Insecticidal composition as well as preparation method and application thereof

Abstract

The invention provides an insecticidal composition as well as a preparation method and application thereof, and the insecticidal composition comprises the following components in percentage by mass: 2-7% of spinetoram, 2-7% of cyantraniliprole, 0.2-0.8% of a thickening agent, 3-7% of a wetting dispersant, 0.02-0.06% of a defoaming agent, 0.1-0.5% of a preservative and 0.5-3% of an anti-freezing agent. By using the magnesium aluminum silicate compounded thickening agent, the insecticidal composition disclosed by the invention effectively improves the control effect on various noctuidae pests.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of pesticides, and specifically provides an insecticidal composition, a preparation method and application thereof. BACKGROUND

[0002] Spodoptera exigua, Tryporyza incudens, Spodoptera littoralis and Spodoptera exigua belong to the Lepidoptera family, have a mixed diet, strong reproductive capacity, wide adaptability and other abilities, and cause great harm to crops, can harm more than 100 crops, and the larvae will cause notching and holes after feeding on crop leaves, and in severe cases, only leaf veins remain, and also burrow inside, causing plants to lodge, such as Spodoptera littoralis feeding on the heart leaf of corn, Tryporyza incudens boring into the stem of rice, causing dead heart seedlings and dead heart clusters, and if the infestation is severe, it can cause crop yield to decrease by 30%-70%.

[0003] Spinetoram is a highly effective and broad-spectrum biological insecticide, which belongs to the Spinosyns family and is a new generation of derivative obtained by introducing an ethyl group into the molecular structure of Spinosyn. It acts on the acetylcholine receptor (AChR) and gamma-aminobutyric acid (GABA) receptor of insects, interferes with nerve signal transmission, and ultimately paralyzes and kills pests. It has low toxicity to non-target organisms and mammals, and is mainly used to control Lepidoptera, Diptera, Coleoptera and Thysanoptera insects.

[0004] Cyantraniliprole is a second-generation diamide insecticide developed by Codex, which belongs to the ryanodine receptor inhibitor. It mainly causes pests to die by continuously contracting muscles due to excessive release of intracellular calcium ions, and has the characteristics of broad-spectrum, high efficiency and strong systemicity. It has high efficiency in killing Lepidoptera, Coleoptera, Diptera and Hemiptera pests.

[0005] There have been attempts to use these two types of pesticides together in the art (CN103120165A, CN103518733A, CN118947688A), but most of them are limited to studying the proportion and applicable objects of the two, and the specific dosage form is not sufficient.

[0006] Enteromorpha belongs to the large green algae of the Ulvaceae family, and often breaks out to form disasters along the coast of China. Using Enteromorpha or its extract for medical and fertilizer purposes is an important way to turn waste into treasure, fully utilize this resource and solve the disaster problem. SUMMARY

[0007] In one aspect, the present application provides an insecticidal composition comprising spinetoram 2-7%, cyantraniliprole 2-7%, thickening agent 0.2-0.8%, wetting dispersant 3-7%, antifoaming agent 0.02-0.06%, preservative 0.1-0.5%, antifreezing agent 0.5-3% by mass percentage.

[0008] Further, the insecticidal composition is a suspension concentrate

[0009] Further, the wetting dispersant is naphthalene sulfonate formaldehyde condensate, the antifoaming agent is SAG 630, the preservative is sodium benzoate, and the antifreezing agent is propylene glycol.

[0010] Further, the thickening agent is Enteromorpha prolifera extract and magnesium aluminum silicate at a mass ratio of 5:1.

[0011] Further, the Enteromorpha prolifera extract is prepared by the following method: washing, drying and crushing Enteromorpha prolifera to obtain Enteromorpha prolifera dry powder; adding 8 times mass of water to the Enteromorpha prolifera dry powder, extracting at 90°C for 4 hours to obtain an extract; and freeze-drying the extract after concentration to obtain the Enteromorpha prolifera extract.

[0012] Further, the insecticidal composition comprises, by mass percentage, spinetoram 5%, cyantraniliprole 5%, Enteromorpha prolifera extract 0.5%, magnesium aluminum silicate 0.1%, naphthalene sulfonate formaldehyde condensate 5.5%, SAG 630 0.05%, sodium benzoate 0.3%, and propylene glycol 2%, with the balance being deionized water.

[0013] In another aspect, the present application provides a preparation method of the above-mentioned insecticidal composition, which comprises: mixing spinetoram, cyantraniliprole, deionized water and wetting dispersant, and then grinding with a sand mill for 1-4 hours at a grinding temperature ≤50°C, so that the particles of spinetoram and cyantraniliprole are controlled at D90 ≤5 μm; and then adding thickening agent, preservative, antifreezing agent and antifoaming agent in sequence, and mixing uniformly by high-pressure homogenization.

[0014] In another aspect, the present application provides the use of the above-mentioned insecticidal composition in the control of noctuidae pests.

[0015] Further, the noctuidae pest is Spodoptera frugiperda, Sesamia inferens or Spodoptera exigua.

[0016] Further, in the use, the above-mentioned insecticidal composition is foliarly sprayed.

[0017] By compounding Enteromorpha prolifera extract and magnesium aluminum silicate thickening agent, the control effect of the insecticidal composition of the present application, especially on rice large caterpillar of the Helicoverpa genus, is effectively improved under the condition that the basic formulation performance is similar. Since Enteromorpha prolifera polysaccharide has not been reported to have insecticidal activity (only some modified substances have bactericidal and antiviral effects), it may be related to the physiological state regulation of polysaccharides and some protein / peptide components in Enteromorpha prolifera extract on plants or pests. The present application provides an effective way to improve the control effect of spinetoram and cyantraniliprole pesticides, especially on Helicoverpa pests such as rice large caterpillar. DETAILED DESCRIPTION

[0018] Main raw materials and methods of example 1

[0019] Main raw materials:

[0020] Spinetoram, cyantraniliprole, xanthan gum, pectin, polyvinyl alcohol, sodium polyacrylate, carboxymethyl cellulose, magnesium aluminum silicate, naphthalene sulfonate formaldehyde condensate, SAG 630, propylene glycol, sodium benzoate are domestic or imported commercial products.

[0021] Enteromorpha prolifera extract is provided by Shanyang Lianfeng Biotechnology Co., Ltd. The preparation method provided by the company is as follows: Enteromorpha prolifera is washed, dried and crushed to obtain Enteromorpha prolifera dry powder; the Enteromorpha prolifera dry powder is added to 8 times the mass of water, and extracted at 90°C for 4 hours; the extract is concentrated and freeze-dried to obtain.

[0022] Instruments:

[0023] The liquid chromatograph is Agilent 1290; the pulverizer, drying oven, electronic balance, sand mill, high-pressure homogenizer, vibrating screen, pH meter, particle size analyzer and other instruments are domestic conventional models.

[0024] Basic preparation method:

[0025] First, spinetoram and cyantraniliprole technical material are mixed with deionized water and wetting dispersant (such as naphthalene sulfonate formaldehyde condensate), then ground with a sand mill for 1-4 hours, the grinding temperature is ≤50°C, and the particle size of the technical material is controlled at D90≤5μm, then the thickening agent (such as Enteromorpha prolifera extract, xanthan gum, pectin, polyvinyl alcohol, sodium polyacrylate, carboxymethyl cellulose, magnesium aluminum silicate), preservative (such as sodium benzoate), antifreeze (such as propylene glycol), and defoaming agent (such as SAG 630) are added in turn, and then high-speed shearing is performed using a high-pressure homogenizer. After mixing, the suspension concentrate is prepared.

[0026] Basic detection method:

[0027] The mass fraction of active ingredients is detected by a liquid chromatograph, and other physical and chemical properties are determined according to national quality standards.

[0028] Adjustment of thickening agent in Example 2

[0029] Based on the prior art, similar composition preparation experience and previous experiments, the wetting dispersant is selected as naphthalenesulfonate formaldehyde condensate, the defoaming agent is selected as SAG 630, the preservative is selected as sodium benzoate, and the antifreeze is selected as propylene glycol. The research focus of further improving the effect is placed on the thickening agent.

[0030] A variety of types of thickening agents are selected for basic dosage form research: Enteromorpha extract, xanthan gum, pectin, polyvinyl alcohol, sodium polyacrylate, carboxymethyl cellulose, and magnesium aluminum silicate. These excipients are used alone and in combination to produce basic suspension performance, thermal decomposition performance as the main consideration index.

[0031] The results show that the formula using sodium polyacrylate and carboxymethyl cellulose has obvious defects in suspension performance, with a suspension rate of less than 80% and easy to precipitate; the thermal stability of pure polysaccharide thickening agent combination is poor. The polysaccharide plus polyvinyl alcohol or polysaccharide plus magnesium aluminum silicate scheme has generally good basic formulation performance, and multiple formulations can be practical (as shown in Tables 1 and 2).

[0032] Table 1 Formulation of preferred formulations

[0033]

[0034] In Table 1, "Enteromorpha" represents Enteromorpha extract, "silicon" represents magnesium aluminum silicate, "yellow" represents xanthan gum, "fruit" represents pectin, and "olefin" represents polyvinyl alcohol.

[0035] Table 2 Basic performance of preferred formulations

[0036]

[0037]

[0038] Example 3 Field control effect of formulations 1-8 on beet armyworm

[0039] Test crop:

[0040] Corn, growth period is small trumpet period, and the growth is consistent, and the test site is selected in Liufuding test base.

[0041] Test pests:

[0042] Beet armyworm, instar is three to five instar

[0043] Test design:

[0044] Set up treatment group and control group, each treatment is repeated three times, randomly arranged in blocks, and set up protection row, and the control group treatment is "Wodongong" bromocyanoacetamidemethyl acetate emulsion produced by Liufuding.

[0045] Test method:

[0046] Using an electric backpack sprayer with a water capacity of 15L / bucket, spray the pesticide solution evenly onto the corn leaves according to the dosage of 30L / 667㎡.

[0047] Survey Methodology:

[0048] Before applying the pesticide, a five-point sampling method was used to select 10 corn plants at each point to investigate the number of live insects and mark them. Insect population surveys were conducted 1 day and 5 days after pesticide application, and the mortality rate was calculated and the average value was taken.

[0049] Experimental results:

[0050] As shown in Table 3, formulations 1-8 were significantly more effective than the control group treated with cyantraniliprole alone. Formulations 3, 4, 6, and 7 were particularly effective, with mortality rates 3-5% higher than the others at both 1 and 5 days post-application.

[0051] Table 3 Field control efficacy against beet armyworm

[0052]

[0053] Example 4: Field control efficacy of formulations 1-8 against fall armyworm

[0054] Experimental crops:

[0055] The rice plants were in the large trumpet stage of their growth period and grew uniformly. The experimental site was located in Lingshan County, Qinzhou City, Guangxi Zhuang Autonomous Region.

[0056] Test pests:

[0057] The fall armyworm has instars from newly hatched larvae to the fifth instar.

[0058] Experimental Design:

[0059] Treatment and control groups were set up, with each treatment repeated three times in a randomized block design and a guard row included. The control group received a combination of ethyl spinosad and bromocyanamide without any synergist.

[0060] Test method:

[0061] Using an electric backpack sprayer with a water capacity of 15L / bucket, spray the pesticide solution evenly onto the rice, according to the dosage of 30L / 667㎡.

[0062] Survey method: In the field, a five-point sampling method was used to select 10 corn plants at each point to investigate the number of live insects before pesticide application and mark them. Insect population surveys were conducted 1 day and 5 days after pesticide application, and the mortality rate was calculated and the average value was taken.

[0063] Test results:

[0064] As shown in Table 4, the overall experimental results were similar to Example 3. Compared with the control group of bromocyclenamide alone, the effects of formulations 1-8 were all obviously better. Among them, the effects of formulations 4, 6 and 7 were better than the others, and the dead insect rates were 3-6% higher than those of other formulations at 1d and 5d after treatment.

[0065] Table 4 Field control effect of formulations 1-8 on Spodoptera exigua

[0066]

[0067]

[0068] Example 5 Field control effect of formulations 1-8 on Diaphania perspectalis

[0069] Test crop:

[0070] Rice, the growth period was jointing and booting stage, and the growth was consistent. The test site was selected in Hanshou County, Changde, Hunan.

[0071] Test pest:

[0072] Diaphania perspectalis, the instar was from newly hatched larvae to the third instar

[0073] Test design:

[0074] Treatment groups and control groups were set up, each treatment was repeated three times, randomly arranged in blocks, and protective rows were set up. The control group was treated with bromocyclenamide suspension concentrate produced by "Wodongong" of Liufuding.

[0075] Test method:

[0076] An electric backpack sprayer was used, the water capacity was 15L / barrel, and the pesticide was sprayed on the rice according to the dosage of 30L / 667m2.

[0077] Investigation method:

[0078] In the field, five-point sampling method was used to select 10 rice plants from each point, the number of live insects before treatment was investigated, and the plants were marked. After 1d and 5d of treatment, the insect population was investigated once, and the dead insect rate was calculated, and the average value was taken. Test results:

[0079] As shown in Table 5, the control effects of each formulation and the control on Diaphania perspectalis were generally not as good as those on Spodoptera exigua or Spodoptera exigua of the control group. Compared with the control group of bromocyclenamide alone, the effects of formulations 1-8 were all obviously better. Among them, the effect of formulation 6 was better than the others, and the dead insect rates were more than 10% higher than those of other formulations at 1d and 5d after treatment.

[0080] Table 5 Field control effect of formulations 1-8 on Diaphania perspectalis

[0081]

[0082]

Claims

1. An insecticidal composition, characterized by comprising, The insecticidal composition comprises, calculated in mass percentage, spinetoram 2-7%, cyantraniliprole 2-7%, thickening agent 0.2-0.8%, wet dispersing agent 3-7%, antifoaming agent 0.02-0.06%, preservative 0.1-0.5%, antifreezing agent 0.5-3%.

2. The insecticidal composition according to claim 1, which is a suspension concentrate.

3. The insecticidal composition according to claim 1 or 2, wherein the wet dispersing agent is naphthalene sulfonate formaldehyde condensate, the antifoaming agent is SAG 630, the preservative is sodium benzoate, and the antifreezing agent is propylene glycol.

4. The insecticidal composition according to any one of claims 1-3, wherein the thickening agent is Enteromorpha extract and magnesium aluminum silicate at a mass ratio of 5:

1.

5. The insecticidal composition according to claim 4, which comprises, calculated in mass percentage, spinetoram 5%, cyantraniliprole 5%, Enteromorpha extract 0.5%, magnesium aluminum silicate 0.1%, naphthalene sulfonate formaldehyde condensate 5.5%, SAG 630 0.05%, sodium benzoate 0.3%, propylene glycol 2%, and the balance is deionized water.

6. The insecticidal composition according to claim 4 or 5, wherein the Enteromorpha extract is prepared by the following method: washing, drying and crushing Enteromorpha to obtain Enteromorpha dry powder; adding the Enteromorpha dry powder into 8 times mass of water, extracting at 90℃ for 4 hours to obtain an extract; and freeze-drying the extract after concentration to obtain the Enteromorpha extract.

7. A process for the preparation of an insecticidal composition according to any one of claims 1 to 6, said process comprising: The spinetoram, cyantraniliprole, deionized water and wet dispersing agent are mixed, and then ground by a sand mill for 1-4 hours at a grinding temperature ≤50℃, so that the particles of spinetoram and cyantraniliprole are controlled at D90≤5μm; then the thickening agent, preservative, antifreezing agent and antifoaming agent are sequentially added, and a high-pressure homogenizer is used for high-speed shearing and mixing.

8. Use of the insecticidal composition according to any one of claims 1-6 in the control of Noctuidae pests.

9. The use according to claim 8, wherein the Noctuidae pest is Spodoptera frugiperda, Conocephalus sp. or Spodoptera exigua.

10. The use according to claim 8 or 9, wherein the insecticidal composition according to any one of claims 1-6 is foliarly sprayed.

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