CN106305761A - Compound thiamethoxam and spirotetramat suspending agent and preparation method thereof - Google Patents
Compound thiamethoxam and spirotetramat suspending agent and preparation method thereof Download PDFInfo
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- CN106305761A CN106305761A CN201610723423.5A CN201610723423A CN106305761A CN 106305761 A CN106305761 A CN 106305761A CN 201610723423 A CN201610723423 A CN 201610723423A CN 106305761 A CN106305761 A CN 106305761A
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- suspending agent
- ethyl ester
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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
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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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
- 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
- A01N47/02—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 no bond to a nitrogen atom
- A01N47/06—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 no bond to a nitrogen atom containing —O—CO—O— groups; Thio analogues thereof
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- Engineering & Computer Science (AREA)
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Abstract
The invention provides a compound thiamethoxam and spirotetramat suspending agent and a preparation method thereof and relates to the technical field of prevention and control of citrus tree scale insects. The compound thiamethoxam and spirotetramat suspending agent is prepared from, at least, 18 parts of thiamethoxam, 12 parts of spirotetramat, 3 parts of fatty alcohol-polyoxyethylene ether, 3 parts of styryl phenol polyoxyethylene ether, 0.3 part of xanthan gum, 0.4 part of sodium benzoate, 0.3 part of defoaming agent and the balance deionized water, and the total amount is 100 parts. All the raw materials are sucked into a preparation kettle and mixed and stirred and then are primarily grinded by a colloid mill, the mixture is finely grinded by a sand mill, sampling analysis is performed, and filtration, metering, package and warehousing are performed after the mixture is qualified. The 30% compound thiamethoxam and spirotetramat suspending agent can play an obvious synergic effect when being used through mixing according to the proportion of 3 to 2, and the range of the obvious synergic effect cannot be reached by other preparations used through mixing according to other proportions.
Description
Technical field
The present invention relates to mandarin tree scale insect Prevention Technique field, be specifically related to a kind of Diacloden and spiral shell worm ethyl ester compounds
Suspending agent and preparation method thereof.
Background technology
At present, the existing Pesticidal combination for preventing and treating mandarin tree scale insect, such as Chinese patent " CN 103814931
" disclosing one " containing the Pesticidal combination of spiral shell worm ethyl ester Yu thiacloprid ", its effective ingredient is spiral shell worm ethyl ester and thiacloprid two to A
Unit is compounding.Wherein spiral shell worm ethyl ester is 1~50: 50~1 with the mass ratio of thiacloprid, effective ingredient spiral shell worm ethyl ester and thiophene worm in preparation
The mass fraction ratio 1%~80% of quinoline, remaining is the auxiliary element allowing in pesticide to use and accept.Separately there is Chinese patent " CN
103814931 A " disclose one " containing the Pesticidal combination of spiral shell worm ethyl ester Yu thiacloprid ", its effective ingredient is spiral shell worm ethyl ester
With thiacloprid binary built.Wherein spiral shell worm ethyl ester is 1~50: 50~1 with the mass ratio of thiacloprid, effective ingredient spiral shell worm in preparation
The mass fraction ratio 1%~80% of ethyl ester and thiacloprid, remaining is the auxiliary element allowing in pesticide to use and accept.
Inventor verifies through long term test, and these above-mentioned several Pesticidal combinations are primarily present following defect:
1), by concrete proportionings several disclosed in above-mentioned several Pesticidal combinations are tested, find mandarin tree is situated between
The preventing and treating of shell worm cannot play good prevention effect.
2), for several dosage forms disclosed in above-mentioned several Pesticidal combinations, find all to there is difference through verification experimental verification
The defect of problem.Such as, wettable powder easily causes product to bond, and is difficult in water dispersion and suspends, or blocking shower nozzle, in spray
The phenomenon such as reason precipitation in day with fog, causes sprinkling irregular.
3), problem is compounded, by concrete proportionings several disclosed in above-mentioned several Pesticidal combinations are carried out virulence test, heat
Storage stability test and mixture co-toxicity coefficient measure and find, are all unable to reach obvious potentiation.
Summary of the invention
An object of the present invention is to provide a kind of Diacloden and spiral shell worm ethyl ester to compound suspending agent, and the design of this suspending agent is closed
Reason, good to the prevention effect of mandarin tree scale insect, and Diacloden and the notable synergistic effect of spiral shell worm ethyl ester can be realized.
For achieving the above object, present invention employs techniques below scheme:
A kind of Diacloden and spiral shell worm ethyl ester compound suspending agent, are made up of following components according to weight portion:
Diacloden belongs to anabasine insecticide, and its mechanism of action is similar to imidacloprid, alternative suppression insecticide maincenter
Nervous system nicotinic acetylcholine esterase receptor, and then block the normal conduction of insect CNS, cause insect to occur
Death during paralysis machine.Not only but have tag, stomach toxicity, systemic activity, and there is higher activity, more preferable safety, more
The features such as wide insecticidal spectrum and speed of action are fast, lasting period length, are to replace that those are high to mammalian toxicity, have residual and environment
The organophosphor of problem, carbamate, the preferable kind of organochlorine insecticides.To coleoptera, Diptera, Lepidoptera, especially
It is that homoptera pest has high activity, can effectively prevent and treat various aphid, leafhopper, plant hopper, aleyrodid, chafer larva, Rhizoma Solani tuber osi first
The insects such as worm, nematicide, ground beetle, leaf miner and knot polytype chemical pesticide produce the insect of resistance.With imidacloprid, pyridine worm
Amidine, Nitenpyram no interactions resistance.Can be not only used for stem and leaf process, seed treatment, can also be used for soil treatment.Suitable for crop is rice
Class crop, Radix Betae, Brassica campestris L, Rhizoma Solani tuber osi, Cotton Gossypii, Kidney bean, fruit tree, Semen arachidis hypogaeae, Helianthi, Semen sojae atricolor, Nicotiana tabacum L. and mandarin orange etc..Recommending agent
Amount is lower to be used to crop safety, without poisoning.
Spiral shell worm ethyl ester is tetronic acid compounds, has the function Characteristics of uniqueness, is to have two-way Uptake and translocation so far
One of modern pesticides of energy.This compound upwards can move down in whole plant, arrives at blade face and bark, thus
Preventing and treating is as on Caulis et Folium Lactucae Sativae and Chinese cabbage internal lobe, and really corticole insect.The interior absorption of this uniqueness can protect newborn stem, Ye He
Root, prevents ovum and the larval growth of insect.Its another feature was that the lasting period is long, it is possible to provide up to effective preventing and treating of 8 weeks.
Diacloden and the spiral shell worm ethyl ester of the present invention compound suspending agent, and its beneficial effect shows:
1), suspending agent prepared by the present invention is in the side such as suspensibility, persistent foamability, wet screening test etc. and heat storage stability
Face is significantly better than that the product prepared by other proportionings.
2), mixed with 3:2 proportioning by experimental verification, Diacloden and spiral shell worm ethyl ester compounded 30% time Diacloden and
Spiral shell worm ethyl ester compounds suspending agent, can play notable synergistic sphere of action, and the preparation that other proportioning is mixed, all it is unable to reach substantially
Potentiation scope.Meanwhile, the actual toxicity of different ratio does not promote along with the enhancing of theoretical toxicity, actual toxicity and reason
Regular change is there is no between opinion toxicity.
Another object of the present invention is to the preparation method providing a kind of Diacloden and spiral shell worm ethyl ester to compound suspending agent, by former
Through grinding at the beginning of colloid mill after material suction preparation still mix and blend, then through sand mill fine grinding, sample analysis, qualified after filter, metering,
Packaging, warehouse-in.
The Diacloden of the present invention and spiral shell worm ethyl ester compound the preparation method of suspending agent, and preparation technology is relatively simple, it is easy to work
Industry metaplasia is produced.
Detailed description of the invention
Below with reference to embodiment, the present invention is described in detail.But, embodiment content is only to this
Bright example and explanation, described specific embodiment is done various repairing by affiliated those skilled in the art
Change or supplement or use similar mode to substitute, without departing from the design of invention or surmount defined in the claims
Scope, all should belong to protection scope of the present invention.
One, Diacloden and spiral shell worm ethyl ester compound the preparation of suspending agent, and the suspending agent prepared by each embodiment is every
The testing result of technical specification, heat storage stability result of the test.
Embodiment 1
30% Diacloden and spiral shell worm ethyl ester compound suspending agent, and each component and weight proportion thereof are as follows:
Composition | Weight portion |
Diacloden | 18 |
Spiral shell worm ethyl ester | 12 |
Fatty alcohol-polyoxyethylene ether | 3 |
Styrylphenol polyoxyethylene ether | 3 |
Xanthan gum | 0.3 |
Sodium benzoate | 0.4 |
Defoamer | 0.3 |
Deionized water | 63 |
Preparation method: through grinding at the beginning of colloid mill after raw material suction is prepared still mix and blend, then through sand mill fine grinding, sampling
Analyze, qualified after filter, measure, pack, put in storage.
Embodiment 2
29% Diacloden and spiral shell worm ethyl ester compound suspending agent, and each component and weight proportion thereof are as follows:
Composition | Weight portion |
Diacloden | 17 |
Spiral shell worm ethyl ester | 12 |
Fatty alcohol-polyoxyethylene ether | 3 |
Styrylphenol polyoxyethylene ether | 3 |
Xanthan gum | 0.3 |
Sodium benzoate | 0.4 |
Defoamer | 0.3 |
Deionized water | 64 |
Preparation method is with embodiment 1.
Embodiment 3
28% Diacloden and spiral shell worm ethyl ester compound suspending agent, and each component and weight proportion thereof are as follows:
Composition | Weight portion |
Diacloden | 17 |
Spiral shell worm ethyl ester | 11 |
Fatty alcohol-polyoxyethylene ether | 3 |
Styrylphenol polyoxyethylene ether | 3 |
Xanthan gum | 0.3 |
Sodium benzoate | 0.4 |
Defoamer | 0.3 |
Deionized water | 65 |
Preparation method is with embodiment 1.
Embodiment 4
31% Diacloden and spiral shell worm ethyl ester compound suspending agent, and each component and weight proportion thereof are as follows:
Composition | Weight portion |
Diacloden | 18 |
Spiral shell worm ethyl ester | 13 |
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 5
32% Diacloden and spiral shell worm ethyl ester compound suspending agent, and each component and weight proportion thereof are as follows:
Preparation method is with embodiment 1.
Embodiment 6
30% Diacloden and spiral shell worm ethyl ester compound suspending agent, and each component and weight proportion thereof are as follows:
Composition | Weight portion |
Diacloden | 18 |
Spiral shell worm ethyl ester | 12 |
Aucubin | 0.4 |
Fatty alcohol-polyoxyethylene ether | 3 |
Styrylphenol polyoxyethylene ether | 3 |
Xanthan gum | 0.3 |
Sodium benzoate | 0.4 |
Defoamer | 0.3 |
Deionized water | 62.6 |
Preparation method is with embodiment 1.
Diacloden and spiral shell worm ethyl ester prepared by embodiment 1~6 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 it 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 embodiments.
Two, toxicological information
Diacloden: rat acute per os LD50: 1563mg/kg, eyes and skin are had no stimulation by this product.
Spiral shell worm ethyl ester: acute oral LD50: Mus great and mighty or powerful > 21440mg/kg, female rat > 42880mg/kg, male mice >
53600mg/kg, female mice > 107200mg/kg.Acute percutaneous LD50: Mus great and mighty or powerful > 1072mg/kg, female mice > 2140mg/kg.
Three, Diacloden and spiral shell worm ethyl ester compound indoor biological activity (virulence) mensuration of suspending agent.
1 test objective
Determine Diacloden and spiral shell worm ethyl ester compounds the suspending agent activity to mandarin tree scale insect, be used for preventing and treating for this medicament
Mandarin tree scale insect provides foundation.
2 experimental conditions
2.1 for examination worm source
Mandarin tree scale insect, is provided by Hunan Inst. of Tea.Selection body colour is consistent, mandarin tree shell of uniform size
Worm is to be measured.
2.2 condition of culture
Raise under conditions of examination worm is placed in temperature 24 ± 1 DEG C, illumination ∥ dark=16h//8h, humidity 60-70%.
2.3 instrument and equipment
Brush pen, volumetric flask, tweezers, electronic balance, constant incubator, culture dish, graduated cylinder, filter paper, liquid-transfering gun etc..
3 EXPERIMENTAL DESIGN
3.1 reagent
3.1.1 reagent agent
The former medicine of Diacloden, Anhui Meilan Agricultural Development Co., Ltd. provides.
The former medicine of spiral shell worm ethyl ester, Anhui Meilan Agricultural Development Co., Ltd. provides.
3.1.2 other reagent
The reagent such as acetone.
3.2 tests process
3.2.1 dosage processes
The each 1mL of suspending agent prepared by Example 1-6, is settled to 1000ml with acetone, then is diluted to 80mg/L, 40mg/
L, 20mg/L, 10mg/L medicinal liquid is stand-by;
3.2.2 repetition is tested
Often process 4 times and repeat, often repeat 20 examination worms, and set acetone without medicament as blank.
4 test methods
Use the drop method that NY/T 1154.1-2006 recommends: first with appropriate ether by mandarin tree scale insect adult half fiber crops
Liquor-saturated, choose mandarin tree scale insect of the same size with brush pen and be placed in culture dish stand-by.Carry out trying worm in culture dish a little by head
Dripping and process, medicinal liquid drop is on mandarin tree scale insect pronotary, and every some drops physic liquor 1.0 μ L, by the examination worm difference after drop
It is transferred under dependent insect cage normal condition raise.Starting timing after etherization event resolves, 24h checks dead borer population.Often process 4
Secondary repetition, often repeats 20 examination worms, and sets acetone without medicament as blank.Comparison mortality rate is effectively to survey less than 5%
Fixed.
5 data surveys and statistical analysis
5.1 computational methods
According to survey data, calculate the corrected mortality of each process.
Corrected mortality presses formula (1), and formula (2) calculates, and unit is percentage rate (%), and result of calculation retains after arithmetic point two
Position:
In formula: P1Mortality rate
K death borer population
N processes total borer population
In formula: P2Corrected mortality
PtProcess mortality rate
P0Blank mortality rate
If comparison mortality rate < 5%, it is not necessary to correction;Comparison mortality rate, between 5%-20%, should carry out school by formula (2)
Just;Comparison mortality rate > 20%, test need to be reformed.
5.2 statistical analysis
It is independent variable x with the logarithm value of drug concentration (mg/L), with the probit value of corrected mortality for dependent variable y, respectively
Set up virulence regression equation formula, use DPS software to be analyzed, obtain correlation coefficient r value, LC50Value.
5.3 result of the test
Diacloden and spiral shell worm ethyl ester prepared by embodiment 1-6 compound the suspending agent LC to mandarin tree scale insect50Value is followed successively by
1.2485mg/L、2.4445mg/L、2.5487mg/L、2.5883mg/L、2.6468mg/L、1.1725mg/L。
6 conclusions
The present invention passes through appropriate design product forms and each proportioning raw materials, makes 30% Diacloden and the spiral shell worm ethyl ester of preparation
Compounding suspending agent is than other dosage form medicament, and its preventing and treating mandarin tree scale insect effect is obvious.Meanwhile, by the experiment of embodiment 6
After data are it can be seen that with the addition of a small amount of aucubin in suspending agent, prevention effect can be made more preferably.
Claims (2)
1. a Diacloden and spiral shell worm ethyl ester compound suspending agent, it is characterised in that: at least it is made up of the component of following weight portion:
2. prepare Diacloden as claimed in claim 1 and method that spiral shell worm ethyl ester compounds suspending agent for one kind, it is characterised in that: by former
Through grinding at the beginning of colloid mill after material suction preparation still mix and blend, then through sand mill fine grinding, sample analysis, qualified after filter, metering,
Packaging, warehouse-in.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110178851A (en) * | 2019-06-04 | 2019-08-30 | 广西汇丰生物科技有限公司 | A kind of Pesticidal combination of spirotetramat and Diacloden |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2008077922A2 (en) * | 2006-12-22 | 2008-07-03 | Bayer Cropscience Ag | Pesticidal composition comprising fenamidone and an insecticide compound |
CN101489393A (en) * | 2006-07-11 | 2009-07-22 | 拜尔农作物科学股份公司 | Active ingredient combinations with insecticidal and acaricidal properties |
CN101637159A (en) * | 2009-09-08 | 2010-02-03 | 深圳诺普信农化股份有限公司 | Pesticide composition with synergistic action |
CN103688979A (en) * | 2013-12-19 | 2014-04-02 | 李视辉 | Pesticidal composition containing thiamethoxam and spirotetramat |
-
2016
- 2016-08-25 CN CN201610723423.5A patent/CN106305761A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101489393A (en) * | 2006-07-11 | 2009-07-22 | 拜尔农作物科学股份公司 | Active ingredient combinations with insecticidal and acaricidal properties |
WO2008077922A2 (en) * | 2006-12-22 | 2008-07-03 | Bayer Cropscience Ag | Pesticidal composition comprising fenamidone and an insecticide compound |
CN101637159A (en) * | 2009-09-08 | 2010-02-03 | 深圳诺普信农化股份有限公司 | Pesticide composition with synergistic action |
CN103688979A (en) * | 2013-12-19 | 2014-04-02 | 李视辉 | Pesticidal composition containing thiamethoxam and spirotetramat |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110178851A (en) * | 2019-06-04 | 2019-08-30 | 广西汇丰生物科技有限公司 | A kind of Pesticidal combination of spirotetramat and Diacloden |
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Application publication date: 20170111 |