CN114698637A - Poaceae plant sterilization composition and preparation method and application thereof - Google Patents

Poaceae plant sterilization composition and preparation method and application thereof Download PDF

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Publication number
CN114698637A
CN114698637A CN202111504335.3A CN202111504335A CN114698637A CN 114698637 A CN114698637 A CN 114698637A CN 202111504335 A CN202111504335 A CN 202111504335A CN 114698637 A CN114698637 A CN 114698637A
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composition
agent
prothioconazole
composition according
raw materials
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徐海燕
毕强
苑志军
张芝平
于邦威
王大中
于静静
张艳民
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Shanghai Shengnong Pesticide Co Ltd
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Shanghai Shengnong Pesticide Co Ltd
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/24—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients to enhance the sticking of the active ingredients
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647—Triazoles; Hydrogenated triazoles
    • A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention belongs to the technical field of pesticides, and particularly relates to a gramineous plant sterilization composition and a preparation method and application thereof. The invention provides a gramineous plant bactericidal composition in a first aspect, which comprises a composition I or a composition II; the raw materials for preparing the composition I comprise prothioconazole and/or prochloraz; the raw materials for preparing the composition II comprise prothioconazole and/or tebuconazole. The sterilization composition provided by the invention has a better effect on the sterilization of gramineous plants, can realize the synergistic effect by the synergistic effect of the composition I and the composition II, avoids the occurrence of drug resistance, and has a better effect on the prevention and treatment of wheat rust disease, wheat sharp eyespot, rice sheath blight disease and wheat scab; the composition prepared by the invention has excellent storage stability, does not change at all when stored for two weeks under high temperature in the test process, and improves the use value.

Description

Poaceae plant sterilization composition and preparation method and application thereof
Technical Field
The invention belongs to the technical field of pesticides, and particularly relates to a gramineous plant sterilization composition as well as a preparation method and application thereof.
Background
The infection of germs and the like in the planting process of plants influences the growth of crops, and further directly influences the harvest of the crops, so that the income of farmers is greatly reduced, and even larger cost loss occurs.
Therefore, the infection of crops at the present stage is an important task for drug researchers, with the development of society, the environmental protection requirement on pesticides is improved, the control of some active ingredients is increased, and the research of a drug which is efficient, nontoxic and harmless to the health of drug applicators becomes a significant challenge for the drug researchers. The Chinese patent with the patent application number of 201610727046.2 discloses a prothioconazole and tebuconazole compound suspending agent and a preparation method thereof, wherein the prothioconazole and tebuconazole are compounded in the disclosed patent in the weight ratio of 5: 3, the better control effect on the gibberellic disease is shown, but in the research process, researchers find that the control effect on crops can be further improved on the basis of reducing the active ingredients by optimizing the active ingredients or the auxiliary agents.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides in a first aspect a gramineous bactericidal composition comprising composition i or composition ii;
the raw materials for preparing the composition I comprise prothioconazole and/or prochloraz;
the raw materials for preparing the composition II comprise prothioconazole and/or tebuconazole.
In some preferred embodiments, the weight ratio of prothioconazole to prochloraz is (1-3): (1-5).
In some preferred embodiments, the weight ratio of prothioconazole to prochloraz is 1: 1.
in some preferred embodiments, the weight ratio of prothioconazole to prochloraz is 3: 2.
in some preferred embodiments, the weight ratio of prothioconazole to tebuconazole is (1-10): (10-1).
Further preferably, the weight ratio of the prothioconazole to the tebuconazole is 1: 1.
in some preferred embodiments, the preparation feedstock further comprises auxiliary adjuvants.
In some preferred embodiments, the composition is prepared into at least one of wettable powder, water dispersible granule, suspending agent, suspoemulsion, emulsion in water, microemulsion, microcapsule suspending agent and granule.
Further preferably, the composition I is prepared into a microemulsion.
More preferably, the composition II is prepared into a suspending agent.
In some preferred embodiments, the microemulsion is prepared from raw materials including: composition I, auxiliary agent, water and solvent.
In some preferred embodiments, the suspending agent is prepared from raw materials comprising: composition II, auxiliary agent and water.
In some preferred embodiments, the auxiliary agent is selected from at least one of a thickening agent, a wetting agent, a disintegrating agent, a stabilizing agent, a suspending agent, a dispersing agent, an antifoaming agent, an antifreeze agent, an adsorbent, an emulsifier, a pH adjuster, and the like.
In some preferred embodiments, when a microemulsion is prepared, the auxiliary agents include emulsifiers, defoamers, and antifreeze agents.
In some preferred embodiments, the emulsifier is selected from the group consisting of styrol polyoxyethylene ether, alkylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol polyoxyethylene polyoxypropylene ether phosphate ester, and tristyryl phenol polyoxypropylene polyoxyethylene block copolymer.
Further preferably, the emulsifier comprises styrene phenol polyoxyethylene ether and triphenylethylphenol polyoxypropylene polyoxyethylene block copolymer.
More preferably, the weight ratio of the styrene phenol polyoxyethylene ether to the tristyrylphenol polyoxypropylene polyoxyethylene block copolymer is 1: (2-3.5).
More preferably, the weight ratio of the styrene phenol polyoxyethylene ether to the tristyrylphenol polyoxypropylene polyoxyethylene block copolymer is 1: 2.5.
styrene phenol polyoxyethylene ether with HLB value of 15-16 and model 601, available from Nantong Chen Runji chemical Co., Ltd;
triphenethylphenol polyoxypropylene polyoxyethylene block copolymer, model PEP, available from Shandong Nature bioengineering, Inc.
More preferably, the model of the triphenylethylphenol polyoxypropylene polyoxyethylene block copolymer is PEP type.
After a great deal of creative experimental research by the applicant in the experimental process, the applicant finds that when the styrene phenol polyoxyethylene ether and the tristyrylphenol polyoxypropylene polyoxyethylene block copolymer are added into the system for use together, the stability of the system can be greatly improved, the active ingredients of the composition I or the composition II are prevented from being precipitated in the high-temperature storage process, and the reduction of the drug effect is avoided, and the reason why the phenomenon is caused is presumed to be that: in the system, when styrene phenol polyoxyethylene ether and triphenylethylphenol polyoxypropylene polyoxyethylene block copolymer exist at the same time, along with the rise of temperature, the action form of a composition I existing in the system on the surface of an emulsifier is changed, the bonding strength between hydrogen bonds and oxygen bonds in the triphenylethylphenol polyoxypropylene polyoxyethylene block copolymer is influenced, and the stability between preparation raw materials in the system is further influenced, and the weight ratio of the styrene phenol polyoxyethylene ether to the triphenylethylphenol polyoxypropylene polyoxyethylene block copolymer is 1: 2.5, mixed micelles can be formed between the styrene phenol polyoxyethylene ether and the triphenyl phenol polyoxypropylene polyoxyethylene block copolymer, and micelles mainly comprising the triphenyl phenol polyoxypropylene polyoxyethylene block copolymer are formed, and due to the addition of the styrene phenol polyoxyethylene ether, the charge density on the surfaces of the mixed micelles is increased, so that the high-temperature resistance of the composition prepared by the system is improved, the stability of the composition in the high-temperature storage process is improved, the sedimentation of active ingredients of the composition I is avoided, and the reduction of the pesticide effect is avoided.
In some preferred embodiments, when a suspension is prepared, the auxiliary agents include thickening agents, wetting agents, suspending agents, anti-freezing agents.
In some preferred embodiments, the thickener is at least one selected from xanthan gum, magnesium aluminum silicate, polyvinyl alcohol, and ester thickeners.
In some preferred embodiments, the weight ratio of xanthan gum to magnesium aluminum silicate is 5: (1-3).
Further preferably, the weight ratio of the xanthan gum to the magnesium aluminum silicate is 5: 2.
in the experimental process, the applicant finds that the control of the viscosity of the medicament in the preparation process not only has a certain influence on the efficacy of the composition II, but also influences the suspension rate of the composition II in the use process, so that the selection of a proper type of the thickening agent has a great influence on the control effect of the composition in the use process. The applicant has made extensive and inventive experimental studies to find that the use of xanthan gum and magnesium aluminum silicate as co-thickeners, in combination with other preparation raw materials in the system, can greatly improve the suspension effect during use and the stability during storage of the compositions provided herein, in particular when the weight ratio of xanthan gum to magnesium aluminum silicate is 5: (1-3), the present inventors speculated that the reason for this phenomenon is that: magnesium aluminum silicate's existence, can guarantee the wetting agent in the system and reduce the tendency of becoming thin or destroyed, strengthened the emulsifying capacity of wetting agent to composition II, for composition II provides the spreadability in the system, simultaneously, because of the existence of xanthan gum, can form intertwine's synergism between the three-dimensional space chain structure with magnesium aluminum silicate, promote its steric hindrance effect in the system, when promoting viscosity, avoided active ingredient's settlement, promoted the effect activity in the use.
In some preferred embodiments, the suspending agent comprises white carbon black.
More preferably, the specific surface area of the white carbon black is 150-300m2/g。
More preferably, the white carbon black has a specific surface area of 200m2/g。
White carbon black, type 529, purchased from Rugao Feida chemical plant.
In the present application, the antifreeze agent is not particularly limited as long as the technical solution of the present application can be achieved.
In the present application, ethylene glycol may be used as the antifreeze.
In some preferred embodiments, the preparation feedstock herein further comprises deionized water.
The second aspect of the present invention provides a preparation method of a gramineous plant bactericidal composition, comprising the steps of:
and mixing the composition I or the composition II with auxiliary agents, and stirring to prepare the composition.
The third aspect of the invention provides application of the gramineous plant sterilization composition in preventing and treating powdery mildew, banded sclerotial blight, leaf spot, rust disease and gibberellic disease.
More preferably, the gramineous plant bactericidal composition is used for preventing and treating wheat scab.
Has the advantages that: compared with the prior art, the gramineous plant sterilization composition provided by the invention has the following advantages:
the sterilization composition provided by the invention has a better effect on the sterilization of gramineous plants, can realize the synergistic effect by the synergistic effect of the composition I and the composition II, avoids the occurrence of drug resistance, and has a better effect on the prevention and treatment of wheat rust disease, wheat sharp eyespot, rice sheath blight disease and wheat scab;
the composition prepared by the invention has excellent storage stability, has better stability when stored at high temperature in the test process, and improves the use value.
Drawings
FIG. 1 shows the indoor combined toxicity determination of rice sheath blight disease by different ratios of prothioconazole and tebuconazole;
FIG. 2 shows the indoor combined toxicity determination of rice sheath blight disease by different proportions of prothioconazole and prochloraz;
FIG. 3 shows the indoor combined toxicity measurement of prothioconazole and tebuconazole in different ratios to wheat scab.
Detailed Description
Examples
Example 1
A gramineous plant bactericidal composition comprises a composition I with a mass concentration of 40%;
the preparation raw materials comprise a composition I, auxiliary additives and deionized water.
The preparation raw materials comprise, by weight, 40% of the composition I, 19% of auxiliary additives and 100% of deionized water.
The composition I comprises prothioconazole and prochloraz in a weight ratio of 1: 1.
the auxiliary agent comprises: 12% of emulsifier, 2% of defoaming agent and 5% of antifreeze agent.
The emulsifier is as follows: styrene phenol polyoxyethylene ether and triphenylethylphenol polyoxypropylene polyoxyethylene block copolymer; the weight ratio of the components is 1: 2.5;
the antifoaming agent is HY-462 which is purchased from Beijing Maier chemical engineering Co., Ltd;
the antifreeze agent is glycol.
A preparation method of a gramineous plant bactericidal composition comprises the following steps:
and mixing the composition I and the auxiliary agent, and stirring to prepare the composition.
Example 2
A Gramineae plant bactericidal composition with a mass concentration of 400 g/L;
the preparation raw materials comprise a composition II, auxiliary additives and deionized water.
The preparation raw materials comprise 20g of the composition II, 12g of auxiliary agents and deionized water by weight, and the concentration of the composition is up to 400 g/L.
The composition II comprises prothioconazole and tebuconazole in a weight ratio of 1: 1.
the auxiliary agent comprises: thickening agent, wetting agent, suspending agent and anti-freezing agent.
The auxiliary agent comprises 30% of thickening agent, 25% of wetting agent, 5% of suspending agent and the balance of antifreeze agent to 100% in percentage by weight.
The thickening agent comprises xanthan gum and magnesium aluminum silicate, and the weight ratio of the thickening agent to the thickening agent is 5: 2;
the wetting agent comprises styrene phenol polyoxyethylene ether ammonium sulfate;
styryl phenol polyoxyethylene ether ammonium sulfate salt, purchased from south Tong Han sanden chemical Limited;
the suspending agent comprises white carbon black, and the specific surface area of the white carbon black is 200m2The model 529, is purchased from Rugao Dada chemical factories.
The antifreeze agent is glycol.
A preparation method of a gramineous plant bactericidal composition comprises the following steps:
and mixing the composition II and the auxiliary agent, stirring, grinding and filtering to prepare the composition.
Example 3
A gramineous plant bactericidal composition comprises a composition I with a mass concentration of 40%;
the preparation raw materials comprise a composition I, auxiliary additives and deionized water.
The preparation raw materials comprise, by weight, 40% of the composition I, 19% of auxiliary additives and 100% of deionized water. The composition I comprises prothioconazole and prochloraz in a weight ratio of 3: 2.
the auxiliary agent comprises: 12% of emulsifier, 2% of defoaming agent and 5% of antifreeze agent.
The emulsifier is as follows: styrene phenol polyoxyethylene ether and triphenylethylphenol polyoxypropylene polyoxyethylene block copolymer; the weight ratio of the components is 1: 2.5;
the antifoaming agent is HY-462 which is purchased from Beijing Maier chemical engineering Co., Ltd;
the antifreeze agent is glycol.
A preparation method of a gramineous plant bactericidal composition comprises the following steps:
and mixing the composition I and the auxiliary agent, and stirring to prepare the composition.
Example 4
A gramineous plant bactericidal composition comprises a composition I with a mass concentration of 40%;
the preparation raw materials comprise a composition I, an auxiliary additive and deionized water.
The preparation raw materials comprise, by weight, 40% of the composition I, 19% of auxiliary additives and 100% of deionized water. The composition I comprises prothioconazole and prochloraz in a weight ratio of 2: 4.
the auxiliary agent comprises: 12% of emulsifier, 2% of defoamer and 5% of antifreeze.
The emulsifier is as follows: styrene phenol polyoxyethylene ether and triphenylethylphenol polyoxypropylene polyoxyethylene block copolymers; the weight ratio of the components is 1: 2.5;
the antifoaming agent is HY-462 which is purchased from Beijing Maier chemical engineering Co., Ltd;
the antifreeze agent is glycol.
A preparation method of a gramineous plant bactericidal composition comprises the following steps:
and mixing the composition I and the auxiliary agent, and stirring to prepare the composition.
Example 5
A gramineous plant bactericidal composition is the same as in example 2, except that xanthan gum is used as a thickening agent in example 2.
And (3) performance testing:
firstly, virulence determination:
a: virulence test for composition i:
1. test targets: wheat scab;
2. the culture conditions are as follows: the wheat scab germ is continuously transferred for 2 generations at 26 plus or minus 1 ℃ through PDA culture medium in a room to be used as an experimental strain.
3. The test is according to the method: referring to the second part of 'pesticide indoor bioassay test criteria bactericide': inhibition of pathogenic fungi hyphal growth test plate method (NY/T1156.2-2006) and sixth section: combined effect assay of compounding (NY/T1156.6-2006).
4. Treating a medicament:
under the aseptic operation condition, respectively adding 2.0mL of liquid medicine with different concentrations into a sterilized triangular flask (the standard amount is 50mL) accurately calibrated in advance by using a pipette, then adding a culture medium which is melted and cooled to the appropriate temperature into the triangular flask to the calibrated 50mL scale mark, fully shaking uniformly, pouring the culture medium into 4 culture dishes (the diameter is 9cm) in equal quantity, preparing a PDA plate containing medicine with corresponding concentration, wherein each concentration treatment is divided into 4 times, and the component without containing the effective component of the medicine is used as a blank control.
5. Inoculation: cutting off bacterial cake from the edge of bacterial colony by using a sterilization puncher with the diameter of 5mm under aseptic condition, inoculating the bacterial cake to the center of a drug-containing flat plate by using an inoculator, covering a dish cover, placing the flat plate in a biochemical incubator with the temperature of 26 +/-1 ℃ and the relative humidity of 80% for dark culture, and observing experimental results.
6. Investigation time and method
The colonies in the dishes treated according to the control group grow to 2/3 size of the dish diameter and the experiment is terminated. The diameter of the colonies was measured with a ruler and the diameter was measured perpendicularly every colony by the cross method and averaged (the diameter of the cake was subtracted by 5mm for each measurement).
7. Statistical analysis of data
Calculating the inhibition rate of each treatment concentration on the hypha growth of the test strain according to the measurement result, then calculating the experiment result by using DPS data processing software, and respectively solving the toxicity regression equation and EC of the experiment product50、EC90And 95% confidence limits.
Calculating the hypha growth inhibition rate of each treatment concentration on the target bacteria to be tested according to the formula (1) and the formula (2), and respectively solving the toxicity regression equation and EC of the experimental product50、EC90And 95% confidence limits.
Formula (1);
D＝D1-D2in the formula: d is the colony growing diameter; d1The diameter of the colony is shown; d2The diameter of the fungus cake.
Formula (2):
I＝(D0-Dt/D0) X 100; in the formula: i is the hypha growth inhibition rate; d0Growing the diameter of the colony for the blank control; dtThe colonies grow in diameter for agent treatment.
Calculating co-toxicity coefficient (CTC) according to Sun Yunpei method, and evaluating synergistic effect of the combination of the medicines according to the value of the co-toxicity coefficient (CTC), i.e. the antagonism is achieved when CTC is less than or equal to 80, the additivity is achieved when CTC is more than 80 and less than 120, and the synergy is achieved when CTC is more than or equal to 120. The co-toxicity coefficient (CTC) is calculated according to the formulas (3), (4) and (5).
Formula (3)
ATI is S/M × 100; in the formula: ATI is the measured virulence index of the composition; s is EC of standard medicament50In mg/l; m is EC of the composition50The unit is mg/l.
Formula (4)
TTI＝TIA×PA+TIB×PB(ii) a In the formula: TTI is the theoretical virulence index of the composition; TIAIs the virulence index of prothioconazole; p isAIs the percentage content of the prothioconazole in the composition, unit percentage%; TIBIs toxicity index of prochloraz; pBThe percentage of the prochloraz in the composition is unit percent.
Formula (5)
CTC ═ ATI/TTI × 100; in the formula: CTC is co-toxicity coefficient;
the toxicity test results of the prothioconazole and the prochloraz are recorded in the following table.
Figure BDA0003403550750000081
Figure BDA0003403550750000091
The above experimental results prove that the weight ratio of prothioconazole to prochloraz in the application is 3: 2 and 1: when the toxicity coefficient is 1, the co-toxicity coefficient is more than 120, which shows that the synergistic effect is better.
B: virulence test for composition ii:
test targets: sheath blight of rice
1. The test medicaments of prothioconazole (A) and tebuconazole (B) are respectively prepared into 1.0 multiplied by 10 by using dimethylformamide as a solvent4And (5) putting the mg/L mother liquor in a refrigerator for later use.
2. The ratio of the mixed effective components of the two is prothioconazole: tebuconazole is 3: 1. 2: 1. 1: 1. 1: 2 and 1: 3, preparing into 1.0 multiplied by 104And (4) putting the dimethylformamide mother liquor of mg/L into a refrigerator for later use.
3. On the basis of a pre-test experiment, the mother liquor is diluted by an aqueous solution containing 0.1% of Tween 80, 5 concentrations are designed for each treatment, and the concentrations of two medicaments and different proportions thereof are set as follows:
prothioconazole (a): 0.1, 0.2, 0.4, 0.8, 1.6mg/L
Tebuconazole (B): 0.375, 0.75, 1.5, 3, 6mg/L
A：B(3：1)：0.125、0.25、0.5、1、2mg/L
A：B(2：1)：0.15、0.3、0.6、1.2、2.4mg/L
A：B(1：1)：0.15、0.3、0.6、1.2、2.4mg/L
A：B(1：2)：0.2、0.4、0.8、1.6、3.2mg/L
A：B(1：3)：0.25、0.5、1、2、4mg/L
4. Test basis method
The method refers to a hypha growth rate method (NY/T1156.2-2006) specified in agricultural chemical indoor bioassay test quasi-lateral bactericide and combined action measurement (NY/T1156.6-2006) of bactericide mixing.
5. Drug treatment
Under the aseptic operation condition, respectively adding 2.0mL of liquid medicine with different concentrations into a sterilized triangular flask (the standard amount is 50mL) accurately calibrated in advance by using a pipette, then adding a culture medium which is melted and cooled to the appropriate temperature into the triangular flask to the calibrated 50mL scale mark, fully shaking uniformly, pouring the culture medium into 4 culture dishes (the diameter is 9cm) in equal quantity, preparing a PDA plate containing medicine with corresponding concentration, wherein each concentration treatment is divided into 4 times, and the component without containing the effective component of the medicine is used as a blank control.
6. Inoculation: cutting off bacterial cake from the edge of bacterial colony by using a sterilization puncher with the diameter of 5mm under aseptic condition, inoculating the bacterial cake to the center of a drug-containing flat plate by using an inoculator, covering a dish cover, placing the flat plate in a biochemical incubator with the temperature of 26 +/-1 ℃ and the relative humidity of 80% for dark culture, and observing experimental results.
7. Investigation time and method
The colony in the culture dish treated according to the control group grows to 2/3-4/5 of the diameter of the culture dish, and then the test is stopped. The diameter of the colonies was measured with a ruler, and the diameter was measured perpendicularly by the cross method for each colony, and the average value was taken (the diameter of the cake was subtracted by 5mm for each measurement).
8. Statistical analysis of data
According to the measurement result, the hypha growth inhibition rate of each treatment concentration on the test strain is calculated, then DPS data processing software is used for calculating the experiment result, and the toxicity regression equation and EC of the single agent and the mixed agent with different proportions of the test agent are respectively obtained50、EC90And 95% confidence limits, and finding twoCo-toxicity coefficient (CTC) of different ratios of the medicament, and screening out the optimal ratio of the test medicament
Calculating the hypha growth inhibition rate of each treatment concentration on the target bacteria to be tested according to the formula (1) and the formula (2), and respectively solving the toxicity regression equation and EC of the experimental product50、EC90And 95% confidence limits.
Formula (1);
D＝D1-D2in the formula: d is the colony growing diameter; d1The diameter of the colony is shown; d2The diameter of the fungus cake.
Formula (2):
I＝(D0-Dt/D0) X 100; in the formula: i is the hypha growth inhibition rate; d0Growing the diameter of the colonies for the blank control; dtThe colonies grow in diameter for agent treatment.
Calculating co-toxicity coefficient (CTC) according to Sun Yunpei method, and evaluating synergistic effect of the combination of the medicines according to the value of the co-toxicity coefficient (CTC), i.e. the antagonism is achieved when CTC is less than or equal to 80, the additivity is achieved when CTC is more than 80 and less than 120, and the synergy is achieved when CTC is more than or equal to 120. The co-toxicity coefficient (CTC) is calculated according to the formulas (3), (4) and (5).
Formula (3)
ATI is S/M × 100; in the formula: ATI is the measured virulence index of the composition; s is EC of standard medicament50In mg/l; m is EC of the composition50The unit is mg/l.
Formula (4)
TTI＝TIA×PA+TIB×PB(ii) a In the formula: TTI is the theoretical virulence index of the composition; TIAIs the virulence index of prothioconazole; pAIs the percentage content of the prothioconazole in the composition, unit percentage%; TIBIs the virulence index of tebuconazole; pBIs the percentage content of tebuconazole in the composition and has unit percentage.
Formula (5)
CTC ═ ATI/TTI × 100; in the formula: CTC is co-toxicity coefficient;
the results of the experiment are recorded in fig. 1, in particular in fig. 1.
C: virulence test for composition i:
test targets: sheath blight of rice
1. The test drugs prothioconazole (A) and prochloraz (B) are respectively prepared into 1.0 multiplied by 10 by using dimethylformamide as a solvent4And (5) putting the mg/L mother liquor in a refrigerator for later use.
2. The ratio of the mixed effective components of the two is prothioconazole: the prochloraz is 3: 1. 2: 1. 1: 1. 1: 2 and 1: 3, preparing into 1.0 multiplied by 104And (5) putting mg/L dimethylformamide mother liquor into a refrigerator for later use.
3. On the basis of a pre-test experiment, the mother liquor is diluted by an aqueous solution containing 0.1% of Tween 80, 5 concentrations are designed for each treatment, and the concentrations of two medicaments and different proportions thereof are set as follows:
prothioconazole (a): 0.1, 0.2, 0.4, 0.8, 1.6mg/L
Prochloraz (B): 5. 10, 20, 40 and 80mg/L
A：B(3：1)：0.15、0.3、0.6、1.2、2.4mg/L
A：B(2：1)：0.2、0.4、0.8、1.6、3.2mg/L
A：B(1：1)：0.2、0.4、0.8、1.6、3.2mg/L
A：B(1：2)：0.375、0.75、1.5、3、6mg/L
A：B(1：3)：0.5、1、2、4、8mg/L
4. Test basis method
The method refers to a hypha growth rate method (NY/T1156.2-2006) specified in agricultural chemical indoor bioassay test quasi-lateral bactericide and combined action measurement (NY/T1156.6-2006) of bactericide mixing.
5. Drug treatment
Under the aseptic operation condition, respectively adding 2.0mL of liquid medicine with different concentrations into a sterilized triangular flask (the standard amount is 50mL) accurately calibrated in advance by using a pipette, then adding a culture medium which is melted and cooled to the appropriate temperature into the triangular flask to the calibrated 50mL scale mark, fully shaking uniformly, pouring the culture medium into 4 culture dishes (the diameter is 9cm) in equal quantity, preparing a PDA plate containing medicine with corresponding concentration, wherein each concentration treatment is divided into 4 times, and the component without containing the effective component of the medicine is used as a blank control.
6. Inoculation: cutting off bacterial cake from the edge of bacterial colony by using a sterilization puncher with the diameter of 5mm under aseptic condition, inoculating the bacterial cake to the center of a drug-containing flat plate by using an inoculator, covering a dish cover, placing the flat plate in a biochemical incubator with the temperature of 26 +/-1 ℃ and the relative humidity of 80% for dark culture, and observing experimental results.
7. Investigation time and method
The colony in the culture dish treated according to the control group grows to 2/3-4/5 of the diameter of the culture dish, and then the test is stopped. The diameter of the colonies was measured with a ruler, and the diameter was measured perpendicularly for each colony by the cross method, and the average value was taken (the diameter of the cake was subtracted by 5mm for each measurement).
8. Statistical analysis of data
According to the measurement result, the hypha growth inhibition rate of each treatment concentration on the test strain is calculated, then the DPS data processing software is used for calculating the experiment result, and respectively solving the toxicity regression equation and EC of the single agent and the mixed agent with different proportions of the test agent50、EC90And 95% confidence limit, calculating co-toxicity coefficient (CTC) of two drugs at different ratios, and screening out the optimal ratio of test drugs
Calculating the hypha growth inhibition rate of each treatment concentration on the target bacteria to be tested according to the formula (1) and the formula (2), and respectively solving the toxicity regression equation and EC of the experimental product50、EC90And 95% confidence limits.
Formula (1);
D＝D1-D2in the formula: d is the colony growing diameter; d1The diameter of the colony is shown; d2The diameter of the fungus cake.
Formula (2):
I＝(D0-Dt/D0) X 100; in the formula: i is the hypha growth inhibition rate; d0Growing the diameter of the colony for the blank control; dtThe colonies grow in diameter for agent treatment.
Calculating co-toxicity coefficient (CTC) according to Sun Yunpei method, and evaluating synergistic effect of the combination of the medicines according to the value of the co-toxicity coefficient (CTC), i.e. the antagonism is achieved when CTC is less than or equal to 80, the additivity is achieved when CTC is more than 80 and less than 120, and the synergy is achieved when CTC is more than or equal to 120. The co-toxicity coefficient (CTC) is calculated according to the formulas (3), (4) and (5).
Formula (3)
ATI is S/M × 100; in the formula: ATI is the measured virulence index of the composition; s is EC of standard medicament50In mg/l; m is EC of the composition50The unit is mg/l.
Formula (4)
TTI＝TIA×PA+TIB×PB(ii) a In the formula: TTI is the theoretical virulence index of the composition; TIAIs the virulence index of prothioconazole; pAIs the percentage content of the prothioconazole in the composition, unit percentage%; TIBIs toxicity index of prochloraz; pBThe percentage of the prochloraz in the composition is unit percent.
Formula (5)
CTC ═ ATI/TTI × 100; in the formula: CTC is co-toxicity coefficient;
the results of the experiment are recorded in fig. 2, in particular fig. 2.
D: virulence test for composition ii:
test targets: scab of wheat
1. The test medicaments of prothioconazole (A) and tebuconazole (B) are respectively prepared into 1.0 multiplied by 10 by using dimethylformamide as a solvent4And (5) putting the mg/L mother solution into a refrigerator for later use.
2. The ratio of the mixed effective components of the two is prothioconazole: tebuconazole is 3: 1. 2: 1. 1: 1. 1: 2 and 1: 3, preparing into 1.0 multiplied by 104And (5) putting mg/L dimethylformamide mother liquor into a refrigerator for later use.
3. On the basis of a pre-test experiment, the mother liquor is diluted by an aqueous solution containing 0.1% of Tween 80, 5 concentrations are designed for each treatment, and the concentrations of two medicaments and different proportions thereof are set as follows:
prothioconazole (a): 0.125, 0.25, 0.5, 1, 2mg/L
Tebuconazole (B): 0.5, 1, 2, 4, 8mg/L
A：B(3：1)：0.125、0.25、0.5、1、2mg/L
A：B(2：1)：0.15、0.3、0.6、1.2、2.4mg/L
A：B(1：1)：0.15、0.3、0.6、1.2、2.4mg/L
A：B(1：2)：0.25、0.5、1、2、4mg/L
A：B(1：3)：0.3、0.6、1.2、2.4、4.8mg/L
4. Test basis method
The method refers to a hypha growth rate method (NY/T1156.2-2006) specified in agricultural chemical indoor bioassay test quasi-lateral bactericide and combined action measurement (NY/T1156.6-2006) of bactericide mixing.
5. Drug treatment
Under the aseptic operation condition, respectively adding 2.0mL of liquid medicine with different concentrations into a sterilized triangular flask (the standard amount is 50mL) accurately calibrated in advance by using a pipette, then adding a culture medium which is melted and cooled to the appropriate temperature into the triangular flask to the calibrated 50mL scale mark, fully shaking uniformly, pouring the culture medium into 4 culture dishes (the diameter is 9cm) in equal quantity, preparing a PDA plate containing medicine with corresponding concentration, wherein each concentration treatment is divided into 4 times, and the component without containing the effective component of the medicine is used as a blank control.
6. Inoculation: cutting off bacterial cake from the edge of bacterial colony by using a sterilization puncher with the diameter of 5mm under aseptic condition, inoculating the bacterial cake to the center of a drug-containing flat plate by using an inoculator, covering a dish cover, placing the flat plate in a biochemical incubator with the temperature of 26 +/-1 ℃ and the relative humidity of 80% for dark culture, and observing experimental results.
7. Investigation time and method
The colony in the culture dish treated according to the control group grows to 2/3-4/5 of the diameter of the culture dish, and then the test is stopped. The diameter of the colonies was measured with a ruler, and the diameter was measured perpendicularly for each colony by the cross method, and the average value was taken (the diameter of the cake was subtracted by 5mm for each measurement).
8. Statistical analysis of data
Calculating the inhibition rate of each treatment concentration on the hypha growth of the test strain according to the measurement result, calculating the experimental result by using DPS data processing software, and respectively calculatingTest of toxicity regression equation and EC of single agent and mixture of different proportions50、EC90And 95% confidence limit, and calculating co-toxicity coefficient (CTC) of the two medicaments in different proportions, and screening out the optimal proportion of the test medicament.
Calculating the hypha growth inhibition rate of each treatment concentration on the target bacteria to be tested according to the formula (1) and the formula (2), and respectively solving the toxicity regression equation and EC of the experimental product50、EC90And 95% confidence limits.
Formula (1);
D＝D1-D2in the formula: d is the colony growing diameter; d1The diameter of the colony is shown; d2The diameter of the fungus cake.
Formula (2):
I＝(D0-Dt/D0) X 100; in the formula: i is the hypha growth inhibition rate; d0Growing the diameter of the colony for the blank control; dtThe colonies grow in diameter for agent treatment.
Calculating co-toxicity coefficient (CTC) according to Sun Yunpei method, and evaluating synergistic effect of the combination of the medicines according to the value of the co-toxicity coefficient (CTC), i.e. the antagonism is achieved when CTC is less than or equal to 80, the additivity is achieved when CTC is more than 80 and less than 120, and the synergy is achieved when CTC is more than or equal to 120. The co-toxicity coefficient (CTC) is calculated according to the formulas (3), (4) and (5).
Formula (3)
ATI is S/M × 100; in the formula: ATI is the measured virulence index of the composition; s is EC of standard medicament50In mg/l; m is EC of the composition50The unit is mg/l.
Formula (4)
TTI＝TIA×PA+TIB×PB(ii) a In the formula: TTI is the theoretical virulence index of the composition; TIAIs the virulence index of prothioconazole; pAIs the percentage content of the prothioconazole in the composition, unit percentage%; TIBIs the virulence index of tebuconazole; pBIs the percentage content of tebuconazole in the composition and has unit percentage.
Formula (5)
CTC ═ ATI/TTI × 100; in the formula: CTC is co-toxicity coefficient;
the results of the experiment are recorded in fig. 3, in particular fig. 3.
2. And (3) testing the high-temperature stability: the compositions prepared in examples 1, 2 and 5 were used for the high temperature stability test, the prepared compositions were sealed in 10 ml ampoules, left at 54 ℃ for two weeks, observed for changes in the compositions and the results are recorded in the following table.
Experiment of High temperature stability
Example 1 Without any change
Example 2 Without any change
Example 5 The caking phenomenon appears

Claims (10)

1. A gramineous plant bactericidal composition is characterized by comprising a composition I or a composition II;
the raw materials for preparing the composition I comprise prothioconazole and/or prochloraz;
the raw materials for preparing the composition II comprise prothioconazole and/or tebuconazole.
2. The gramineae plant sterilizing composition according to claim 1, characterized in that the weight ratio of prothioconazole to prochloraz is (1-3): (1-5).
3. The gramineae plant sterilizing composition according to claim 1, characterized in that the weight ratio of prothioconazole and tebuconazole is (1: 10): (10-1).
4. The graminaceous plant bactericidal composition according to any one of claims 1 to 3, characterized in that the raw materials for preparation further comprise auxiliary aids.
5. The gramineous plant bactericidal composition according to claim 4, wherein said auxiliary agent is at least one selected from the group consisting of a thickener, a wetting agent, a disintegrating agent, a stabilizer, a suspending agent, a dispersing agent, an antifoaming agent, an antifreeze agent, an adsorbent, an emulsifier, a pH adjuster, and the like.
6. The graminaceous plant bactericidal composition according to claim 5, characterized in that the raw material for preparation further comprises a solvent and/or water.
7. The graminaceous plant bactericidal composition according to claim 6, wherein said solvent is at least one selected from the group consisting of cyclohexanone, mineral spirits, methanol and isopropanol.
8. The gramineae plant sterilizing composition according to any one of claims 1 to 3, wherein the composition is prepared as at least one of wettable powder, water dispersible granule, suspending agent, suspoemulsion, aqueous emulsion, microemulsion, microcapsule suspending agent and granule.
9. A method for preparing the graminaceous plant sterilizing composition according to any one of claims 4 to 8, comprising the steps of:
and mixing the composition I or the composition II with auxiliary agents, and stirring to prepare the composition.
10. The use of the graminaceous plant bactericidal composition according to any one of claims 4 to 8, wherein said composition is used for controlling wheat powdery mildew, wheat sharp eyespot, rice sheath blight, wheat rust and wheat scab.
CN202111504335.3A 2021-12-10 2021-12-10 Poaceae plant sterilization composition and preparation method and application thereof Pending CN114698637A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103918693A (en) * 2014-03-31 2014-07-16 海利尔药业集团股份有限公司 Bactericidal composition containing prothioconazole and prochloraz
CN104604920A (en) * 2013-11-05 2015-05-13 南京华洲药业有限公司 Sterilization composition containing prochloraz nantokite and triazole bactericide as well as application thereof
CN104621168A (en) * 2013-11-15 2015-05-20 南京华洲药业有限公司 Sterilization composition containing prothioconazole and prochloraz-manganese chloride and application thereof
CN104642367A (en) * 2013-11-15 2015-05-27 南京华洲药业有限公司 Bactericidal composition containing prothioconazole and prochloraz and application thereof
CN104642331A (en) * 2013-11-15 2015-05-27 南京华洲药业有限公司 Bactericidal composition containing prothioconazole and tebuconazole and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104604920A (en) * 2013-11-05 2015-05-13 南京华洲药业有限公司 Sterilization composition containing prochloraz nantokite and triazole bactericide as well as application thereof
CN104621168A (en) * 2013-11-15 2015-05-20 南京华洲药业有限公司 Sterilization composition containing prothioconazole and prochloraz-manganese chloride and application thereof
CN104642367A (en) * 2013-11-15 2015-05-27 南京华洲药业有限公司 Bactericidal composition containing prothioconazole and prochloraz and application thereof
CN104642331A (en) * 2013-11-15 2015-05-27 南京华洲药业有限公司 Bactericidal composition containing prothioconazole and tebuconazole and application thereof
CN103918693A (en) * 2014-03-31 2014-07-16 海利尔药业集团股份有限公司 Bactericidal composition containing prothioconazole and prochloraz

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