CN106342821A - Prothioconazole- tebuconazole compounded suspending agent and preparation method thereof - Google Patents

Prothioconazole- tebuconazole compounded suspending agent and preparation method thereof Download PDF

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Publication number
CN106342821A
CN106342821A CN201610727046.2A CN201610727046A CN106342821A CN 106342821 A CN106342821 A CN 106342821A CN 201610727046 A CN201610727046 A CN 201610727046A CN 106342821 A CN106342821 A CN 106342821A
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CN
China
Prior art keywords
tebuconazole
preparation
suspending agent
parts
prothioconazole
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610727046.2A
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Chinese (zh)
Inventor
徐长才
毛堂富
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ANHUI MEILAND AGRICULTURAL DEVELOPMENT Co Ltd
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ANHUI MEILAND AGRICULTURAL DEVELOPMENT Co Ltd
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Priority to CN201610727046.2A priority Critical patent/CN106342821A/en
Publication of CN106342821A publication Critical patent/CN106342821A/en
Pending legal-status Critical Current

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Classifications

    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647Triazoles; Hydrogenated triazoles
    • A01N43/6531,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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 liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels

Abstract

The invention provides a prothioconazole-tebuconazole compounded suspending agent and a preparation method thereof and relates to the technical field of prevention and control of wheat scab. The compounded suspending agent is at least prepared from the following components in parts by weight (100 parts in total): 20 parts of prothioconazole, 12 parts of tebuconazole, 3 parts of fatty alcohol-polyoxyethylene ether, 3 parts of styrylphenol polyoxyethylene ether, 0.3 part of xanthan gum, 0.4 part of sodium benzoate, 0.3 part of a defoaming agent and the balance of deionized water. The preparation method comprises the steps of pumping all the raw materials into a preparation kettle, mixing, stirring, carrying out primary grinding by virtue of a colloid mill, carrying out fine grinding by virtue of a sand mill, carrying out sampling and analysis, and after the sample is qualified, carrying out filtration, measurement, packaging and warehousing. According to the preparation method, the compounded suspending agent including 32% of prothioconazole and tebuconazole in a ratio of 5 to 3 has the effect of effectively expanding the action range, but preparations blended in other proportions do not have the effect.

Description

A kind of prothioconazoles and Tebuconazole compound suspending agent and preparation method thereof
Technical field
The present invention relates to wheat scab Prevention Technique field, it is specifically related to a kind of prothioconazoles and Tebuconazole compounds and hangs Floating agent and preparation method thereof.
Background technology
At present, the existing bactericidal composition for preventing and treating wheat scab, such as Chinese patent cn 104106580 a Disclose a kind of " preventing and treating the compound disinfectant of wheat scab ", with albendazole and Tebuconazole as base material, according to albendazole It is formulated with the quality proportioning of Tebuconazole 7: 1~1: 7.Preferably albendazole and Tebuconazole quality proportioning are 1: 2.Rosickyite Imidazoles is the bactericide original drug of mass fraction 97%, and Tebuconazole is the bactericide original drug of mass fraction 98.43%.Separately there is China specially Sharp cn 104686529 a discloses a kind of " for preventing and treating pharmaceutical agent combinations and its application of wheat scab ", and effective ingredient is penta The complex composition of azoles alcohol and trichlamide, the weight of the two ratio is for 1:4~4:1.
Inventor verifies through long term test, and this above-mentioned several bactericidal composition is primarily present following defect:
1), by testing to concrete proportionings several disclosed in above-mentioned several bactericidal compositions, find to gibberella saubinetii The preventing and treating of disease cannot play good prevention effect.
2), it is directed to several dosage forms disclosed in above-mentioned several bactericidal compositions, find all to exist difference through verification experimental verification The defect of problem.For example, wettable powder easily causes product to bond, and is difficult dispersion in water and suspends, or blocking shower nozzle, in spray In day with fog, the phenomenon such as reason precipitation, causes to spray irregular.
3), compound problem, by virulence test, heat are carried out to concrete proportionings several disclosed in above-mentioned several bactericidal compositions Storage stability test and mixture co-toxicity coefficient measure and find, are all unable to reach obvious potentiation.
Content of the invention
An object of the present invention is to provide a kind of prothioconazoles and Tebuconazole to compound suspending agent, and the design of this suspending agent is closed Reason, good to the prevention effect of wheat scab, and can achieve the notable synergistic effect of prothioconazoles and Tebuconazole.
For achieving the above object, present invention employs technical scheme below:
A kind of prothioconazoles and Tebuconazole compound suspending agent, are made up of following components according to weight portion:
Prothioconazoles are mainly used in preventing and treating numerous diseases such as frumentum, wheat and barley legume crop, and prothioconazoles toxicity is low, no causes Abnormal, mutagenesis type, to embryo's avirulence, to human and environment safety.Its mechanism of action is precursor --- the sheep of sterol in suppression funguses Demethylation effect on hair sterol or 2,4- methylene dihydro Pilus Caprae seu Oviss steroid 14.Not only there is good systemic activity, excellent Protection, treat and root out activity, and the lasting period is long.By substantial amounts of field control effectiveness test, result shows prothioconazoles to work Thing not only has good safety, and preventing disease theraping effect is good, and increases production substantially, compared with triazole type biocide agent, rosickyite bacterium Azoles has broader spectrum of sterilization and lives.
Tebuconazole is a kind of efficient, wide spectrum, absorbability triazole bactericidal agent, has protection, treats, roots out three zones, Wide sterilization spectrum, lasting period are long.This product is used for preventing and treating sclerotinia rot of colza, and not only preventive effect is good, and has resistant to lodging, and production-increasing function is bright Aobvious the features such as.Mechanism of action to pathogenic bacteria is the demethylation suppressing ergosterol on its cell membrane so that pathogenic bacteria cannot be formed Cell membrane, thus kill pathogenic bacteria.
The prothioconazoles of the present invention and Tebuconazole compound suspending agent, and its advantage shows:
1), the suspending agent of present invention preparation is in suspensibility, persistent foamability, wet screening test etc. and the side such as heat storage stability Face is significantly better than that the product prepared by other proportionings.
2), pass through experimental verification, prothioconazoles and Tebuconazole mixed with 5:3 proportioning compounded 32% when prothioconazoles Compound suspending agent with Tebuconazole, notable synergistic sphere of action can be played, and the preparation that other proportioning is used with, all it is unable to reach substantially Potentiation scope.Meanwhile, the actual toxicity of different ratio is not lifted with the enhancing of theoretical toxicity, actual toxicity and reason By having no regular change between toxicity.
Another object of the present invention is to providing a kind of prothioconazoles and Tebuconazole to compound the preparation method of suspending agent, will be former Material suction prepare kettle mix and blend after through grinding at the beginning of colloid mill, then through sand mill fine grinding, sample analysis, qualified after filter, metering, Packaging, warehouse-in.
The prothioconazoles of the present invention and Tebuconazole compound the preparation method of suspending agent, preparation technology relatively simple it is easy to work Industry metaplasia is produced.
Specific embodiment
Below with reference to embodiment, the present invention is described in detail.But, embodiment content is only to this Bright example and explanation, affiliated those skilled in the art do various repairing to described specific embodiment Change or supplement or using similar mode substitute, without departing from invention design or surmount defined in the claims Scope, all should belong to protection scope of the present invention.
First, the preparation of prothioconazoles and the compounding suspending agent of Tebuconazole, and the items of the suspending agent prepared by each embodiment The testing result of technical specification, heat storage stability result of the test.
Embodiment 1
32% prothioconazoles and Tebuconazole compound suspending agent, and each component and its weight proportion are as follows:
Composition Weight portion
Prothioconazoles 20
Tebuconazole 12
Fatty alcohol-polyoxyethylene ether 3
Styrylphenol polyoxyethylene ether 3
Xanthan gum 0.3
Sodium benzoate 0.4
Defoamer 0.3
Deionized water 61
Preparation method: raw material suction is prepared through grinding at the beginning of colloid mill after kettle mix and blend, then through sand mill fine grinding, samples Analysis, qualified rear filtration, metering, packaging, warehouse-in.
Embodiment 2
31% prothioconazoles and Tebuconazole compound suspending agent, and each component and its weight proportion are as follows:
Composition Weight portion
Prothioconazoles 19
Tebuconazole 12
Fatty alcohol-polyoxyethylene ether 3
Styrylphenol polyoxyethylene ether 3
Xanthan gum 0.3
Sodium benzoate 0.4
Defoamer 0.3
Deionized water 62
Preparation method is with embodiment 1.
Embodiment 3
30% prothioconazoles and Tebuconazole compound suspending agent, and each component and its weight proportion are as follows:
Preparation method is with embodiment 1.
Embodiment 4
33% prothioconazoles and Tebuconazole compound suspending agent, and each component and its weight proportion are as follows:
Composition Weight portion
Prothioconazoles 20
Tebuconazole 13
Fatty alcohol-polyoxyethylene ether 3
Styrylphenol polyoxyethylene ether 3
Xanthan gum 0.3
Sodium benzoate 0.4
Defoamer 0.3
Deionized water 60
Preparation method is with embodiment 1.
Embodiment 5
34% prothioconazoles and Tebuconazole compound suspending agent, and each component and its weight proportion are as follows:
Preparation method is with embodiment 1.
Embodiment 6
32% prothioconazoles and Tebuconazole compound suspending agent, and each component and its weight proportion are as follows:
Composition Weight portion
Prothioconazoles 20
Tebuconazole 12
Cupreol 0.6
Fatty alcohol-polyoxyethylene ether 3
Styrylphenol polyoxyethylene ether 3
Xanthan gum 0.3
Sodium benzoate 0.4
Defoamer 0.3
Deionized water 60.4
Preparation method is with embodiment 1.
Prothioconazoles prepared by embodiment 1~6 and Tebuconazole compound suspending agent, the detection knot of product all technical As shown in table 1, product heat storage stability result of the test is as shown in table 2 for fruit.
16 embodiments of table prepare the testing result of product all technical
26 embodiments of table prepare product heat storage stability result of the test
By table 1 and 2 as can be seen that the product of embodiment 1 and 6 preparation is in suspensibility, persistent foamability, wet screening test etc. And the aspect such as heat storage stability is significantly better than that the product prepared by other embodiment.
2nd, toxicological information
Prothioconazoles: acceptable daily intake is 0.05mg/kg/day, acute oral ld50: rat (female/male) > 6200mg/kg;Acute percutaneous ld50: rat (female/male) > 2000mg/kg.
Tebuconazole: rat acute ld50For 4000mg/kg, the oral ld of male chmice acute50About 2000mg/kg is female little Mus acute oral ld50For 3933mg/kg, rat acute percutaneous ld50>5000mg/kg.Rat acute sucks lc50(4h)> 0.8mg/l air (aerosol), > 5.1mg/l (powder).This medicine is to fish moderate toxicity, Carassius auratuses lc50It is within (96 hours) 8.7mg/l.
3rd, indoor biological activity (virulence) of prothioconazoles and the compounding suspending agent of Tebuconazole measures.
1st, experiment purpose
It is intended to measure prothioconazoles, Tebuconazole and the two virulence to head blight for the different proportion proportioning, to judge the two not Whether there is potentiation with proportioning to suppression head blight.
2nd, experimental condition
2.1 for examination target
Gibberellic hypha, by Hefei City's water baseization biological material Engineering Technical Research Centre separation, purification, preserves and carries For.
2.2 condition of culture
Culture, 25 ± 1 DEG C of temperature, relative humidity 85-95% in bio-incubator.
2.3 instrument and equipment
Electronic balance (sensibility reciprocal 0.1mg), bio-incubator, diameter 9cm culture dish, pipet/rifle, inoculator, card punch, Slide calliper rule etc..
3rd, EXPERIMENTAL DESIGN
3.1 examination materials prepare
Gibberellic hypha pathogen is placed on culture in biochemical cultivation case, standby.
3.2 medicament
Prothioconazoles active compound, Anhui Meilan Agricultural Development Co., Ltd. provides.
Original Tebuconazole, Anhui Meilan Agricultural Development Co., Ltd. provides.
3.3 medicaments are prepared
With acetone, medicament prepared by embodiment 1-6 is diluted to 5 series mass concentration.
4th, test method
Carry out with reference to " farm-chemical indoor determination test rule ----antibacterial " (ny/t1156.6 2006).In order to touch The activity to strains tested for each medicament of rope, first carries out preliminary experiment.Will mycelia be placed on containing higher and low concentration Cultivated under the culture medium of medicament, estimated ec50, then further according to the ec of estimation50Value, culture medium is made into its ec50Left and right The pastille culture medium of variable concentrations gradient cultivated.
This test adopts plate mycelial growth rate method to measure the virulence to gibberellic hypha for the medicament.Concrete grammar is as follows: warp The gibberellic hypha bacterial strain psa culture medium culturing of switching activation, when bacterium colony length is to culture dish 3/4ths size, with internal diameter be The card punch of 5mm punches from edge, and the mycelia block breaking into is as inoculum.Respectively medicament mother solution is added the psa that people's sterilizing is melted In culture medium, fully shake up, make medicament ultimate density (calculating by effective ingredient) reach variable concentrations gradient.15ml poured into by every ware Left and right pastille culture medium, if not dosing is comparison, often processes 4 repetitions.The mycelia block (diameter 5mm) of the new growth of transposing is in flat board Central authorities, after be placed in culture 2d (gibberellic hypha), 7d (gibberellic hypha) and 15d (gibberellic hypha) in 25 DEG C of incubators.Use decussation Method measures colony diameter, calculates each process net growth, mycelial growth inhibition rate.
In formula: a diameter of 5mm of bacterium dish.
5th, data statistic analysis
Mycelial growth inhibition rate is converted into probit value (y), drug concentration (μ g/ml) is converted into logarithm value (x), with minimum Square law tries to achieve virulence regression equation (y=a+bx).With dps statistical software to the log concentration value of each single dose and different mixture and Corresponding suppression ratio probit value carries out regression analyses, calculates ec50Value and 95% confidence limit.
According to ec50Calculate actual measurement toxicity index (ati), theoretical toxicity index (tti) and the co-toxicity coefficient of built agent (ctc).
Built agent actual measurement toxicity index (ati)=single dose ec50/ built agent ec50×100.
Built agent theoretical toxicity index (tti)=a toxicity index × a content (%)+b toxicity index × b in built agent Content (%) in built agent.
Co-toxicity coefficient (ctc)=ati/tti × 100.
Medicament different ratio synergy ratio (ctc) is calculated according to the abundant method of Sun Yun, ctc≤80 are antagonism, 80 < Ctc < 120 is summation action, and ctc >=120 are potentiation.
6th, result and analysis
The suspending agent of embodiment 1 and 6 preparation shows as notable synergistic effect to the co-toxicity of head blight, and (co-toxicity coefficient divides Do not reach 195,200), and the suspending agent of embodiment 2-5 preparation is showed only as summation action (poison altogether to the co-toxicity of head blight Coefficient is followed successively by 80,85,90,80).Meanwhile, be can be seen that by the experiment of embodiment 6 and with the addition of in compounding suspending agent less After the cupreol of amount, prothioconazoles and the compounding synergy of Tebuconazole can be made to be lifted further.

Claims (2)

1. a kind of prothioconazoles and Tebuconazole compound suspending agent it is characterised in that: be at least made up of the component of following weight portion:
2. a kind of prepare prothioconazoles as claimed in claim 1 and Tebuconazole compound suspending agent method it is characterised in that: will be former Material suction prepare kettle mix and blend after through grinding at the beginning of colloid mill, then through sand mill fine grinding, sample analysis, qualified after filter, metering, Packaging, warehouse-in.
CN201610727046.2A 2016-08-25 2016-08-25 Prothioconazole- tebuconazole compounded suspending agent and preparation method thereof Pending CN106342821A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113519539A (en) * 2021-07-20 2021-10-22 溧阳中南化工有限公司 Compound antibacterial suspension medicament for preventing and treating wheat diseases and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1109499C (en) * 1997-04-18 2003-05-28 拜尔公司 Fungicide active substance combinations
CN100521940C (en) * 2003-09-11 2009-08-05 拜尔农作物科学股份公司 Use of fungicides for disinfecting cereal seed
EP2837287A1 (en) * 2013-08-15 2015-02-18 Bayer CropScience AG Use of prothioconazole for increasing root growth of Brassicaceae
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
CN105532675A (en) * 2015-12-24 2016-05-04 安徽美兰农业发展股份有限公司 Prothioconazole and tebuconazole compound suspending agent and preparing method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1109499C (en) * 1997-04-18 2003-05-28 拜尔公司 Fungicide active substance combinations
CN100521940C (en) * 2003-09-11 2009-08-05 拜尔农作物科学股份公司 Use of fungicides for disinfecting cereal seed
EP2837287A1 (en) * 2013-08-15 2015-02-18 Bayer CropScience AG Use of prothioconazole for increasing root growth of Brassicaceae
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
CN105532675A (en) * 2015-12-24 2016-05-04 安徽美兰农业发展股份有限公司 Prothioconazole and tebuconazole compound suspending agent and preparing method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113519539A (en) * 2021-07-20 2021-10-22 溧阳中南化工有限公司 Compound antibacterial suspension medicament for preventing and treating wheat diseases and preparation method thereof

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Application publication date: 20170125