blocked, and foam is easily sprayed, resulting in uneven spraying of the liquid medicine.

[0057] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An insecticide microemulsion composition, characterized in that: In terms of mass percentage, it contains the following components: Fluphenacamide 3-30%, spinetoram 2-6%, emulsifier 13-18%, synergist 2-6%, organic solvent 43-47%, water to make up 100%.

2. The insecticidal microemulsion composition according to claim 1, characterized in that: The ratio of flonicamid to spinetoram is 5:1-1:

2.

3. The insecticidal microemulsion composition according to claim 1, characterized in that: The emulsifier is one or more of agricultural milk series, calcium dodecylbenzene sulfonate, tristyrylphenol polyoxyethylene ether ammonium sulfate, castor oil polyoxyethylene ether phosphate, isomeric tridecanol polyoxyethylene ether, and nonylphenol polyoxyethylene ether.

4. The insecticidal microemulsion composition according to claim 1, characterized in that: The synergist is polyether-modified silicone.

5. The insecticidal microemulsion composition according to claim 1, characterized in that: The organic solvent is one or more of toluene, xylene, ethyl acetate, butyl acetate, N-formylmorpholine, N,N-dimethyldecylamide, and N-methylpyrrolidone.

6. The method for preparing the insecticidal microemulsion composition according to any one of claims 1 to 5, characterized in that: The following steps are involved: First, dissolve flonicamid and spinetoram in an organic solvent and stir evenly; then add an emulsifier and a synergist to form an emulsion; finally, add water to make a finished product and test it.

7. Use of the insecticidal microemulsion composition according to any one of claims 1 to 5 or the insecticidal microemulsion composition prepared by the preparation method of claim 6 in controlling crop pests.

8. The use of the insecticide microemulsion according to claim 7, characterized in that: The crop pests include aphids, leafhoppers, plant hoppers, and thrips.

9. The use of the insecticide microemulsion according to claim 8, characterized in that: The crop pest is eggplant thrips.

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