WO2006058478A1

WO2006058478A1 - Water dispersible granules of abamectin or its derivatives and their production methods

Info

Publication number: WO2006058478A1
Application number: PCT/CN2005/001660
Authority: WO
Inventors: Jiugao Xie; Kaichun Lin; Guoan Zhang
Original assignee: Wuhan Green-Century Bioengineering Company Ltd.
Priority date: 2004-12-03
Filing date: 2005-10-10
Publication date: 2006-06-08

Abstract

The present invention relates to water dispersible granules of abamectin or its derivatives and their production methods. The water dispersible granules are prepared as follows firstly selecting water soluble crystals, for example, saccharides such as sucrose and lactose, inorganic salts such as KCl, NaCl, NH4Cl, Na2SO4, K2SO4, (NH4)2SO4, NaNO3, KNO3, KH2PO4, K2HPO4, NH4H2PO4, or chemical fertilizers such as carbamide, as carriers of the water dispersible granules secondly coating the mixture of methylaminoabamectin benzoate, emulsifiers and high penetrating agents on their surfaces finally dressing the coated granules with powdery dressing agents while wet.

Description

Water-dispersible granule of avermectin or its derivative and preparation method thereof

The invention belongs to the field of pesticide preparation, and particularly relates to a water-dispersible granule of avermectin or a derivative thereof and a preparation method thereof.

Background technique

Avermectins are macrolide antibacterial antibiotics with high-efficiency, broad-spectrum acaricidal and insecticidal activity, stomach poisoning and contact killing effects on mites and insects, and strong permeability. The liquid sprayed on the leaf surface quickly penetrated into the mesophyll to form numerous micro sachets. The adult mites and nymphs and insect larvae immediately appeared paralyzed after taking food and contact with the liquid, inactive, not feeding, 2 - After 4 days, he died. Since the residual leaf surface has few agents and is quickly decomposed into non-toxic substances, it is less harmful to natural enemies.

Emamectin benzoate (hereinafter referred to as "a vitamin salt") is a highly effective insecticidal compound obtained after structural modification of avermectin Bl _a . Its insecticidal activity, especially against the larvae of Helicoverpa armigera, Spodoptera exigua and Spodoptera litura, is much higher than that of avermectin 6, and the toxicity to mammals is greatly reduced. Therefore, the vitamin A has become an important agricultural product for controlling agricultural pests. However, at present, the commercial dosage forms of the Awei salt are relatively single, mainly including emulsifiable concentrates and microemulsions. The water-dispersible granules have not been reported yet and no patent application has been found.

Since the organic solvent content in the emulsifiable concentrate is as high as 90%, the widespread use of emulsifiable concentrates causes environmental pollution of organic solvents, and on the other hand, wastes valuable organic resources. When the wettable powder is produced, there is dust pollution to the environment, and more importantly, the suspension rate of the wettable powder is generally about 70%, which affects the effect of the drug. The microemulsion is essentially a thick emulsion containing about 50% of cosolvent and emulsifier and stabilizer. The cosolvent is actually an organic solvent. Therefore, the microemulsion basically does not solve the waste of organic solvent and environmental pollution. problem.

Summary of the invention

The invention provides a water-dispersible granule of avermectin and its derivative, which is composed as follows The composition is made of: avermectin or its derivative 0.3 ~ 15%, solvent 4 - 30%, emulsifier 1 ~ 15%, coating agent 5 ~ 12%, the balance is carrier material, solvent is dried in granules Recycling in the process.

Preferably, the formazan-dispersed granules of the present invention are prepared from the following components: avermectin or a derivative thereof 0.5 to 10%, a solvent 5 to 15%, an emulsifier 4 to 10%, and a coating agent 4 to 10 %, the balance is the carrier, and the solvent is recovered during the drying of the granules.

The weight percentages of the above components are based on the weight of the final formulation.

Wherein the avermectin derivative is emamectin benzoate.

1. Carrier: a core for use as a water-dispersible granule of avermectin or a derivative thereof of the present invention, selected from the group consisting of: crystallization of disaccharides and monosaccharides such as sucrose, lactose, glucose; urea, KC1, NH ₄ CL KN0 ₃ , K ₂ S0 ₄ , NH ₄ N0 ₃ , (NH ₄ ) ₂ S0 ₄ , NH ₄ HC0 ₃ , ammonium phosphate, potassium dihydrogen phosphate, superphosphate, borax (rapid boron fertilizer produced from borax), ZnS0 ₄ and other commonly used fertilizers and trace element fertilizers in agricultural production, crystals or particles of compound fertilizer; crystals of inorganic salts such as NaCl, Na ₂ S0 ₄ , NaN0 ₃ , Na3⁄4P0 ₄ . One of the above substances may be used as a carrier, or two or more kinds may be used in a ratio of a mixture as a carrier.

2. Solvent: The avermectin or its derivative may be dissolved in a single solvent or a mixed solvent. The solvent is selected from the group consisting of: methanol, absolute ethanol, 95% ethanol, propanol, isopropanol, n-butanol, sec-butanol, tert-butanol, dichloromethane, acetone, ethyl acetate, dimethyl Sulfoxide and N-methylformamide.

3. Emulsifier: It is a mixture of nonionic emulsifier and anionic emulsifier. The nonionic emulsifier is selected from one or more of Span-40, Span-80, Tween 60, and Tween 80. The anionic emulsifier is selected from one or more of sodium dodecyl succinate, sodium dodecyl benzene sulfonate, and sodium dodecyl benzene sulfonate.

'The two-type and cationic emulsifiers have higher cost, poor emulsification efficiency, and have a decomposing effect on pesticides having ester bonds, so they are not used.

The nonionic emulsifier and the anionic emulsifier which we choose have better miscibility, can form a uniform solution quickly, are convenient to use, and have good emulsification effect. 4. Coating agent: selected from dextrin, soluble starch, white carbon black, talcum powder, saponin powder, tea powder (bleaching), carboxymethyl cellulose, kaolin, sodium dodecyl sulfonate, twelve Two or more kinds of substances such as sodium decylbenzenesulfonate and calcium dodecylbenzenesulfonate are mixed, various solvents, various emulsifiers, various coating agents, and various There is no particular requirement for the weight ratio between the carrier phosphates.

The present invention designs a water-dispersible granule of avermectin or a derivative thereof into a three-layer structure of a drug core, a drug layer and a coating layer. The addition of a suitable emulsifier to the drug layer and the coating layer achieves the purpose of allowing the avermectin or its derivative to rapidly disintegrate and uniformly disperse in water.

In addition to the toxicity of avermectin in the granules of the present invention, most other components are substantially non-toxic, more than 80% of the components are easily soluble in water, about 10% of the components are completely emulsified in water, and the components insoluble in water are about 5%, high suspension rate, strong permeability and low toxicity. This dosage form not only maintains the high insecticidal activity of avermectin, but also has the effect of foliar fertilization. Since the preparation does not contain organic solvents such as xylene and toluene, the product is environmentally friendly and is also easy to transport and store. More importantly, it reduces the pollution of the agricultural ecological environment by the above-mentioned toxic organic solvents, which is conducive to the sustainable development of agriculture and food safety. detailed description

Formulation example

Example 1 Preparation of 1% methyl salt dispersion granules

The solvent is prepared by mixing methanol and ethyl acetate in equal proportions. The emulsifier is prepared by mixing Span-80 and calcium dodecylbenzenesulfonate in equal proportions. The coating agent is bleached tea powder, lauryl Sodium benzenesulfonate and dextrin (3:3:4) were thoroughly mixed and pulverized to 400 mesh or more by a jet mill.

First, 1.0 kg of the vitamin A salt (calculated according to the composition of the component) was dissolved in 5 kg of the solvent, and then 12 kg of the emulsifier was added to the solution, and the mixture was thoroughly mixed to form a mixed solution of the methyl salt. Weigh the carrier (white sugar crystal) 79 kg, and put it into a rotary granulator (Beijing Teli Jie Machinery Technology Co., Ltd. TLJ-125 type). The motor is turned on to rotate the drum at a speed of 80 rpm. The prepared mixed solution of the methyl salt was uniformly sprayed onto the surface of the carrier, and then 8 kg of the coating agent was wet-sprayed on the surface of the granules, and the coating was carried out. After the coating is finished, the cold air is blown into the drum, the air temperature is room temperature, and the air drying time is about 1 hour, so that the produced granules are dried. Finally, 99.2 kg of the dry salt of the methacrylate salt was obtained, and the content of the thyme salt (B!) in the granule was 1.01%. Example 2 Preparation of 1.5% Navitamin Salt Dispersible Granules

The solvent is a single solvent, 95% ethanol. The emulsifier is prepared by mixing Tween-60 with sodium dodecylbenzenesulfonate in a ratio of 2:3. The coating agent is thoroughly mixed with sodium dodecyl sulfate, yunyun mother powder and soluble starch (4:3:3) and then pulverized to 400 mesh with a jet mill! 3⁄4 on standby.

^: Accurately weigh 1.5 kg of methicillin salt (calculated according to the content of ^ component), dissolve it with 6 kg of 95% ethanol, and prepare a solution of methyl methacrylate. Add 12 kg of emulsifier to the solution and mix well. The carrier (urea and KC1, 1 : 1, w/w) was weighed and added to a total of 90 kg of solids, which was placed in a self-made stirring granulator. Start stirring and adjust the stirring speed to 120 rpm. The drug substance is slowly added to the granulator through a pipe, coated on the surface of the carrier, and stirred while adding the drug substance. After the addition of the drug substance, the mixture was stirred for 30 minutes and then dampened. 10 kg of the coating agent was applied to the surface of the granules for coating, and the stirring speed during the coating was increased by 100 rpm. After the coating agent was applied, the surface of the granules was dried by blowing at room temperature for 1 hour. The stirring speed should be kept at 60 rpm during the drying process. In this example, 101.5 kg of dried granules of strontium salt were finally obtained, and the content of methicone (Β) in the granules was 1.49%. Example 3 Preparation of 2% Navitamin Salt Dispersible Granules

The solvent was prepared by mixing anhydrous ethanol, isopropanol and dimethyl sulfoxide (6:3:1). The emulsifier is prepared by thoroughly mixing and mixing Tween 80 and sodium dodecyl succinate (2:3). The coating agent consists of saponin powder, dextrin, sodium dodecylbenzene sulfonate and white carbon black (1:2: 4:3) After mixing, it is prepared and pulverized to 400 mesh or more by a jet mill.

Accurately weigh 2 kg of KV salt (calculated according to the content of ^ component), spare. Weigh 8 kg of solvent and 15 kg of emulsifier. After mixing well, add 2 kg of carbaryl salt to it and continue to stir for more than 1 hour. The mixture is completely dissolved and becomes a drug substance. About 72 kg of the carrier (NaN0 ₃ crystal) was weighed, and the carrier material was placed in a rotary granulator to start the granulator. The specific spraying method, coating method and drying method are the same as those in Example 2. The amount of coating agent is 11 kg. Finally, 100.08 kg of a dry salt of the vitamin A was obtained, and the content of the methyl salt (Bj) in the granule was 2.04%. Example 4 Preparation of 3% Navitamin Salt Dispersible Granules

The solvent was homogeneously mixed with dichloromethane, acetone and dimethyl sulfoxide (4:5:1). The emulsifier is prepared by mixing and mixing Span-60 and calcium dodecylbenzenesulfonate (3:7). The coating agent was thoroughly mixed by white carbon black powder (light), carboxymethyl cellulose, soluble starch and sodium dodecylsulfonate (4:3:3:10) and then pulverized to 400 by a jet mill. Above the target.

Accurately weigh 3 kg of K-Mal salt (calculated according to the content of the component), and dissolve it with 10 kg of the above solvent. Further, 16 kg of an emulsifier was added to the solvent, and the mixture was thoroughly stirred to form a drug substance. 70 kg of the carrier (K ₂ S0 ₄ crystal) was weighed and placed in a rotary granulator, and granulated and coated in the same manner as in Example 1. The dosage of the coating agent is 11 kg. In the present example, 98.9 kg of dry KVI brine dispersible granules were obtained. The content of the methyl salt (B!) in the granules was 3.02%. Example 5 Preparation of 4% Navitamin Salt Dispersible Granules

The solvent was prepared by mixing anhydrous ethanol and sec-butanol (3:2). The emulsifier is thoroughly stirred by calcium dodecylbenzenesulfonate, Tween 80, Span-40 and (3:1:1). The coating agent was mixed with saponin powder, diatomaceous earth and sodium dodecylsulfonate (1:1:3), and then pulverized to 400 mesh or more by a jet mill. Accurately weigh out 4 kg of K-Mal salt (calculated according to the content of the components), dissolve it with 12 kg of the above solvent, then add 16 kg of emulsifier, stir well and set aside. In this example, the fast-dissolving boron fertilizer granules were used as the carrier, and the instant boron fertilizer granules were used in an amount of about 68 kg to supplement the solid weight of all the raw materials in this example to 100 kg. Granulation, drying and solvent recovery were carried out as in Example 2. The amount of the coating agent is 12 kg. In this example, 100.4 kg of dry powder of the methicillin salt was finally obtained, and the content of the methicillin ( ) in the granule was 3.99%. Example 6 Preparation of 1% Avermectin Water-Dispersible Granules

The solvent ratio is: isopropanol 60%, dichloromethane 40%, and the two are mixed. The ratio of emulsifier is: Tween 80 60%, calcium dodecylbenzenesulfonate 40%, and the two are mixed well.

The ratio of the coating agent is: Juansi powder 70%, sodium dodecylbenzenesulfonate 30%, the two are thoroughly mixed and pulverized to 325 mesh.

The first step is to accurately weigh 80 kg of solvent and 60 kg of emulsifier. The two are thoroughly mixed into a homogeneous solution. Then we accurately weighed 10 kilograms of avermectin crystals (calculated according to the B _la component). In this case, urea is used as the carrier, and in the third step, 855 kg of urea is accurately weighed. Finally weighed 100 kg of mixed coating agent and the total weight of the material was 1108 kg.

First, 10 kg of avermectin was carefully dissolved in the prepared mixed solution, and the carrier urea was placed on the disc of the granulator to start the machine to reciprocate the disc. The sprayer was started, and the mixed solution in which avermectin was dissolved was uniformly sprayed on the surface of the urea granules until the mixed solution was sprayed. The duster is further turned on, and the coating agent is carefully sprayed on the surface of the above wet granules for coating. It is rapidly air-dried with hot air at 40 ° C until the water content is less than 4%. Finally, 998 kg of dry granules were obtained. The content of B _la component of avermectin in the granules was 1.002% as determined by HPLC. Example 7 Preparation of 2% Avermectin Water-Dispersible Granules The solvent ratio is: 60% n-butanol, 30% dichloromethane, 10% dimethyl sulfoxide, and the three are thoroughly mixed.

The ratio of emulsifier is: Tween 60 70%, calcium 12-dodecylbenzenesulfonate 30%, and the two are well mixed.

The ratio of the coating agent is: soluble starch 85%, sodium dodecylbenzenesulfonate 15%, and the two are thoroughly mixed and pulverized to 325 mesh.

Accurately weigh 80 kg of solvent and 80 kg of emulsifier. The two are thoroughly stirred to form a homogeneous mixed solution. Accurately weigh 20 kg of avermectin crystals (calculated as 8^ components), and dissolve them into the above 160 kg mixed solution to form avermectin B _la solution. In this example, KC1 was used as the carrier, and KC1 836 kg was weighed. Put the avermectin B _la solution into the granulator, start stirring, put 840 kg of the carrier into it and stir for more than 1 hour, then slowly add 100 kg of the mixed coating agent to continue stirring, and from the air inlet to the granulator The hot air of about 40 ° C is blown in the middle, and the granules produced are dried to be a finished product. In this example, 1000 kg of avermectin water-dispersible granules were finally obtained. The content of avermectin B _{Ia in the} granules was 2.01% as determined by HPLC. Example 8 Preparation of 2.5% avermectin water-dispersible granules

Solvent ratio ^ : Anhydrous ethanol 60%, xylene 30% and dimethyl sulfoxide 10%, mixed.

The ratio of emulsifier is: Tween 80 45%, calcium dodecylbenzenesulfonate 55%, and the two are thoroughly mixed.

The ratio of the coating agent is: dextrin 40%, carboxymethylcellulose 10%, sodium dodecylbenzenesulfonate 50%, and the three are mixed and pulverized to 325 mesh.

' Accurately weigh 90 kg of solvent, 90 kg of emulsifier, and mix well to form a mixed solution. Then accurately weigh 25.0 kg of avermectin crystal (calculated according to the B _Ia component), and carefully dissolve it into the above 180 kg mixed solution to become avermectin B _la solution. In this case, sucrose (white sugar) plus urea (2:1) was used as the carrier, and the mixed carrier was weighed. 830 kg, and loaded into the granulator. The granulator was started, and the avermectin mixed solution was sprayed onto the surface of the carrier particles, and then 100 kg of the mixed coating agent was sprayed onto the surface of the granules by a duster to coat. Finally, it is finished by 45 Ό hot air drying. In this example, 1000 kg of avermectin water-dispersible granules were finally obtained, and the avermectin B _la content in the granules was 2.50%. Example 9 Preparation of 1.8% Avermectin Water-Dispersible Granules

The solvent ratio is: anhydrous ethanol 40%, propanol 50% and dimethyl sulfoxide 10%.

The ratio of emulsifier is: calcium dodecylbenzenesulfonate 60%, Tween 40 40%, and the two are thoroughly mixed.

The ratio of coating agent is: white carbon black powder (light) 10%, soluble starch 40%, sodium dodecyl benzene sulfonate 50%, and the three are mixed and pulverized to 325 mesh for use.

Accurately weigh 100 kg of solvent and 70 kg of emulsifier. The two are thoroughly stirred and become a mixed solution. Then accurately weighed 18.0 kg of avermectin crystals (calculated according to the B _la component), and carefully dissolved in the above 180 kg of the mixed solution to become the avermectin B _la solution and charged into the granulator. In this example, NaCl and urea (1:2) were used as carriers, and 845 kg of the mixed carrier was weighed and put into a granulator. The granulation, coating and drying process was carried out according to the method of Example 2, and 1000 kg of avermectin water-dispersible granules were obtained, and the avermectin B _la content in the granules was 1.8%. Example 10 Preparation of 2% Docetaxel Water Dispersible Granules

The solvent is prepared by mixing propanol and methanol (3:2). The emulsifier is prepared by thoroughly mixing the dodecylbenzene sulfonate and Tween 80 (2:3). The coating agent was prepared by mixing white carbon black, dextrin and sodium dodecylbenzenesulfonate (6:1:3), and pulverized to 400 mesh or more by a jet mill.

Accurately weigh 2 kg of doramectin (calculated according to the content of 100%), spare. Weigh 8 again 2 kg of solvent, 3 kg of emulsifier, the two are thoroughly mixed, 2 kg of doramectin is added to it, stirring is continued for more than 1 hour, until the doramectin is completely dissolved, becoming a drug substance. In this example, NaCl and urea (1:2) were used as carriers, and about 76 kg of the mixed carrier was weighed. The carrier material was charged into a rotary granulator to start the granulator. The specific spraying method, coating method and drying method are the same as those in Example 2. The amount of coating agent is 11 kg. Finally, 100 kg of doramectin dry particles were obtained, and the content of doramectin in the granules was 2%. Example 11 Preparation of 3% Doxorubicin Water Dispersible Granules

The solvent was mixed with decyl alcohol, methanol and isopropanol propanol and methanol (1:3:1) for use. The emulsifier is well mixed with calcium dodecylbenzenesulfonate and Span-80 (3:7). The coating agent was prepared by mixing white carbon black, cellulose powder, sodium lignosulfonate and soluble starch (5:2:1:2), and pulverized to 400 mesh or more by a jet mill.

Accurately weigh 3 kg of doramectin (calculated according to the content of 100%), spare. Weigh 12 kg of solvent and 4 kg of emulsifier. After mixing the two wells, add 3 kg of doramectin to it and continue to stir for 1 hour or more until the doramectin is completely dissolved. In this example, KC1 plus urea (1:1) was used as the carrier, and the mixed carrier was added to make up the total amount of solids of 88 kg. The carrier material was charged into a rotary granulator to start the granulator. The specific spraying method, coating method and drying method are the same as those in Example 2. The amount of coating agent is 12 kg. Finally, 100 kg of doramectin dry particles were obtained, and the content of doramectin in the granules was 3%. Biological examples: (Awei saline dispersion granules hereinafter referred to as: TOG)

Example 12 1%, 1.5%, 2%, 3%, 4% five kinds of KM salt dispersed granules and

Comparison of insecticidal activity in 0.6% methyl sulphate

In order to determine whether the insecticidal effect of the inactivated virgin granules of the present invention on the main target pest is the same as that of the same dose of the carbaryl salt, a comparison of the insecticidal activity was carried out. The test insect was a 3rd instar larva of Helicoverpa armigera. The insect-feeding room of the Bt Research and Development Center of Hubei Academy of Agricultural Sciences is fed with artificial feed. Healthy larvae. The measurement method is the blade dipping method: taking the cabbage leaves, immersing in the sample solution for 30 seconds, taking out, drying to the surface of the blade without clear water, writing a label, respectively, and installing a plate, 20 worms per dish. Six concentration gradients were made for each sample. Treated with water as a control. Repeat three times. After 48 hours, the test results were checked, and the median lethal concentration (LC _5Q ) was calculated. The insecticidal activity of the six preparations was tested for significant difference according to the new complex range method. The results are shown in Table 1.

Table 1 Comparison results of insecticidal activities of six kinds of methicone salt preparations against cotton bollworm

The letters a and A are signs of difference significance.

• E.C stands for Emulsion, and WDG stands for water-dispersible granules.

The results in Table 1 show that 1%, 1.5%, 2%, 3%, 4% of five different concentrations of the KM salt dispersed granules prepared by the method of the present invention are compared with the conventional 0.6% KM salt emulsion. There was no significant difference between the insecticidal virulence. Example 13 Effect of 6 Kinds of Synthetic Salt Formulations on Field Control of Spodoptera exigua

The field efficacy test of beet armyworm was carried out on 5 kinds of N-type salt water-dispersed granules prepared by the method of the invention and 0.6% bismuth salt emulsifiable concentrates, such as 1%, 1.5%, 2.0%, 3.0%, 4.0%. The test crop was cabbage, and the control object was beet armyworm/y3⁄4 e^ ^ The majority of the larvae were from the end of the first to the second. Dilute all 6 preparations into the liquid A comparative test was carried out under the same conditions of the same active ingredient concentration. The spray volume is 60 kg of potion per acre. Repeat three times for each treatment. The number of pests was investigated at 2, 3 and 7 days after the drug, and the mortality and control effects were calculated. Spray water as a blank control. The significance of the difference between the treatments was tested by the new complex range method. The experimental results are shown in Table 2. Table 2 Effect of 6 kinds of methicone salt preparations on field control of beet armyworm

The test shows that the KM salt dispersion granule prepared by the method of the present patent has the same effect on the field control effect of the beet armyworm, and the field holding time can be guaranteed. More than 7 days. Example 14 Effect of 6 Kinds of Synthetic Salt Formulations on Controlling Spodoptera litura in the Field

': In order to further verify the insecticidal effects of the five kinds of the Krabi salt dispersible granules of the present invention, Spodoptera liturci ^^m was controlled. The field control targets are mainly 1 ~ 2 instar larvae and a few 3rd instar larvae. The test crop is steamed bread. With clear water as a blank control, 0.6% Awei salt oil was used as a standard drug control. Dilute the 6 kinds of thymite salt preparations to the insecticidal active component (spray at the same concentration of BJ, spray the amount of 100 liters per square meter. Repeat three times per treatment. 1 day after spraying, 3 The number of pests in the field was investigated in days and 5 days, and the control effect was calculated. The difference test method was the same as in Example 7.

The experimental results are shown in Table 3. As can be seen from Table 3, there is no significant difference in the effect of the one-dimensional salt-dispersed granules of this patent on the control of Spodoptera litura at the same concentration. Table 3 Comparison of the effects of six kinds of avidin salt preparations on the control of Spodoptera litura

Example 15

The insecticidal activity of the 1% avermectin water-dispersible granules of Example 6 against Plutella xylostella was determined. Test insects: Plutella xyhstella larvae of Plutella xylostella, bred by Wuhan Tianhui Bioengineering Co., Ltd., and feedstuffs are cotyledons of rapeseed sprouting.

Test insect age: 3rd instar larvae.

Test method: 'Leaf impregnation method. Take the leaves of Shanghai green cabbage, take it in the sample solution for 30 seconds, take it out, and dry it to the surface of the leaf without clear water, and install the plate, each three leaves. Use an insect pen to gently pick the test insects as consistent as possible into the dish, 20 worms per dish. Each concentration was set to 3 replicates, counting 60 worms. Each sample was diluted to 5 concentrations. With clear water as the blank control, 1.8% avermectin EC was used as the standard drug control. Repeat three times. Check the test results after 48 hours.

Table 1 Comparison of insecticidal activity of 1% avermectin water-dispersible granules with 1.8% avermectin emulsifiable concentrate in Example 6

* The letter a is a significant difference sign, both a, indicating that the bioactivity of 1% water-dispersible granules is comparable to that of 1.8% avermectin EC at the same concentration, with no significant difference. Example 16

The insecticidal activity of 2% avermectin water-dispersible granules in Example 7 and 1.8% avermectin water-dispersible granules in Example 9 against spider mites was measured.

Test insects: Citrus leafhopper (

Dr , collected from the citrus garden of Huazhong Agricultural University.

Insect age: If you become a cockroach.

Test method: Slide impregnation method: Apply double-sided tape to one end of the slide, in the dissection mirror Select a strong leafhopper, gently pick it up with a small brush, and make it back down, gently stick to the tape. Each slide has 25 worms, 4 pieces per concentration, and 100 worms. After standing for 2 hours and confirming that there is no dead insect, immerse one end of the slideworm in the liquid to be tested, take it out after 5 seconds, and blot the excess liquid with absorbent paper. The test results were examined under a dissecting microscope after standing at room temperature for 24 hours. With clear water as a blank control, 1.8% avermectin EC was used as a standard drug control.

Table 2 Comparison of insecticidal activities of 2.0% and 1.8% avermectin water-dispersible granules with 1.8% avermectin emulsifiable concentrate in Examples 7 and 9.

* The letter a is a significant difference marker, and all three are a, indicating that there is no significant difference between the three dosage forms. Example 17

The insecticidal activity of 2.5% avermectin water-dispersible granules in Example 8 against cotton bollworm was determined.

Test insects: Helicoverpa armpits othis armigera ), purchased from the B.t Research and Development Center of the Hubei Academy of Agricultural Sciences.

Insect-like insect state: newly hatched larvae.

Test method: Mixed feed method. See the Ministry of Agriculture industry standards for specific methods of operation.

Table 3 Comparison of insecticidal activity of 2.5% avermectin water-dispersible granules and 1.8% avermectin emulsifiable concentrate in Example 8 LC ₅₀ (active ingredient g/ml) LC50 agent mean and difference repeat 1 repeat 2 repeat 3

Heterogeneity *

2.5% water dispersible 12.07 10.89 11.42 11.46 ^a granule

1.8% emulsifiable concentrate 9.97 11.62 10.87 10.82 ^a

* The letter a is the difference significance mark, both of which are a, indicating that there is no significant difference between the three dosage forms.

Datian Application Example

The avermectin water-dispersible granules prepared in the present invention were compared with 1.8% emulsifiable concentrates for field insecticidal effects, and the insects in the field control were larvae of the second to third instar larvae, and the crops were pakchoi. Spray application at a dose of 60 kg of water per acre. The comparison results are as follows:

1. The carrier is urea. The concentration of the chemical solution is 0.1 g / kg 0.05 g / kg 0.025 g / kg.

(active ingredient) water water water

24-hour control (%) 87.71 73.96 65.79

48 hours control (%) 97.76 92.93 89.81

2. The main component of the carrier is urea. The concentration of the drug solution is 0.1 g / kg 0.05 g / kg 0.025 g / kg (active ingredient) water water water

24-hour control (%) 84.77 72.93 67.11

48 hours control effect (%) 98.47 94.62 89.19

3. The main component of the carrier is KC1 concentration of 0.1 g / kg 0.05 g / kg 0.025 g / kg (active ingredient) water water water

24-hour control (%) 84.33 72.11 71.47 48 hours control (%) 98.64 94.60 -: 86.11, the main component of the carrier is NaCl plus urea (1: 2, w/w) concentration of 0.1 g / kg 0.05 g / kg 0.025 g / kg (active ingredient) water Water

² 4 hours control effect (%:) 89.00 80.13 72.95

48 hours control (%) 100 92.21 89.63, carrier is sucrose solution concentration 0.1 g / kg 0.05 g / kg 0.025 g / kg (active ingredient) water water water

24-hour control (%) 90.34 86.17 78.52

48 hours control (%) 100 94.12 89.97, control (1.8% avermectin EC) concentration 0.1 g / kg 0.05 g / kg 0.025 g / kg (active ingredient) water water water

^24- hour control (%) 87.09 83.80 77.51

48 hours control (%) 97.54 92.17 89.95

Claims

Claim

A water-dispersible granule of avermectin or a derivative thereof, characterized in that the components are used in the following percentages by weight:

Abamectin or its derivatives 0.3 - 15%, solvent 4 ~ 30%, emulsifier 1 ~ 15%, coating agent 5 ~ 12%, carrier 45 ~ 85%.

2. The water-dispersible granule according to claim 1, wherein the avermectin derivative is emamectin benzoate or ethyl avermectin benzoate. Acid salt, or doramectin.

3. The water-dispersible granule according to claim 1 or 2, wherein the solvent is one or more selected from the group consisting of methanol, absolute ethanol, 95% ethanol, and propanol. Isopropanol, n-butanol, sec-butanol, tert-butanol, dichloromethane, acetone, ethyl acetate, dimethyl sulfoxide and N-methylformamide.

The water-dispersible granule according to claim 1 or 2, wherein the emulsifier is a mixture of a nonionic emulsifier and an anionic emulsifier.

5. The water-dispersible granule according to claim 4, wherein the nonionic emulsifier is one or more selected from the group consisting of Span-40, Span-80, Tween 60 , Tween 80.

6. The water-dispersible granule according to claim 4, wherein the anionic emulsifier is one or more selected from the group consisting of sodium dodecyl succinate , calcium dodecylbenzenesulfonate, sodium dodecylbenzenesulfonate.

7. The water-dispersible granule according to claim 1 or 2, wherein the carrier is one or more selected from the group consisting of sucrose, lactose, glucose, KC1, NaCl, and Li ₄ Cl , N _a N0 ₃ , KN0 ₃ , NH ₄ N0 ₃ , KH ₂ P0 ₄ , NaH ₂ P0 ₄ , 丽 43⁄4P0 ₄ , K ₂ S0 ₄ , Na2S0 ₄ , H ₄ HC0 ₃ , (NH ₄ ) ₂ S0 ₄ , ZnS04 , puffed instant boron fertilizer and urea.

The water-dispersible granule according to claim 1 or 2, wherein the coating agent is one or more selected from the group consisting of dextrin, soluble starch, and white carbon. Black, talcum powder, saponin powder, tea powder, carboxymethyl cellulose, juvenile mica powder, sodium dodecyl sulfate, calcium lauryl sulfonate, sodium dodecyl benzene sulfonate and twelve Calcium alkylbenzene sulfonate.

The method for producing a water-dispersible granule according to claim 1 or 2, which comprises the steps of: dissolving avermectin or a derivative thereof in a solvent, and adding an emulsifier to the solution. , mixing, forming a mixed solution of avermectin or a derivative thereof; spraying a mixed solution of avermectin and its derivative onto the surface of the carrier, then coating and drying to prepare avermectin and its derivative particles .