CN104886122B - Compound composition containing dufulin and pyrazole amide bactericide and bactericide - Google Patents
Compound composition containing dufulin and pyrazole amide bactericide and bactericide Download PDFInfo
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- CN104886122B CN104886122B CN201510337206.8A CN201510337206A CN104886122B CN 104886122 B CN104886122 B CN 104886122B CN 201510337206 A CN201510337206 A CN 201510337206A CN 104886122 B CN104886122 B CN 104886122B
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Abstract
The invention provides compound composition containing dufulin and a pyrazole amide bactericide and bactericide. The active ingredients of the compound composition comprise dufulin and the pyrazole amide bactericide, wherein the pyrazole amide bactericide is selected from one or more of fluopicolide, Bixafen, sedaxane, isopyrazam, benzovindiflupyr or penflufen; a weight ratio of dufulin to the pyrazole amide bactericide is (40:1)-(1:70). The invention further provides the bactericide. The compound composition accounts for 0.5%-84% of the total weight of the bactericide. The compound composition has remarkable synergistic interaction effect compared with a single pesticide, can effectively control diseases of various crops, has the function of improving the control effect, and has the effects of reducing pesticide application quantity and cost, delaying pesticide resistance and the like.
Description
Technical field
The present invention relates to technical field of pesticide, especially relate to compounding group of toxic fluoride phosphate and pyrazol acid amide fungicide compounding
Compound and its antibacterial.
Background technology
Chemical agent is the important means preventing and treating crop pest, and the change with environment, and crop occurs the journey of virosiss
Degree increases, but crop is caused harm with being also subjected to other diseases while being caused harm by virosiss, and can prevent and treat multiple diseases on market
The medicament shortcoming of evil or the big preventive effect of resistance decline.And carrying out compounding using the pesticide active ingredient of the different mechanisms of action is to grind at present
Pesticide new product processed and a kind of effective quick way preventing and treating resistance pest and disease damage.After different pesticide active ingredients carry out compounding,
Three kinds of type of action: summation action, potentiation and antagonism can be shown.Generally, only by substantial amounts of test ability
Learn different pesticide active ingredients compound after type of action.
Through overtesting, inventor finds that toxic fluoride phosphate and pyrazol acid amide fungicide compounding prevent and treat crop pest, potentiation shows
Write.
Toxic fluoride phosphate is that inventor transfers the possession of, by Guizhou University, the plant virus resistance product (patent No. of new generation coming
Zl200510003041.7), it is a kind of novel fluorine-containing amino phosphonate ester new Antiphytoviral medicament of structure.In view of it
Structure novelty, the characteristic such as mechanism of action uniqueness, toxic fluoride phosphate is used for preventing and treating virosiss effect very prominent.But in pesticide field
In, it is also noted that protection during good Pesticide use, find different classes of pesticide species and use with its mixture, improve prevention effect
While, the service life of excellent pesticide can also be delayed.
The preferred fluopicolide of pyrazole amide series bactericidal agent, biphenyl pyrrole bacterium amine, fluorine azoles ring bacterium amine, isopyrazam, benzo
Alkene fluorine bacterium azoles, fluorine azoles bacterium aniline.Above-mentioned pyrazole amide series bactericidal agent is known in this field and published antibacterial kind.
The cas 239110-15-7 of fluopicolide, English name fluopicolide.
The cas 581809-46-3, English name bixafen of biphenyl pyrrole bacterium amine.
The cas 874967-67-6 of fluorine azoles ring bacterium amine, empirical formula c18h19f2n3o.
Isopyrazam is a kind of fungicidal activity composition having prevention and treatment property concurrently, belongs to sdhi series bactericidal agent, energy
Long-acting prevention and control crop diseases.The mechanism of action of this composition is the respiratory enzyme in suppression pathogen mitochondrial membrane.
Benzo alkene fluorine bacterium azoles, English name benzovindiflupyr, many crops such as preventing and treating Semen Tritici aestivi, Semen Maydiss all present
Outstanding preventive effect to Major Diseases.
The cas 494793-67-8 of fluorine azoles bacterium aniline, iso common name penflufen.
Through retrieval, do not find the relevant report of the complex composition of toxic fluoride phosphate and pyrazole amide series bactericidal agent.
Content of the invention
In view of this, in view of the shortcomings of the prior art, present invention aim at providing one kind to contain toxic fluoride phosphate and pyrazoles
The complex composition of acid amide fungicides and antibacterial, this complex composition and antibacterial have significantly collaborative with respect to single dose
Potentiation, improves bactericidal activity, reduces the dosage of pesticide, reduces cost, expanding prevention is composed, and also delays the drug resistance of pathogen
Property.
For the actual arrival purpose of the present invention, adopt the technical scheme that:
The present invention provides a kind of complex composition, and this complex composition active component is sterilized by toxic fluoride phosphate and pyrazol acid amide
Agent forms;Described pyrazole amide series bactericidal agent is selected from fluopicolide, biphenyl pyrrole bacterium amine, fluorine azoles ring bacterium amine, isopyrazam, benzene
And any one or a few in alkene fluorine bacterium azoles, fluorine azoles bacterium aniline;Described toxic fluoride phosphate and the weight of pyrazole amide series bactericidal agent
Than for 40:1 to 1:70.
Preferably, the weight of described toxic fluoride phosphate and pyrazole amide series bactericidal agent is than for 20:1 to 1:40;It is highly preferred that weight
Amount ratio is 10:1 to 1:20.
The present invention also provides a kind of antibacterial of complex composition described above, and complex composition described above accounts for sterilization
The 0.5-84% of agent gross weight.Preferably, complex composition described above accounts for the 4-60% of antibacterial gross weight.
The antibacterial that the present invention provides, in addition to including toxic fluoride phosphate and pyrazole amide series bactericidal agent, also includes can connecing on pesticide
The auxiliary element being subject to.
On pesticide of the present invention, acceptable auxiliary element includes filler, solvent, emulsifying agent, wetting agent, dispersant
Deng other conventional functionality auxiliary agents such as antifreezing agent, thickening agent, defoamer, disintegrating agent, film former also can be added if necessary.
Filler is precipitated calcium carbonate, Kaolin, bentonite, kieselguhr, soil powder, carbamide, montmorillonite.
Solvent is water, Ketohexamethylene, n- methyl pyrrolidone, methyl oleate, vegetable oil, dimethylbenzene, c10 aromatic hydrocarbons.
Emulsifying agent, wetting agent, dispersant are styrylphenol polyoxyethylene ether, calcium dodecyl benzene sulfonate, polycarboxylic acids
Salt, thermally coupled distillation columns, alkylaryl polyoxyethylene polyoxypropylene ether again, alkylphenol polyoxyethylene phosphate ester,
Fatty alcohol-polyoxyethylene ether, phenethyl phenyl polyoxyethylene poly-oxygen propylene aether, styryl phenyl polyoxyethylene ether, nonyl phenol gather
Oxygen vinyl Ether, alkyl polyoxyethylene sulfate salt, alkylnaphthalene sulfonate, tea saponin, Negel, naphthalene sulfonate, dodecane
Base sodium sulfate, sodium butylnaphthalenesulfonate, lauryl alcohol polyethylene glycol oxide base ether, sodium laurylsulfate, sodium carboxymethyl cellulose, methylene two
Sodium naphthalene sulfonate, the formaldehyde condensation products of methyl naphthalene sulfonic acid sodium, sodium lignin sulfonate, alkylphenol-polyethenoxy base phosphate ester, lignin
Sulfoacid calcium, aliphatic alcohol polyethenoxy base ether, aliphatic alcohol polyoxyvinethene phosphate, acrylate homopolymer sodium salt.
Disintegrating agent is ammonium chloride, potassium sulfate, sodium sulfate, ammonium carbonate, calcium superphosphate, carbamide, Diammonium phosphate (DAP).
Thickening agent is xanthan gum, pectin, Magnesiumaluminumsilicate, arabic gum.
Antifreezing agent is glycerol, ethylene glycol, isopropanol.
Warning coloration is pinkish red, acid scarlet.
Film former is carboxymethyl cellulose, starch, polyvinyl alcohol.
Binding agent is ethyl cellulose, polyvinyl alcohol, starch.
Antibacterial of the present invention can be prepared into following dosage form: wettable powder, water dispersible granules, suspending agent, seed
Process dry powder doses, granule or ultra low volume liquids.
Antibacterial of the present invention can be used for preventing and treating various crop pests, concrete such as cucumber downy mildew, tomato virus disease.
Antibacterial of the present invention can be applied by commonsense method, such as spraying cauline leaf process, also can soil treatment, such as
Solid root spreads fertilizer over the fields or liquid pouring root is moreover it is possible to seed dressing, seed soaking or seed pelleting use.
The complex composition of the present invention and antibacterial have the advantages that with respect to prior art
(1) complex composition of the present invention, in certain ratio range, mixture shows excellent potentiation, and preventing and treating is made
The co-toxicity coefficient of thing disease is more than 120, and the bactericidal effect of complex composition is significantly improved compared with its single dose.
(2) reduce the using dosage of pesticide, reduce peasant's drug cost.
(3) utilize the different mechanisms of action of two kinds of active components, mutual supplement with each other's advantages can be played, reasonably mixture, both extend
In the Pesticide use life-span, delay the drug-fast generation of pathogen again.
Specific embodiment
Below by embodiment, the invention will be further described.It should be noted that the embodiment of the present invention is only to use
In the explanation present invention, rather than limitation of the present invention.Toxic fluoride phosphate active compound used in the present invention is synthesized by inventor, and other make
Active compound and preparation are commercial.In the application if no special instructions, percentage ratio is all weight percentage.
First, the preparation of wettable powder
Preparation method: toxic fluoride phosphate, pyrazole amide series bactericidal agent (abbreviation component b), wetting agent, dispersant, white carbon, are filled out
Material mix homogeneously, after pulverizing through jet mill, stirs 30min, obtains the wettable powder of antibacterial of the present invention.
2nd, the preparation of water dispersible granules
Preparation method: by toxic fluoride phosphate, pyrazole amide series bactericidal agent (abbreviation component b), wetting agent, dispersant, filler mixing
Uniformly, through jet mill pulverizing after, stir 30min, mediate and add pelletize in fluid bed, then use drying machine in be dried,
Screening obtains the water dispersible granules of antibacterial of the present invention.
3rd, the preparation of suspending agent
Preparation method: by emulsifying agent, antifreezing agent, thickening agent, deionized water mixing, through high speed shear mix homogeneously, successively
Add toxic fluoride phosphate, pyrazole amide series bactericidal agent (abbreviation component b), abrading-ball 2~3 hours in ball crusher, prepared present invention sterilization
The suspending agent of agent.
4th, seed treatment dry powder doses
By formula proportion, by toxic fluoride phosphate and pyrazole amide series bactericidal agent (abbreviation component b), each auxiliary agent premixing uniformly, so
Pulverize through pulverizer afterwards, pulverize and complete mix homogeneously again, obtain final product the seed treatment dry powder doses of antibacterial of the present invention.
5th, the preparation of granule
By toxic fluoride phosphate, pyrazole amide series bactericidal agent, (abbreviation component b), auxiliary agent, solid carrier are mixed in airtight compounding kettle
Close uniformly, using peplos method pelletize, screened, drys, check after, that is, obtain the granule of antibacterial of the present invention.
6th, the preparation of ultra low volume liquids
BIOLOGICAL ACTIVITY EXAMPLES
Toxicity Determination:
Following indoor biometricses test calculates co-toxicity coefficient (ctc) to evaluate mixed effect using the abundant method of Sun Yun.
Toxicity index ti (b)=(ec of standard agent a50The ec50 of ÷ b agent) × 100
Actual toxicity index ati (ab)=(ec of a50The ec50 of ÷ ab) × 100
Theoretical toxicity index tti (ab)=ti (a) × a percentage in mixture in the percent+ti (b) in mixture × b
Number
Co-toxicity coefficient (ctc)=[mixture actual measurement toxicity index (ati) ÷ mixture theoretical toxicity index (tti)] × 100
Evaluation criterion: (ctc) >=120 show as potentiation;Ctc≤80 show as antagonism;80 < ctc < 120
Show as summation action.
Toxicity Determination embodiment one
Test method: with reference to " nyt 1156.7-2006 " and " ny/t 1156.6-2006 ", calculate the ec of each medicament50, and
Calculate the co-toxicity coefficient of mixture according to the abundant method of Sun Yun.Measurement result is shown in Table 1-3.
The Toxicity Determination result of cucumber downy mildew prevented and treated by table 1
Composition | ec50(μg/ml) | ati | tti | ctc |
Toxic fluoride phosphate (a) | 112.60 | 100.00 | / | / |
Fluopicolide (b) | 6.31 | 1784.47 | / | / |
A:b=40:1 | 58.35 | 192.97 | 141.08 | 136.78 |
A:b=30:1 | 49.71 | 226.51 | 154.34 | 146.77 |
A:b=20:1 | 38.04 | 296.00 | 180.21 | 164.25 |
A:b=10:1 | 27.52 | 409.16 | 253.13 | 161.64 |
A:b=5:1 | 15.05 | 748.17 | 380.74 | 196.50 |
A:b=2.5:1 | 10.53 | 1069.33 | 581.28 | 183.96 |
A:b=1:1 | 6.67 | 1688.16 | 942.23 | 179.17 |
A:b=1:2.5 | 4.54 | 2480.18 | 1303.19 | 190.32 |
A:b=1:5 | 3.87 | 2909.56 | 1503.72 | 193.49 |
A:b=1:10 | 3.08 | 3655.84 | 1631.34 | 224.10 |
A:b=1:20 | 3.18 | 3540.88 | 1704.26 | 207.77 |
A:b=1:30 | 3.75 | 3002.67 | 1730.13 | 173.55 |
A:b=1:40 | 4.22 | 2668.25 | 1743.38 | 153.05 |
A:b=1:50 | 4.31 | 2612.53 | 1751.44 | 149.16 |
A:b=1:60 | 4.82 | 2336.10 | 1756.85 | 132.97 |
A:b=1:70 | 5.22 | 2157.09 | 1760.74 | 122.51 |
The Toxicity Determination result of cucumber downy mildew prevented and treated by table 2
The Toxicity Determination result of cucumber downy mildew prevented and treated by table 3
Composition | ec50(μg/ml) | ati | tti | ctc |
Toxic fluoride phosphate (a) | 114.50 | 100.00 | / | / |
Fluorine azoles ring bacterium amine (d) | 12.85 | 891.05 | / | / |
A:d=40:1 | 75.09 | 152.48 | 119.29 | 127.82 |
A:d=30:1 | 67.24 | 170.29 | 125.52 | 135.67 |
A:d=20:1 | 55.31 | 207.02 | 137.67 | 150.37 |
A:d=10:1 | 36.68 | 312.16 | 171.91 | 181.58 |
A:d=5:1 | 25.42 | 450.43 | 231.84 | 194.28 |
A:d=2.5:1 | 21.55 | 531.32 | 326.01 | 162.98 |
A:d=1:1 | 12.74 | 898.74 | 495.53 | 181.37 |
A:d=1:2.5 | 10.39 | 1102.02 | 665.04 | 165.71 |
A:d=1:5 | 9.81 | 1167.18 | 759.21 | 153.74 |
A:d=1:10 | 8.82 | 1298.19 | 819.14 | 158.48 |
A:d=1:20 | 8.94 | 1280.76 | 853.38 | 150.08 |
A:d=1:30 | 9.20 | 1244.57 | 865.53 | 143.79 |
A:d=1:40 | 9.56 | 1197.70 | 871.76 | 137.39 |
A:d=1:50 | 9.36 | 1223.29 | 875.54 | 139.72 |
A:d=1:60 | 10.10 | 1133.66 | 878.08 | 129.11 |
A:d=1:70 | 10.52 | 1088.40 | 879.91 | 123.69 |
From table 1-3, toxic fluoride phosphate and pyrazole amide series bactericidal agent are compounding in the range of 40:1-1:70, prevent and treat Fructus Cucumidis sativi
The co-toxicity coefficient of downy mildew is more than 120, shows obvious synergistic function.
Toxicity Determination embodiment two
Test method: indoor pot Nicotiana tabacum L. susceptible variety plant to 4-5 leaf phase, is mixed with the medicinal liquid of different ratio variable concentrations
Close isopyknic virus juice frictional inoculation, often process 3 plants, 3 leaves of often selecting good strains in the field for seed, it is repeated 4 times, after 3-4 days, investigate withered spot number, meter
Calculate suppression ratio, press the abundant method of Sun Yun with ec50 value and calculate co-toxicity coefficient.Measurement result is shown in Table 4-6.
The Toxicity Determination result of tomato virus disease prevented and treated by table 4
Composition | ec50(μg/ml) | ati | tti | ctc |
Toxic fluoride phosphate (a) | 34.56 | 100.00 | / | / |
Fluopicolide (b) | 121.60 | 28.42 | / | / |
A:b=40:1 | 26.33 | 131.26 | 98.25 | 133.59 |
A:b=30:1 | 25.16 | 137.36 | 97.69 | 140.61 |
A:b=20:1 | 25.60 | 135.00 | 96.59 | 139.76 |
A:b=10:1 | 24.53 | 140.89 | 93.49 | 150.69 |
A:b=5:1 | 25.42 | 135.96 | 88.07 | 154.37 |
A:b=2.5:1 | 21.29 | 162.33 | 79.55 | 204.06 |
A:b=1:1 | 29.71 | 116.32 | 64.21 | 181.16 |
A:b=1:2.5 | 36.28 | 95.26 | 48.87 | 194.91 |
A:b=1:5 | 48.27 | 71.60 | 40.35 | 177.44 |
A:b=1:10 | 58.56 | 59.02 | 34.93 | 168.96 |
A:b=1:20 | 69.50 | 49.73 | 31.83 | 156.23 |
A:b=1:30 | 75.31 | 45.89 | 30.73 | 149.33 |
A:b=1:40 | 73.55 | 46.99 | 30.17 | 155.76 |
A:b=1:50 | 83.36 | 41.46 | 29.82 | 139.01 |
A:b=1:60 | 91.16 | 37.91 | 29.59 | 128.10 |
A:b=1:70 | 93.63 | 36.91 | 29.43 | 125.42 |
The Toxicity Determination result of tomato virus disease prevented and treated by table 5
The Toxicity Determination result of tomato virus disease prevented and treated by table 6
The Toxicity Determination result of tomato virus disease prevented and treated by table 6
Composition | ec50(μg/ml) | ati | tti | ctc |
Toxic fluoride phosphate (a) | 33.10 | 100.00 | / | / |
Fluorine azoles bacterium aniline (g) | 138.80 | 23.85 | / | / |
A:g=40:1 | 27.11 | 122.10 | 98.14 | 124.41 |
A:g=30:1 | 25.26 | 131.04 | 97.54 | 134.34 |
A:g=20:1 | 23.58 | 140.37 | 96.37 | 145.66 |
A:g=10:1 | 24.29 | 136.27 | 93.08 | 146.41 |
A:g=5:1 | 19.62 | 168.71 | 87.31 | 193.23 |
A:g=2.5:1 | 25.34 | 130.62 | 78.24 | 166.95 |
A:g=1:1 | 30.75 | 107.64 | 61.92 | 173.83 |
A:g=1:2.5 | 44.98 | 73.59 | 45.61 | 161.36 |
A:g=1:5 | 59.63 | 55.51 | 36.54 | 151.92 |
A:g=1:10 | 73.26 | 45.18 | 30.77 | 146.84 |
A:g=1:20 | 86.22 | 38.39 | 27.47 | 139.73 |
A:g=1:30 | 89.14 | 37.13 | 26.30 | 141.17 |
A:g=1:40 | 95.53 | 34.65 | 25.70 | 134.80 |
A:g=1:50 | 93.66 | 35.34 | 25.34 | 139.46 |
A:g=1:60 | 102.27 | 32.37 | 25.10 | 128.97 |
A:g=1:70 | 104.35 | 31.72 | 24.92 | 127.29 |
From table 4-6, toxic fluoride phosphate and pyrazole amide series bactericidal agent are compounding in the range of 40:1-1:70, prevent and treat Fructus Lycopersici esculenti
The co-toxicity coefficient of virosiss is more than 120, shows obvious synergistic function.
Land for growing field crops test examples
For the prevention effect to each crop pest when clear and definite toxic fluoride phosphate is alone with pyrazole amide series bactericidal agent and mixed, this
Different regions have carried out substantial amounts of field test to patent application people at home.Wettable powder abbreviation wp.Water dispersible granules are referred to as
Wdg, suspending agent abbreviation sc, ultra low volume liquids abbreviation ulv.
Comparison medicament is:
Ck1:30% toxic fluoride phosphate wettable powder, registration card ls20130359, Guangxi Tianyuan Biochemical Co., Ltd.;
Ck2:20% fluopicolide wettable powder, self-control;
Ck3:20% biphenyl pyrrole bacterium aqueous amine dispersible granule, self-control;
Ck4:20% fluorine azoles ring bacterium amine wettable powder, self-control;
Ck5:20% isopyrazam wettable powder, self-control;
Ck6:20% benzo alkene triflumizole water dispersant, self-control;
Ck7:20% fluorine azoles bacterium aniline wettable powder, self-control.
Field efficacy embodiment one:
Test method: test method and investigation method: with reference to " gb/t17980.26-2000 pesticide field efficacy medicine test is accurate
Then (one): bactericidal agent for preventing and treating cucumber downy mildew ", carry out first time dispenser before disease is sent out or when beginning and seeing scab, after 5d, carry out second
Secondary dispenser, twice, each processes plot area is 20m for dispenser altogether2, number of repetition 4 times.Result of the test is shown in Table 7.
The field control effectiveness test result of cucumber downy mildew prevented and treated by table 7
According to field control effectiveness test result table 7, toxic fluoride phosphate respectively with fluopicolide, biphenyl pyrrole bacterium amine, fluorine azoles ring
Bacterium amine compounds during preventing and treating cucumber downy mildew on the premise of consumption a small amount of single dose consumption, and its preventive effect is apparently higher than comparison single dose, table
Reveal obvious potentiation.Complex preparation 14d after second medicine can also keep good drug effect (all more than 88%), holds
The effect phase is long.
Field efficacy embodiment two:
Test method and investigation method: with reference to " ny/t1464.8-2007 pesticide field efficacy medicine test criterion the 8th part: kill
Tomato virus disease prevented and treated by microbial inoculum ", before disease occurs or early period of origination for the first time sprays dispenser, after 5d, second spray is applied
Medicine.Twice, each processes plot area is 20m for dispenser altogether2, number of repetition 4 times.
Investigation method: 7d, 14d investigation before dispenser and after last dispenser, the random 5 points of samplings of every cell, every takes 6
Strain, investigation total strain number, diseased plant number at different levels.Result of the test is shown in Table 8.
The field control effectiveness test result of tomato virus disease prevented and treated by table 8
According to field control effectiveness test result table 8, toxic fluoride phosphate compounds anti-respectively with fluopicolide, isopyrazam etc.
Control during tomato virus disease on the premise of consumption a small amount of single dose consumption, its preventive effect, apparently higher than comparison single dose, shows significantly
Potentiation.Complex preparation 14d after second medicine can also keep good drug effect (all more than 83%), and the lasting period is long.
Claims (9)
1. a kind of complex composition is it is characterised in that described complex composition active component is killed by toxic fluoride phosphate and pyrazol acid amide
Microbial inoculum forms;Described pyrazole amide series bactericidal agent is fluopicolide;Described toxic fluoride phosphate and the weight of pyrazole amide series bactericidal agent
Amount ratio is 40:1 to 1:70.
2. complex composition according to claim 1 is it is characterised in that described toxic fluoride phosphate and pyrazole amide series bactericidal agent
Weight than for 20:1 to 1:40.
3. complex composition according to claim 2 is it is characterised in that described toxic fluoride phosphate and pyrazole amide series bactericidal agent
Weight than for 10:1 to 1:20.
4. a kind of antibacterial containing the arbitrary described complex composition of claim 1-3 is it is characterised in that described compounded combination
Thing accounts for the 0.5-84% of antibacterial gross weight.
5. antibacterial according to claim 4 is it is characterised in that described complex composition accounts for the 4- of antibacterial gross weight
60%.
6. antibacterial according to claim 4 is it is characterised in that described antibacterial also includes acceptable auxiliary on pesticide
Composition.
7. antibacterial according to claim 4 is it is characterised in that described antibacterial is prepared into following dosage form: wettable powder
Agent, water dispersible granules, suspending agent, seed treatment dry powder doses, granule or ultra low volume liquids.
8. purposes in preventing and treating crop pest for the antibacterial described in claim 4.
9. purposes in preventing and treating crop pest for the antibacterial described in any one of claim 5-7.
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