CN108464307A - A kind of compound thiophene composition of rice disease prevention - Google Patents

A kind of compound thiophene composition of rice disease prevention Download PDF

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Publication number
CN108464307A
CN108464307A CN201810266007.6A CN201810266007A CN108464307A CN 108464307 A CN108464307 A CN 108464307A CN 201810266007 A CN201810266007 A CN 201810266007A CN 108464307 A CN108464307 A CN 108464307A
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China
Prior art keywords
thiophene
compound
composition
rice
disease prevention
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CN201810266007.6A
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付美彦
杨雪
冷超
蒋美玉
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Li Yingmiao
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Li Yingmiao
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Priority to CN201810266007.6A priority Critical patent/CN108464307A/en
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    • 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
    • A01N43/72Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/82Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms

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

Abstract

A kind of compound thiophene composition of rice disease prevention, is 1 by least one auxiliary material and mass ratio:0.8~1.2 thiophene and 3 O (2 base of N (5 ((4 pyridyl group) sulfydryl) 1,3,4 thiadiazoles, 2 base) acetamide) 3 ', 4 ', 5 ', 5,7 pentamethoxyl myricetins (A14) form.The dosage form of the rice disease protective agents is wettable powder, and the gross mass of thiophene and compound (A14) accounts for the 15%~30% of bactericide gross mass.The auxiliary material is the auxiliary material suitable for wettable powder, including dispersant, wetting agent, suspending agent and carrier.

Description

A kind of compound thiophene composition of rice disease prevention
Technical field
The present invention relates to a kind of rice diseases to prevent medication.
Background technology
Bacterial blight of rice occurs mainly in East China, Central China, South China rice region as one of three major disease of China's rice.By The rice underproduction infected is up to 50-60%, or even total crop failure.Bacterial blight of rice pathogen belongs to Pseudomonas alba, yellow sporangium Belong to.To prevent bacterial blight of rice, plant fungicide is mostly used.Thiophene (N.N '-methylene-bis- (2- amino -5- sulfenyls - 1,3,4- thiadiazoles)) it is a kind of bactericide of China's independent research, it includes the white leaf of rice to be then used to prevent in pesticide field The various bacterias such as blight and fungal disease.But is widely used by semicentennial, bacterial blight of rice to thiophene Stronger resistance is produced, so that thiophene has been difficult to continue to apply to the prevention of bacterial blight of rice.
A series of myricetin derivative of amide containing thioether thiadiazoles is disclosed in Chinese patent literature CN107602548A, and It is disclosed to can be used for preparing disinfectant use in agriculture and antivirotic.The document specifically discloses 3-O- (N- (5- ((4- pyridines Base) sulfydryl) -1,3,4- thiadiazoles -2- bases)-acetamide -2- bases) -3 ', 4 ', 5 ', 5,7- pentamethoxyl myricetins (A14), though So show the control effect certain to bacterial blight of rice in isolated experiment, but effect with only (i.e. thiophene is withered with Yekuzuo Azoles),.Therefore in prior art basis, based on the above problem in the prior art, how with thiophene compound plant is rationally formed Fungicide becomes urgent problem to be solved in the prior art to improve the rice diseases control effect such as bacterial blight of rice.
Invention content
Under study for action it was found that using 3-O- (N- (5- ((4- pyridyl groups) sulfydryl) -1,3,4- thiadiazoles -2- bases)-second Amide -2- bases) -3 ', 4 ', 5 ', 5,7- pentamethoxyl myricetins (A14) and thiophene compatibility be when being made compound, and it can be significant The control effect for plant diseases such as bacterials blight of rice is improved, is based on this, the present invention provides following technical schemes:
A kind of compound thiophene composition of rice disease prevention, it is characterized in that the composition by least one auxiliary material and Mass ratio is 1:0.8~1.2 thiophene and 3-O- (N- (5- ((4- pyridyl groups) sulfydryl) -1,3,4- thiadiazoles -2- bases)-second Amide -2- bases) -3 ', 4 ', 5 ', 5,7- pentamethoxyls myricetin (A14) composition.
The compound thiophene composition of a kind of rice disease prevention, it is characterized in that thiophene in the composition Mass ratio with compound (A14) is 1:0.9~1.1.
The compound thiophene composition of a kind of rice disease prevention, it is characterized in that the dosage form of the composition is selected from Wettable powder.The gross mass of thiophene and compound (A14) accounts for the 15%~30% of bactericide gross mass.
The auxiliary material is the auxiliary material suitable for wettable powder, including dispersant, wetting agent, suspending agent and carrier.
The dispersant is selected from APES formaldehyde condensation products sulfat (SOPA), Nekal BX, naphthalene sulfonic acids Sodium formaldehyde condensation product (NNO), one kind, polyoxyethylene sorbitan monooleate in sodium lignin sulfonate;The polyoxy second The preferred polysorbate60 of alkene Sorbitan Monooleate or Tween 80.
The wetting agent is in lauryl sodium sulfate, sodium alkyl benzene sulfonate, Negel formaldehyde condensation products It is one or more.
The suspending agent is selected from at least one of polyethylene glycol, sodium carboxymethylcellulose, hydroxypropyl methyl cellulose.
The carrier in attapulgite, diatomite, kaolin, talcum powder, precipitated calcium carbonate, white carbon at least one Kind.
The compound thiophene composition of a kind of rice disease prevention provided by the invention, by thiophene and compound (A14) Compatibility is carried out with special ratios, the bacteriostatic activity to bacterial blight of rice pathogenic bacteria is significantly improved, significantly improves white to rice The control effect of leaf blight.The form that this traditional plant fungicide of thiophene passes through composition compound can be made to retrieve popularization Using.It, which belongs to low toxicity compounds, is shown to the acute toxicity detection of compound (A14).Found in recipe determination, thiophene with The proportioning of compound (A14) is 1:When 0.8~1.2, apparent synergistic effect can be generated when preventing bacterial blight of rice, more High or lower compound (A14) addition can not all generate this effect, and the ratio of thiophene and compound (A14) is preferred It is 1:When 0.9~1.1, the effect for improving prevention bacterial blight of rice becomes apparent.And we send out in option screening in advance Now only have compound (A14) and thiophene energy compatibility and synergistic effect is generated to the prevention of bacterial blight of rice, when normal with others When with bacterial blight of rice protective agents compatibility, apparent effect is had no.
Specific implementation mode
One, in vitro antibacterial activity test
(1) test method
Using nephelometry, each experimental drug is tested to rice leaf spot bacteria The inhibitory activity of (Xanthomonasoryzaepv.oryzae (Xoo)), concrete operation step are as follows:
A. in 2000mL beakers be added 1000mL sterile purified waters, sequentially added under electromagnetic agitation peptone 5.0g, Yeast powder 1.0g, glucose 10.0g, beef extract 3.0g, it is to be mixed uniformly after pH adjusted to neutrality with sodium hydrate aqueous solution (7.2±0.2);
B. test tube sterilizing is cleaned to be placed on rack for test tube, using liquid-transfering gun into every test tube solution in removing step A After 4.0mL plus rubber stopper, every 6 test tubes packaging is primary, after the 20min that sterilize at 121 DEG C using autoclave for use;
C. 0.00375-0.0042g samples to be tested are weighed in centrifuge tube, to pipette 80 μ respectively after 150 μ L DMSO dissolvings After L and 40 μ L to sterilizing in numbered centrifuge tube, 40 μ LDMSO are separately added to the centrifuge tube equipped with 40 μ L sample solution, upwards It states and 4mLTween-20 is respectively added in centrifuge tube, while setting Thiodiazole-copper and comparing medicament, DMSO makees blank.It is molten in every centrifuge tube Liquid pipettes (to be operated, prevent other germ contaminations) in the sterile medium test tube that 1mL to 3 fills step B before alcolhol burner;
E. 96 orifice plate of blank is taken, blank OD values is surveyed and excludes the hole that OD values are more than 0.05,200 to be added in backward each available hole Solution is surveyed OD values and is recorded in test tube in μ L (4), and the rice leaf spot bacteria after 40 μ L activation is finally accessed into every test tube Strain, 24~48h of shaken cultivation in 30 DEG C, 180rpm constant-temperature tables, during which in test tube solution O D values to track bacterium Growth conditions take 200 μ L solution to survey OD values and record in test tube after culture;
F. Bacteria suppression rate calculation formula is as follows,
Correct the OD values=values of OD containing bacterium culture medium-aseptic culture medium OD values
Sample to be tested grouping is as follows with when experimental result:(n=3)
The compound (A14) used in experiment is provided by Tianjin Kai Yin Science and Technology Ltd.s, and >=98%, lot number is content 20170905, Thiodiazole-copper uses 20% suspending agent, and drug dose to be measured is calculated with active constituent actual content in each experimental group. The result shows that it is 11 to match:9 to 9:11 thiophene shows better bacteriostatic activity with compound (A14), wherein 10: 10 experimental group 5 is not only higher than the experimental group 6/7 that two kinds of drugs are used alone, and also higher than existing thiophene and novel plant kill Microbial inoculum Thiodiazole-copper.
Two, embodiment
A kind of compound thiophene composition of rice disease prevention provided by the invention, preparing becomes wettable powder, by Thiophene, compound (A14) and auxiliary material composition.The formula of the composition is respectively as shown in Examples 1 to 5 in following table, simultaneously Prepare comparative example 1~5 (percentage shown in table is the mass percent for accounting for composition gross mass, disregards moisture):
The preparation method of the composition is:
1) thiophene crushes respectively with compound (A14),
2) by dispersant, wetting agent, mixed with suspending agent after grind, the obtained active constituent powder of step 1) is added, It adds after carrier mixes well and crosses 200 mesh sieve;Obtain wettable powder (moisture content < 1%).
The preferred NNO of dispersant, wetting agent preferably sodium dodecyl sulfate, the preferred hydroxypropyl methyl cellulose of suspending agent carry Body is weight ratio 100:5 kaolin and talcum powder.
Three, control effect is tested
Bacterium method for measuring, which is connect, with field leaf-cutting tests thiophene and the compound (A14) of different proportion to rice bacterial leaf spot The control effect of disease, experimental procedure are as follows
1, using the rice leaf spot bacteria strain of Zhejiang Academy of Agricultural Science plant protection and the offer of institute of microbiology (Xanthomonasoryzaepv.oryzae (Xoo)), culture become 109After the suspension of a/ml, with the dissecting scissors for being moistened with bacterium solution 3~4cm of rice blade tip, 20 rice leaves of every group of selection are subtracted, the spray prevention in 7 days after connecing bacterium is examined or check and compareed for 10 days after administration The control effect (calculating control effect with Spot expansion) and use Excel that group is compared carry out t inspections, water used to experimental result Rice varieties are middle morning 39 (authorization number is that rice 2009039 is examined in Zhejiang)
2, grouping see the table below (means ± s, n=20) with administration with effect situation
By above-mentioned each group drug, experimental group 1~7 and control 1~2 by suspending agent made from each embodiment and comparative example according to Active ingredient final concentration 200ppm is diluted, and control 3 is using commercially available 20% Thiodiazole-copper suspending agents according to active ingredient final concentration 200ppm is diluted, and positive controls are diluted with water 1000 times using the suspending agent (active substance) of comparative example 5.
It is above-mentioned the experimental results showed that, bactericide preferred thiophene and the compound that the embodiment of the present invention 1~5 provides (A14) ratio is 1:0.8~1.2, compared with thiophene or compound (A14) is applied alone, prevention rice bacterial leaf spot can be improved The effect of disease prevention.The control effect compared with compareing 1,2 group of experimental group 1~5 is significantly increased (P < 0.05).Using comparison The experimental group 6/7 of example 1/2, control effect has been decreased obviously.Illustrate thiophene with compound (A14) in the technology of the present invention side Synergistic effect is produced under the ratio selected in case.And in embodiment 2~4 thiophene and compound (A14) preferred proportion (1: 0.9~1.1) better control effect, can be generated when preventing rice bacterial leaf spot, control effect is sterilized better than novel plant Agent Thiodiazole-copper.

Claims (5)

1. a kind of compound thiophene composition of rice disease prevention, it is characterized in that the composition is by least one auxiliary material and matter Amount is than being 1:0.8~1.2 thiophene and 3-O- (N- (5- ((4- pyridyl groups) sulfydryl) -1,3,4- thiadiazoles -2- bases)-acetyl Amine -2- bases) -3 ', 4 ', 5 ', 5,7- pentamethoxyls myricetin (A14) composition.
2. the compound thiophene composition of a kind of rice disease prevention as described in claim 1, it is characterized in that the combination The mass ratio of thiophene and compound (A14) is 1 in object:0.9~1.1.
3. the compound thiophene composition of a kind of rice disease prevention as claimed in claim 1 or 2, it is characterized in that the combination The dosage form of object is wettable powder, and the gross mass of thiophene and compound (A14) accounts for the 15%~30% of composition gross mass.
4. the compound thiophene composition of a kind of rice disease prevention as claimed in claim 3, it is characterized in that the auxiliary material is Suitable for the auxiliary material of wettable powder, including dispersant, wetting agent, suspending agent and carrier.
5. the compound thiophene composition of a kind of rice disease prevention as claimed in claim 4, it is characterized in that the dispersant Selected from APES formaldehyde condensation products sulfat (SOPA), Nekal BX, naphthalenesulfonic acid-formaldehyde condensate (NNO), One kind, polyoxyethylene sorbitan monooleate in sodium lignin sulfonate;The wetting agent be selected from lauryl sodium sulfate, It is one or more in sodium alkyl benzene sulfonate, Negel formaldehyde condensation products;The suspending agent is selected from polyethylene glycol, carboxylic first At least one of base sodium cellulosate, hydroxypropyl methyl cellulose;The carrier is selected from attapulgite, diatomite, kaolin, talcum At least one of powder, precipitated calcium carbonate, white carbon.
CN201810266007.6A 2018-03-28 2018-03-28 A kind of compound thiophene composition of rice disease prevention Pending CN108464307A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101069516A (en) * 2007-05-18 2007-11-14 山东省农业科学院植物保护研究所 Plant disease preventing controlling agent
CN107602548A (en) * 2017-09-14 2018-01-19 贵州大学 A kind of myricetin derivative, the Preparation method and use of amide containing thioether thiadiazoles

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101069516A (en) * 2007-05-18 2007-11-14 山东省农业科学院植物保护研究所 Plant disease preventing controlling agent
CN107602548A (en) * 2017-09-14 2018-01-19 贵州大学 A kind of myricetin derivative, the Preparation method and use of amide containing thioether thiadiazoles

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Application publication date: 20180831