Detection method of flonicamid-containing preparation

Abstract

The invention relates to a method for analyzing effective components of a flonicamid-veratrine compound preparation. The effective components flonicamid and veratrine in the compound preparation are quantitatively analyzed at the same time by a high performance liquid chromatography external standard method. The binary compound insecticide taking the flonicamid and the veratrine as the effective components has an obvious synergistic effect, is good in fast-acting property and persistent effect and relatively small in dosage of the effective components, reduces the production cost, and is suitable for preventing and treating aphids on cucumber crops.

Description

[0001] SPECIFICATION TECHNICAL FIELD

[0002] The present application relates to the technical field of pesticide compounding, in particular to a preparation detection method containing flonicamid. BACKGROUND

[0003] Flonicamid is an organic compound with the molecular formula C9H6F3N3O. It belongs to a new type of low-toxicity pyridine amide insect growth regulator insecticide. Flonicamid has not only contact and stomach toxicity, but also good neurotoxicity and rapid antifeeding effect. After aphids and other piercing-sucking mouthpart pests ingest plant sap containing flonicamid, they are quickly prevented from sucking sap, and no excretion occurs within 1 hour, eventually dying of hunger.

[0004] The present agent is effective against various piercing-sucking mouthpart pests and has good penetration. It can penetrate from the roots to the stems and leaves, but the penetration from the leaves to the stems and roots is relatively weak. The agent works by hindering the sucking action of pests. After pests ingest the agent, they quickly stop sucking, and eventually die of hunger. According to the analysis of electronic insect sucking behavior (EMIF), the agent can prevent the stylet tissue of aphids and other sucking pests from inserting into plant tissue and thus works.

[0005] Due to the unique mechanism of action and extremely high biological activity of flonicamid, as well as its extremely high safety to humans, animals and the environment, and its effectiveness against pests resistant to other insecticides, the present agent has great development potential.

[0006] The main chemical components of veratrine are cevadine and veratridine. It has strong irritation and toxicity to mucous membranes. Veratrine exists in plants of the lily family and the genus Eupatorium, and the seeds of Eupatorium and the rhizomes of Veratrum are mainly used as plant raw materials for insecticides. The plant raw materials are extracted with ethanol to obtain the product. Plant-derived insecticides have contact and stomach toxicity on insects. They can be used to control houseflies, cockroaches, lice and other sanitary pests, and also can be used to control cabbage worms, aphids, leafhoppers, aphids and stink bugs.

[0007] Veratrine is an insecticide extracted from Chinese herbal medicine with ethanol, which has contact and stomach toxicity. The main mechanism of action of the agent is that after entering the digestive system through the insect cuticle or sucking, it causes local irritation, leading to reflex excitement of the insect body, first inhibiting the sensory nerve endings of the insect body, and then inhibiting the central nervous system, resulting in the death of the insect. Veratrine has low toxicity to humans and animals, low residue, and does not pollute the environment. Its efficacy can last for more than 10 days, and it is highly effective for the control of vegetable pests.

[0008] In the aspect of agricultural insecticide, long-term application of single chemical agent can easily cause agent residue, environmental pollution and pest resistance, and thus it is urgent to develop a compound insecticide with good insecticidal effect and good speed and persistence. The compound of flonicamid and veratrine meets the requirements of compound insecticide based on indoor toxicology test and field test. SUMMARY

[0009] Based on the above, the present application aims to provide a preparation detection method containing flonicamid, which is suitable for aphid control on cucumber crops.

[0010] The technical solution of the present application is realized by the following measures:

[0011] The present application provides an insecticidal composition containing flonicamid, which comprises flonicamid and veratrine, and the mass ratio of flonicamid to veratrine is 1:(0.1-0.3).

[0012] The insecticidal composition can be prepared into emulsifiable concentrate, suspension concentrate, wettable powder, water emulsion and microemulsion, etc. Preferably, it is a suspension concentrate, which can contain pesticide raw material, dispersant, wetting agent, thickening agent, antifreezing agent, stabilizer and defoaming agent. The mass percentage of each component is as follows: flonicamid 10-30%, veratrine 3-10%, lignin sulfonate (dispersant) 0.3-3%, sodium dioctyl sulfosuccinate (wetting agent) 0.2-1%, magnesium aluminum silicate (thickening agent) 0.2-5%, ethylene glycol (antifreezing agent) 5-10%, white carbon black (stabilizer) 0.1-10% and organosilicone (defoaming agent) 0-5%.

[0013] The insecticidal composition and its preparation have obvious control effect on aphids on cucumber crops.

[0014] The specific embodiments of the pesticide dosage form prepared from the insecticidal composition are as follows:

[0015] The insecticidal composition is an emulsifiable concentrate, and the mass percentage of each component is as follows: flonicamid 10-30%, veratrine 3-10%, emulsifier 5-20%, synergist 2-5% and solvent. The specific production steps of the emulsifiable concentrate are as follows: first, the effective components flonicamid and veratrine are added into the solvent to completely dissolve, then the emulsifier and synergist are added, and the mixture is stirred uniformly to form a uniform transparent oily liquid, which is filled and packaged to prepare the emulsifiable concentrate of the present application.

[0016] The insecticidal composition is a suspension agent, and the mass percentage of the components is: 10-30% of flonicamid, 3-10% of veratrine, 0.3-3% of dispersing agent, 5-10% of antifreezing agent, 0.2-5% of thickening agent, 0-5% of defoaming agent, 0.2-1% of wetting agent, 0.1-10% of stabilizing agent and solvent. The specific production steps of the suspension agent are as follows: other additives are mixed first, uniformly mixed by high-speed shearing, and then flonicamid and veratrine are added, and sand grinding is performed in a sand mill for 2-3 hours to make the particle diameter less than 5 mm, so that the suspension agent preparation of the composition is prepared.

[0017] The insecticidal composition is a wettable powder, and the mass percentage of the components is: 10-30% of flonicamid, 3-10% of veratrine, 2-15% of dispersing agent, 1-5% of wetting agent and filler. The specific production steps of the wettable powder are as follows: flonicamid, veratrine, dispersing agent, wetting agent and filler are mixed according to the above formula, uniformly stirred in a stirring kettle, and then mixed uniformly after air flow crushing, so that the wettable powder of the composition is prepared.

[0018] The insecticidal composition is a water emulsion, and the mass percentage of the components is: 10-30% of flonicamid, 3-10% of veratrine, 3-30% of emulsifier, 3-15% of solvent, 2-10% of stabilizing agent, 2-10% of antifreezing agent, 0.1-8% of defoaming agent, 0.2-5% of thickening agent and water. The specific production steps of the water emulsion are as follows: flonicamid, veratrine, solvent and emulsifier are added first to make the dissolution into a uniform oil phase; other pesticide additives such as part of water and antifreezing agent are mixed together to form a uniform water phase; the oil phase is added to the water phase while stirring at high speed in a reaction kettle, water is slowly added until the phase inversion point is reached, a shearing machine is started for high-speed shearing, the remaining water is added, shearing is performed for about half an hour, an oil-in-water type water emulsion is formed, and the water emulsion of the composition is prepared.

[0019] The insecticidal composition is a microemulsion, and the mass percentage of the components is: 10-30% of flonicamid, 3-10% of veratrine, 15-30% of emulsifier, 1-5% of synergist, 20-35% of cosolvent, 1-5% of penetrating agent, and the rest is water. Flonicamid and veratrine are added to the emulsifier, synergist and other components, uniformly mixed, and then water is added, and the microemulsion is prepared after sufficient stirring.

[0020] The emulsifier is selected from one or a combination of the following: calcium dodecylbenzenesulfonate, fatty acid polyoxyethylene ether, alkylphenol polyoxyethylene ether sulfosuccinate, styrylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty acid polyoxyethylene ester, polyoxyethylene fatty alcohol ether, 2201 emulsifier and 700 emulsifier.

[0021] The solvent is one or a combination of several of xylene, toluene, methanol, ethanol, n-butanol, isopropanol, pine plant oil (code ND-60), solvent oil, dimethyl formamide, dimethyl sulfoxide, water, etc.

[0022] The co-solvent is one or a combination of several of cyclohexanone, alcohol (methanol, ethanol, etc.), phenol (phenol, mixed cresol, etc.), ethyl acetate, dimethyl sulfoxide, etc.

[0023] The dispersant is one or a combination of several of polycarboxylate (code YUS-WG5, TERSPERSE 2700, TERSPERSE 2500), lignin sulfonate (code YUS-WG4, YUS-207K, WLNOK, WLNO100, TERSPERSE 2020), alkyl phenol polyoxyethylene ether methyl ether condensate sulfate, alkyl sulfonate calcium salt, naphthalene sulfonate formaldehyde condensate sodium salt, alkyl phenol polyoxyethylene ether, fatty acid polyoxyethylene ester, fatty amine polyoxyethylene ether, glycerol fatty acid ester polyoxyethylene ether.

[0024] The wetting agent is one or a combination of several of sodium dioctyl sulfosuccinate, sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, Laka powder BX, TERWET 1004, YUS-LXC, TERSPERSE 4894, TERSPERSE 2288, alkyl benzene sulfonate polyoxyethylene triphenyl phosphoric acid salt, soap nut powder, silkworm excrement, soapberry powder.

[0025] The thickening agent is one or a combination of several of xanthan gum, carboxymethyl cellulose, carboxyethyl cellulose, methyl cellulose, magnesium aluminum silicate, polyvinyl alcohol.

[0026] The stabilizer is one or a combination of several of white carbon black, sodium citrate, resorcinol, epoxy soybean oil, epichlorohydrin.

[0027] The antifreeze agent is one of ethylene glycol, glycerol.

[0028] The synergist is one or a combination of several of code SP-4078, organosilicon, high-osmotic anesthetic, de-waxing agent, transdermal agent.

[0029] The defoaming agent is one or a combination of several of silicone oil, silicone compound, C10-20 saturated fatty acid compound, C8-10 fatty alcohol.

[0030] The filler is one or a combination of several of kaolin, diatomite, bentonite, attapulgite, white carbon black, starch, light calcium carbonate.

[0031] The insecticidal composition and its preparation of the present application are toxic to bees and silkworms, and the influence on surrounding bee colonies should be avoided during application, and the insecticidal composition is forbidden to use near flowering plants, silkworm rooms and mulberry fields during flowering period.

[0032] Effects achieved by the present application:

[0033] The compound insecticide with flonicamid and veratrine as effective components has obvious synergistic effect, good quick-acting property and persistence, and is particularly suitable for aphid control on cucumber crops.

[0034] The insecticidal composition of the present application has good insecticidal effect when prepared into wettable powder, and has good stability, good quick-acting property, long persistence time, less use amount of effective components, environmental friendliness, and is suitable for popularization and use. DETAILED DESCRIPTION

[0035] In order to make the technical solutions, objects and advantages of the present application clearer and more apparent, the present application is exemplified by killing aphids, and the following specific examples are used to illustrate the present application.

[0036] In the embodiment of the present application, the operation method of the toxicity test is as follows:

[0037] The indoor toxicity determination is carried out according to the aphid spraying method recommended by FAO (Food and Agriculture Organization of the United Nations). On the basis of pre-test, each pesticide is prepared into 5 concentrations according to equal ratio with pure water containing 0.1% Triton X100. The cucumber leaves planted in the field without contacting the pesticide are beaten into 5.5cm diameter discs, and then the leaves are pasted into 5.5cm diameter culture dishes with the front side facing down. The collected healthy wingless adult aphids are carefully connected to the leaves with a brush, 20 aphids per dish, and then sprayed with a spray head, the spraying amount is 3ml each time, the spraying pressure is 68.9kpa, and then placed into a constant temperature incubator with a temperature of 25℃ and light of L:D=16h:8h for feeding, and the death condition is checked under a dissection microscope after 24h and 48h, the aphids with foot and antenna tremors are live insects, the aphids which are difficult to judge dead or alive are lightly touched with an insect needle, and those without any reaction are considered dead, and the number of dead aphids is counted. Each tube is 1 repetition, each concentration is repeated 3 times, and the clear water is used as a blank control. The toxicity equation and the median lethal concentration LC50 are calculated by the least square method, the toxicity index of the pesticide and the synergistic coefficient (i.e. CTC value) of the mixture are calculated.

[0038] The synergistic effect of the mixed pesticides is evaluated according to the synergistic coefficient (CTC), that is, CTC≤80 is antagonistic effect, 80<CTC<120 is additive effect, and CTC≥120 is synergistic effect.

[0039] The actual toxicity index (ATI) = (LC50 of standard pesticide / LC50 of tested pesticide) x 100;

[0040] Theoretical toxicity index TTI = toxicity index of A × percentage of A in the mixture + toxicity index of B × percentage of B in the mixture;

[0041] Co-toxicity coefficient (CTC) = [measured toxicity index of the mixture (ATI) / theoretical toxicity index of the mixture (TTI)] × 100.

[0042] Example 1: Aphid toxicity test

[0043] The toxicity test was carried out according to the proportions in Table 1, and the results are shown in Table 1.

[0044] Table 1

[0045] Ingredients Ratio LC50 (ug / ml) ATI TTI CTC flonicamid - 4.86 100 - - veratrine - 25.77 18.86 - - flonicamid:veratrine 1:0.1 3.98 122.11 92.62 131.36 flonicamid:veratrine 1:0.2 4.66 104.29 86.47 120.61 flonicamid:veratrine 1:0.3 4.98 97.59 81.27 120.08 flonicamid:veratrine 1:0.5 5.64 86.17 72.96 118.11 flonicamid:veratrine flonicamid:veratrine 1:1 6.88 70.64 59.43 118.86

[0046] The results in Table 1 show that when the ratio of flonicamid to veratrine is 1: (0.1-0.3), the CTC is greater than 120, indicating that the insecticidal composition has a synergistic effect in this ratio range, and shows obvious toxic effect on aphids. And when the ratio of flonicamid to veratrine is 1:0.1, the synergistic effect is significant.

[0047] Example 2: 33% flonicamid·veratrine suspension concentrate

[0048] According to the following weight ratio:

[0049]

[0050] Example 3: 33% flonicamid·veratrine emulsion according to the following weight ratio:

[0051]

[0052] Example 4: 33% flonicamid·veratrine microemulsion according to the following weight ratio:

[0053]

[0054] Example 5: 33% flonicamid·veratrine wettable powder according to the following weight ratio:

[0055]

[0056]

[0057] Example 6: 40% flonicamid·veratrine suspension concentrate according to the following weight ratio:

[0058]

[0059] Example 7: 13% flonicamid·veratrine suspension concentrate according to the following weight ratio:

[0060]

[0061] Comparative Example 1 30% flonicarimicroemulsion was prepared according to the following weight ratio:

[0062]

[0063] Example 8 Field trial for controlling aphids

[0064] The test plot was designed according to the standard of "Guidelines for Field Trial of Pesticides (1)" of the State Quality Supervision Administration. Each plot was 20 m 2 in area, and 38 plots were set up with 1.2 m isolation belt between each plot. The spraying method was spraying, and spraying was carried out once with an electric sprayer.

[0065] Test crop: cucumber

[0066] Test agent: Examples 2-7 and Comparative Example 1, water control. Each group of treatments was set up with 4 repeats.

[0067] Active ingredient dosage: 65 g / hm 2

[0068] Test site: Chengmai County, Hainan Province

[0069] Weather condition: sunny or cloudy, slight wind, temperature: 25-32℃, relative humidity: 50-75%.

[0070] Investigation method: random sampling was used, 10 plants were marked in each plot, and one compound leaf was recorded for each plant. The number of aphids on the leaves was investigated before spraying. Since it was difficult to distinguish the dead and alive aphids in the field 1 day after spraying, the leaves from each treatment area were randomly collected back to the laboratory to observe the aphid death under a dissecting microscope. The number of residual live aphids on the marked leaves in each treatment plot was investigated 3, 7 and 14 days after spraying.

[0071]

[0072] Table 2 Field trial for controlling aphids

[0073]

[0074]

[0075] The results show that the average control effect of the example agent is more than 82% after 3 days of application, indicating that the example agent has rapid effect; the control effect is still more than 75% after 14 days of application, indicating that the example agent has good persistence, wherein the rapid effect and the persistence of the example 2 suspension agent are obviously better, and the control effect is still 95% after 14 days of application. The example 2 shows that the binary compound ratio of 33% (30% flonicamid + 3% veratrine) has significant field test, which is consistent with the effect of the ratio of 1:0.1 of flonicamid and veratrine in the toxicity test, and thus it can be seen that the present application is suitable for the control of aphids on cucumber crops.

[0076] In the examples of the present application, the effective component dosage is 65g / hm 2 achieves good insecticidal effect (the inventors increase the effective component dosage to 100g / hm 2 and find that the 1d, 3d, 7d and 14d control effects are slightly increased), and the conventional dosage of flonicamid is generally 100g / hm 2 (when the effective component dosage of the comparative example 1 is increased to 100g / hm 2 , the 1d, 3d, 7d and 14d control effects are still significantly lower than those of the example agents), and thus it can be seen that the pesticide preparation of the present application not only has good insecticidal effect, but also has less effective component dosage, thereby reducing the impact on the environment.

[0077] The above content is a further detailed description of the present application in combination with specific embodiments, and the specific implementation of the present application cannot be limited to these descriptions. For ordinary skilled persons in the technical field to which the present application belongs, some simple deductions or substitutions can be made without departing from the concept of the present application.

Claims

1. An insecticidal composition comprising flonicamid, characterized in that: The insecticide composition comprises flonicamid and veratrine, and the mass ratio of flonicamid to veratrine is 1:(0.1-0.3).

2. The insecticidal composition containing flupyradifurone according to claim 1, characterized by: The dosage form of the insecticide composition is emulsifiable concentrate, suspension concentrate, wettable powder, emulsion in water and microemulsion.

3. The insecticidal composition containing flupyradifurone according to claim 1, characterized by: The dosage form of the insecticide composition is suspension concentrate, which can contain pesticide raw material, dispersant, wetting agent, thickening agent, antifreezing agent, stabilizer and defoaming agent.

4. The insecticidal composition containing flupyradifurone according to claim 3, characterized by: The mass percentage of each component in the suspension concentrate is as follows: flonicamid 10-30%, veratrine 3-10%, lignin sulfonate (dispersant) 0.3-3%, sodium dioctyl sulfosuccinate (wetting agent) 0.2-1%, magnesium aluminum silicate (thickening agent) 0.2-5%, ethylene glycol (antifreezing agent) 5-10%, white carbon black (stabilizer) 0.1-10% and organosilicone (defoaming agent) 0-5%.

5. The insecticidal composition according to any one of claims 1 to 4, characterized in that: The insecticide composition is used for killing aphids on cucumber plants.

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