阅读说明：本技术 一种含毒氟磷的防治大田作物植物病毒病组合物 (Composition containing Dufulin for preventing and treating field crop plant virus diseases ) 是由 于晓静 张建建 李玉艳 李洪侠 吴磊 成道泉 郑志明 曹同波 成晓彤 张淑艳 于 2021-01-14 设计创作，主要内容包括：本发明属于农药领域,提供了一种含毒氟磷的防治大田作物植物病毒病组合物,该组合物以毒氟磷和(1S,3S)-N’-(环己基亚甲基)-1-甲基-2,3,4,9-四氢吡啶并[3,4-b]吲哚-3-甲酰肼为有效成分,且有效成分占总成分的重量百分比为18％-50％；该组合物可用于防治果树、蔬菜、大田作物的病毒病,并且药效显著提高,还可以有效提高作物的抗逆性,调节作物生长,促开花、提高产量、提高果实品质等。(The invention belongs to the field of pesticides, and provides a composition containing Dufulin for preventing and treating field crop plant virus diseases, which takes Dufulin and (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide as effective components, and the effective components account for 18-50% of the total weight of the components; the composition can be used for preventing and treating virus diseases of fruit trees, vegetables and field crops, has obviously improved drug effect, and can also effectively improve the stress resistance of the crops, regulate the growth of the crops, promote flowering, improve the yield, improve the fruit quality and the like.)

1. A composition containing Dufulin for preventing and treating plant virus diseases is characterized in that: the active ingredients of the compound are Dufulin and (1S,3S) -N '- (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formylhydrazine, the weight percentage of the total active ingredients is 18-50%, wherein Dufulin accounts for 8-35% of the weight percentage of the compound composition, and (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formylhydrazine accounts for 10-35% of the weight percentage of the compound composition; the weight ratio of the Dufulin to the (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formylhydrazine is 1:3-5: 1.

2. The composition for controlling plant viral diseases containing Dufulin according to claim 1, wherein:

the weight ratio of the Dufulin to the (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formylhydrazine is 1:2-2: 1.

3. The composition for controlling plant viral diseases containing Dufulin according to claim 1, wherein: the dosage form of the composition is any one of water aqua, soluble solution, soluble powder, suspending agent and water dispersible granules.

Technical Field

The invention belongs to the technical field of pesticides, and provides a composition containing Dufulin for preventing and treating field crop plant virus diseases.

Background

The Dufulin is a novel anti-virus medicament containing fluoro-phosphoramidates, and has a structure of (N- [ 2-4-methylbenzothiazolyl) ] -2-amino-2-fluorophenyl-O, O-diethyl phosphonate), and can improve the content of signal molecules salicylic acid by activating a tobacco salicylic acid signal conduction path, so as to promote the expression of downstream disease course related proteins; obtaining antiviral ability by inducing the activity of PAL, POD and SOD defense enzymes of tobacco; the TMV particles are gathered to reduce the invasion of virus to hosts, and simultaneously, the plant disease resistance is improved to a certain extent.

Dufulin has the structural formula:

(1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-carboxylic acid hydrazide having the structural formula:

the (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide has very good biological activity on tobacco mosaic virus, is easy to be absorbed by plants, is easy to degrade in the environment and has very good environmental compatibility.

The prior art lacks a technical scheme for matching the two substances, and the prior art does not have corresponding technical inspiration, so how to match the two substances with better drug effects becomes one of the problems to be solved in the prior art.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides a composition containing Dufulin for preventing and treating field crop plant virus diseases, which takes Dufulin and (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide as effective components, and the effective components account for 18-50% of the total components by weight. The composition can be used for preventing and treating virus diseases of fruit trees, vegetables and field crops, has obviously improved drug effect, and can also effectively improve the stress resistance of the crops, regulate the growth of the crops, promote flowering, improve the yield, improve the fruit quality and the like.

The specific technical scheme of the invention is as follows:

a composition containing Dufulin for preventing and treating field crop plant virus diseases comprises active ingredients of Dufulin and (1S,3S) -N '- (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, wherein the weight percentage of the total active ingredients is 18% -50%, the Dufulin accounts for 8% -35% of the weight percentage of the compound composition, and the (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide accounts for 10% -35% of the weight percentage of the compound composition;

the weight ratio of the toxic fluorophosphorus to the (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formylhydrazine is 1:3-5:1, and the more preferable range is 1:2-2: 1.

After the two medicaments are combined according to the proportion, the following beneficial effects can be mainly obtained:

activating photosynthesis to promote plant growth, regulating endogenous plant growth factor to promote root growth, recovering leaf function and lowering yield loss;

secondly, the ethylene content is stimulated to increase to cause adverse defense;

thirdly, the protein interacts with virus coat protein to inhibit virus infection;

the three functions exist simultaneously, and have very important significance on the growth of crops.

Meanwhile, the two medicaments are combined to prevent and treat the crop virus diseases, and no adverse reaction occurs to the crops.

The composition can be directly prepared into various dosage forms, mainly comprises any one of water aqua, soluble solution, soluble powder, suspending agent and water dispersible granules, and the specific preparation method is the conventional preparation method in the field, and the inventor does not need to describe any more.

The composition provided by the invention can effectively prevent and control virus diseases of fruit trees, vegetables and field crops, can improve the stress resistance of the crops, promotes the growth of the crops and improves the yield. Compared with the prior art, the invention has the following beneficial effects: the application range of the single preparation of the Dufulin and the (1S,3S) -N '- (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide is expanded, and the compounding of the Dufulin and the (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide can effectively improve the drug effect of the single preparation, can regulate the growth of crops, promote flowering, improve the yield and quality of fruits, have obvious promotion effect on the growth of the crops, and effectively delay the problems of poor control effect and the like caused by the use of the single preparation.

Detailed Description

The present invention will be described in further detail with reference to the following examples, but it should not be construed that the scope of the above subject matter is limited to the following examples. All the technologies realized based on the above contents of the invention belong to the scope of the invention, the following percentages are weight percentages, and the adopted auxiliary agents are all conventional auxiliary agents in the field.

Example 1

Preparation of 18% Dufulin- (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide aqueous solution

The raw materials comprise: 8 percent of Dufulin, 10 percent of (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, 8 percent of surfactant dodecyl benzene sulfonic acid and deionized water to make up to 100 percent. The materials are uniformly mixed in a mixing and stirring kettle according to the corresponding proportion to prepare the aqueous solution of the active ingredient of the toxic fluorine phosphorus (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide with the content of 18 percent.

Example 2

Preparation of 47% Dufulin- (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-carbohydrazide solution

The raw materials comprise: 12% of Dufulin, 35% (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, 2% of sodium nitrate, 2% of ethylene glycol, 4% of Nongru No. 600, 2% of cyclohexanone and acetone to make up to 100%. The materials are uniformly mixed in a mixing and stirring kettle according to the corresponding proportion to prepare the soluble solution of the active ingredient content of 47 percent of Dufulin (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide.

Example 3

Preparation of 38% Dufulin (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide wettable powder

The raw materials comprise: 20% Dufulin, 18% (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, 8% lignosulfonate, 8% alkylsulfonate, 8% citrate and diatomite which are supplemented to 100%. The materials are mechanically crushed, then are crushed by air flow and are evenly mixed, and the wettable powder of Dufulin (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide with the content of active ingredients being 38 percent is prepared.

Example 4

Preparation of 45% Dufulin (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide wettable powder

The raw materials comprise: 35% Dufulin, 10% (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, 8% lignosulfonate, 7% alkylsulfonate, 10% citrate and diatomite which are supplemented to 100%. The materials are mechanically crushed, then are crushed by air flow and are evenly mixed, thus obtaining wettable powder of the active ingredient content of 45 percent Dufulin- (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide.

Example 5

Preparation of 35% Dufulin- (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide suspension

The raw materials comprise: 15 percent of Dufulin, 20 percent of (1S,3S) -N '- (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, 6 percent of sodium lignosulfonate, 1.2 percent of nekal, 1 percent of xanthan gum, 1 percent of SAG622 organosilicon, 8 percent of glycerol, 0.8 percent of sodium tripolyphosphate and the balance of deionized water are used for complementing, and the suspending agent is prepared according to a conventional suspending agent production mode, namely the suspending agent with the effective component content of 35 percent Dufulin (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide.

Example 6

Preparation of 50% Dufulin- (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide suspension

The raw materials comprise: 25% of Dufulin, 25% (1S,3S) -N '- (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, 6% of sodium lignosulfonate, 1.2% of nekal, 1% of xanthan gum, 1% of SAG622 organosilicon, 8% of glycerol, 0.8% of sodium tripolyphosphate and the balance of deionized water, and the suspending agent is prepared by a conventional suspending agent production mode, wherein the suspending agent contains 50% of Dufulin (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide as an active ingredient.

Example 7

Preparation of 45% Dufulin- (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide water dispersible granule

The raw materials comprise: 15% of Dufulin, 30% (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, 10% of lignosulfonate, 6% of alkylsulfonate, 8% of glucose, 4% of corn starch, kaolin and white carbon black, and the balance being 100%. The materials are crushed by an ultramicro jet mill, kneaded, then added into a fluidized bed granulation dryer for granulation, drying and screening, and the water dispersible granule of the Dufulin (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide with the effective component content of 45 percent is prepared.

Example 8

Preparation of 39% Dufulin- (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide water dispersible granule

The raw materials comprise: 26% Dufulin, 13% (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide, 6% alkylnaphthalene sulfonate, 3% naphthalene sulfonate, 4% sucrose, 3% corn starch, and kaolin to make up to 100%. The materials are crushed by an ultramicro jet mill, kneaded, then added into a fluidized bed granulation dryer for granulation, drying and screening, and the water dispersible granule of the Dufulin (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide with the effective component content of 39 percent is prepared.

Experimental example of field drug effect

In order to verify the control effect of the invention on the virus diseases, field control effect verification is respectively carried out on tomato virus diseases and cucurbita pepo virus diseases. The verification results are as follows:

experimental example one of field test: field efficacy test field assay of Dufulin and (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-carbohydrazide compositions against tomato virus disease: after compositions with different contents of (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide and Dufulin are compounded into 8 different dosage forms, foliar spraying is carried out at the early stage of tomato virus disease attack, and the dosage of each treatment per mu is 6ml of the dosage of example 1; example 2 the amount used was 5 ml; the dosage of the examples 3,4, 6 and 7 is 5 g; example 5 in an amount of 6 g; example 8 in an amount of 7.5 g; adding 15L of water into each mu, adding 15L of water into a 30% Dufulin wettable powder serving as a contrast agent, wherein the dosage of a single preparation is 15g, the dosage of a single preparation is 10% (1S,3S) -N' - (4-chlorphenyl methylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide is 15g, and the dosage of an 8% Ningnanmycin water solution is 15ml, and respectively adding 15L of water; the first pesticide spraying is carried out at the early stage of tomato virus diseases, the pesticide spraying is carried out three times, and each time is 7 days apart. And investigating 7d and 14d after three times of medicines respectively, grading according to related data, counting disease indexes, and calculating prevention effect, wherein the results are shown in table 1.

The classification criteria are as follows:

level 0: no disease;

level 1: the area of the lesion spots accounts for less than 8% of the area of the whole leaf;

and 3, level: the area of the lesion spots accounts for less than 6-10% of the area of the whole leaf;

and 5, stage: the area of the lesion spots accounts for less than 11-20% of the area of the whole leaf;

and 7, stage: the area of the lesion spots accounts for less than 21-80% of the area of the whole leaf;

and 9, stage: the lesion area accounts for more than 80% of the whole leaf area.

The efficacy calculation method is as follows:

disease leaf rate (%). diseased leaf number/total leaf number investigated × 100

Disease index ═ Σ (number of diseased leaves at each stage × relative stage value)/(total investigated leaves number × 9) × 100

The prevention and treatment effect (%) is [1- (disease index before drug treatment in the blank control area x disease index after drug treatment in the treatment area)/(disease index after drug treatment in the blank control area x disease index before drug treatment in the treatment area) ] × 100.

TABLE 1 tomato virus control effect of different drug treatments

The field test shows that: the control effect of the mixture of Dufulin and (1S,3S) -N '- (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formylhydrazine on tomato virus diseases is obviously higher than that of Dufulin single dose, 1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formylhydrazine single dose and Ningnanmycin single dose, and the control effect is higher than 46% after 14 days.

Experimental example two of field test: composition of Dufulin and (1S,3S) -N '- (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide on field efficacy test of Cucurbita pepo virus disease after compositions of (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide and Dufulin with different contents are compounded into 8 different dosage forms, foliar spraying is carried out at the initial stage of onset of the Cucurbita pepo virus disease, and the dosage of each treatment per mu is 6ml of example 1; example 2 the amount used was 5 ml; the dosage of the examples 3,4, 6 and 7 is 5 g; example 5 in an amount of 6 g; example 8 in an amount of 7.5 g; adding 15L of water per mu; the contrast agent is 30% Dufulin wettable powder with single dose of 15g, 10% (1S,3S) -N' - (4-chlorphenyl methylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide with single dose of 15g and 8% Ningnanmycin water with dose of 15ml, which are respectively mixed with 15L of water; the first pesticide spraying is carried out at the initial stage of the viral disease of the cucurbita pepo, the pesticide spraying is carried out for three times, and the intervals of 7 days are kept. And investigating 7d and 14d after three times of medicines respectively, grading according to related data investigation standards, counting disease indexes, and calculating prevention effects, wherein the results are shown in Table 2.

The grading standard and the calculation method of the drug effect are the same as above.

TABLE 2 preventive and therapeutic effects on viral diseases of Cucurbita pepo L by different drug treatments

The field test shows that: the control effect of the mixture of Dufulin and (1S,3S) -N '- (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide on the Cucurbita pepo virus diseases is obviously higher than that of the Dufulin single agent, the (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3,4-b ] indole-3-formhydrazide single agent and the Ningnanmycin single agent, and the control effect is higher than 45 percent after 14 days.

Determination of the yield

According to the control effect contrast in earlier stage between different processing of table 1, later stage verification different processing and table 1 the same usage and equal quantity down have the influence to tomato yield, when the tomato fruit is ripe, pick the fruit that is red on the plant and does not have any plant diseases and insect pests in turn, weigh, make statistics of each district output to calculate the rate of increase: yield increase is (treatment zone yield-control zone yield)/control zone yield × 100%.

TABLE 3 Effect of different agent treatments on tomato yield

Table 3 shows that the tomatoes treated by different agents have a certain effect of increasing the yield of the tomatoes, and the yield is increased by 14906.74-31570.01 kg/hm compared with that of a blank control²Has obvious yield increasing effect and the yield increasing rate of the combination of the two medicaments is obviously higher than that of the Dufulin single agent, (1S,3S) -N' - (cyclohexylmethylene) -1-methyl-2, 3,4, 9-tetrahydropyrido [3, 4-b)]Indole-3-formyl hydrazine single agent and ningnanmycin single agent. The two medicaments are combined for use, so that the growth of crops can be obviously regulated, the flowering is promoted, the yield and the quality of fruits are improved, the growth and the development of tomatoes in each cell are normal, no adverse effect is seen, and the test medicaments are proved to be safe and have higher popularization and application values.