CN1781376A - Use of walnut plant extract as pesticide in preventing and controlling diamondback moth - Google Patents

Use of walnut plant extract as pesticide in preventing and controlling diamondback moth Download PDF

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Publication number
CN1781376A
CN1781376A CN 200410009965 CN200410009965A CN1781376A CN 1781376 A CN1781376 A CN 1781376A CN 200410009965 CN200410009965 CN 200410009965 CN 200410009965 A CN200410009965 A CN 200410009965A CN 1781376 A CN1781376 A CN 1781376A
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juglone
walnut
pesticide
extract
purposes
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CN1314327C (en
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林开春
曾水云
汪威
董岑洲
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LUSHIJI BIO-ENGINEERING Co Ltd WUHAN
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LUSHIJI BIO-ENGINEERING Co Ltd WUHAN
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Abstract

The present invention relates to application of juglans plant extract as pesticide in preventing and controlling diamondback moth. The leaf, fruit coating and branch bark of juglans plant are used as main material to prepare juglone liquid, and the juglone liquid is then compounded into pesticide alone or together with other farm pesticide for preventing and controlling diamondback moth. The present invention has high pesticidal activity on diamondback moth, and compared with other chemical pesticide, the botanical pesticide is more environmental friendly.

Description

The walnut extract is as the application of insecticide pesticide on the control diamond-back moth
[technical field]
The present invention relates to the walnut extract as insecticide pesticide in the application aspect the pest control, particularly relate to the walnut extract as insecticide pesticide in the application of control on the diamond-back moth.
[background technology]
Walnut has 18 kinds, and there are 1 mutation of 4 kinds and 2 introduction cultivated speciess in China.The kernel of walnut, branch, leaf, pericarp can be used as medicine and eat, and have certain economic and are worth.The history in existing more than 100 year of research for the chemical substance in juglandis folia, pericarp, the branch skin.Just determined in 1885 to contain 5-hydroxyl-1 in the leaf, pericarp, branch skin of walnut, the 4-naphthoquinones is commonly called as juglone.Find to contain in these plants Hyperoside, avicularin, juglanin, α-hydrojuglone-4-β-compounds such as D-glucoside later on again.The content of juglone is higher in the above-claimed cpd, can reach 4/10000ths of bright leaf net weight.
To the biologically active and the existing a large amount of reports of application thereof of juglone, think that mainly it is a kind of toxic compounds very malicious to aquatile, high malicious to fish, even under 10ppm concentration, also can cause death to the loach of vitality extra-heavy.Also find the allelopathy of juglone to other plant.The antibacterial action of juglone generally acknowledges that also this material all has very strong bacteriostatic activity to anthrax-bacilus, Salmonella, Diplococcus pneumopniae.Also very strong to bacteriostatic activities such as the disease funguses of crops such as Pyricularia oryzae, the wilting germ of cotton, Rhizoctonia solani Kuhn, cotton-wilt fusariums.Nearly ten years, juglone had a large amount of reports to the inhibitory action of tumour cell.Mainly as the protection of human body and animal tissue's organ ischemia injury with to cardiac muscle cell's protection, avicularin is used to diuresis, treating stranguria to Hyperoside in the walnut extract, the effect that brings high blood pressure down in addition.
At present, only as seen use juglandis folia, pericarp, branch severe edema due to hypofunction of the spleen extract killing aphids and leucoma candida, and with fragmentary reports such as evil mites in the anti-bee colony of the cigarette of juglandis folia burning, but what all undeclared wherein contained insecticide active substance of all reports is, and do not see the report that has juglone to be used to kill diamond-back moth as insecticide so far.
[summary of the invention]
Active substance juglone in the leaf of a large amount of test discovery of the present invention's process walnuts, pericarp, the branch bark extract has stronger insecticidal activity to diamond-back moth.According to this discovery, utilize the walnut extract to prepare list agent of juglone desinsection and compound insecticidal agricultural chemicals, be used to prevent and treat diamond-back moth.
The present invention utilizes the diamond-back moth agricultural chemicals extremely of walnut extract preparation; through evidence; its drug effect is significantly higher than the present conventional biological and chemical that uses and kills the diamond-back moth agricultural chemicals, is the botanical pesticide that kills diamond-back moth of agriculture coideal, compares with general chemical pesticide more to help environmental protection.
Technical scheme of the present invention is specific as follows:
The vegetable material that the present invention is used for raw materials for production is juglans tree, the particularly leaf of Juglans mandshurica, pericarp, branch skin.Leaf will be plucked after the trees result with the branch skin.
One, the pulverizing of vegetable material
Gather the older leaf on the tree that has born fruit, the pericarp of Chinese olive, withe branch skin, do not dry, add clear water by 1: 1~15 (plant fresh weights: water w/w) smash the back paste mill grinding to pieces by its fresh weight, perhaps that leaf, withe is air-dry, be crushed to behind 40~200 purpose powder standby with beater disintegrating machine again.
Two, lixiviate
The main purpose of this method is to extract the juglone compounds, and extracting method can adopt conventional ethanol refluxing process, also can use conventional CO 2Supercritical extraction.Because final purpose of the present invention is to produce agricultural chemicals, so there is no need the juglone purifying.Below be to be used for simple and easy leach extraction method of the present invention:
1, one of leach extraction method (cold water extraction)
(1) behind the fresh plant material defibrination, uses plate compression.With filter residue add again clear water again defibrination once, and then once through plate compression.Discard filter residue, merge filtrate twice.About 60 ℃, be concentrated into paste or pulpous state with vacuum concentrator.
(2) take by weighing above-mentioned plant drymeal, add clear water soak (acidity of water is pH4.0~pH7.5), amount of water 1: 10~20 (dry powder: water, w/w), use plate compression after 4~12 hours.The flooding that filter cake is used above-mentioned pH is more once used plate compression again.Triplicate.Merge three times filtrate, vacuum concentration is to pulpous state.
2, two of leach extraction method (pure extractions)
Quantitatively take by weighing above-mentioned vegetable material dry powder, after soaking into thoroughly with cold methyl alcohol or ethanol, in the stainless steel lixiviate post of packing into, then with cold methyl alcohol or the slow drip washing of ethanol, juglone content with in the HPLC method detection eluate stops drip washing when this activity substance content is lower than 0.001%.Eluate is concentrated into paste.
3, three of leach extraction method (pure water mixing extractions)
With two of leach extraction method, but alcohol wherein changes the mixture of alcohol (comprising methyl alcohol, ethanol) and water into, and its alcohol/water ratio is 10: 1~100.
Three, mother liquor preparation
Above-mentioned 3 kinds of leach extraction methods are extracted the juglone leaching liquor that contains that obtains be concentrated into after pulpous state or the paste, dissolve slurry repeatedly, get clear liquid, be evaporated to thick again with methyl alcohol.When juglone concentration reaches 0.4% in the concentrate, can be used as composite dose and store with mother liquor.Continue to concentrate about 10 times, sampling Detection is the content of juglone wherein, if the amount of juglone is mother liquor greater than 4%.Add 1% Sodium Benzoate and 3% dimethylbenzene stirs, barrelling, the sealing preservation is used as the mother liquor of agent of juglone list and composite dose of production.
Four, juglone pesticidal preparations production method
1, juglone insecticide list agent:
Single agent prescription (cream preparation)
Juglone 0.3%~4% (cubage by juglone in the mother liquor goes out the mother liquor consumption)
Surfactant (farming breast 100 #, Tx-10, farming breast 0203 etc.) 6%~15%
Bleeding agent (azone, thiophene ketone, soon ooze T or the like) 1%~10%
Preservative 1 (Sodium Benzoate) 0.3%~3%
Preservative 2 (dimethylbenzene) 1%~20%
With solvent make-up to 100%, solvent is optional with technical grade ethanol (anhydrous) or part methyl alcohol.
(annotate: farming breast 100 #Be selected from Xingtai City blue sky chemical industry Co., Ltd product with Tx-10, farming breast 0203 is selected from Zhong Mountain chemical industry Co., Ltd of Jiangsu Jing Pu group product.Down together.)
Complex preparation prescription (1) (cream preparation)
Juglone 0.1%~0.8% (cubage by juglone in the mother liquor goes out the mother liquor consumption)
Avermectin 0.6%~1.8% takes by weighing former medicine (crystal or ointment) and uses dissolve with methanol
Surfactant 8%~15% commercially available Avermectin emulsifier special
Bleeding agent (azone, thiophene ketone, soon ooze T) 1%~20%
Supplementing solvent (dimethylbenzene and small amount of methanol) is to 100%
Complex preparation prescription (2) (cream preparation)
Juglone 0.1%~1% (cubage by juglone in the mother liquor goes out the mother liquor consumption)
Pleocidin 0.8%~4.0% takes by weighing former medicine after by former medicine cubage
Surfactant 10%~15% pleocidin special surfactant
Bleeding agent (azone, thiophene ketone, soon ooze T) 1%~20%
Supplementing solvent (the same) is to 100%
Complex preparation prescription (3) (cream preparation)
Juglone 0.1%~2.0% (cubage by juglone in the mother liquor goes out the mother liquor consumption)
Safety hit 1%~5% (using the commercial preparation)
Surfactant 8~15% (commercially available farming breast 0203)
Bleeding agent (azone, thiophene ketone, soon ooze T) 1%~20%
Supplementing solvent (the same) is to 100%
Complex preparation prescription (4) (cream preparation)
Juglone 0.2%~2.0% (cubage by juglone in the mother liquor goes out the mother liquor consumption)
Beta-cypermethrin 1.0%~4.0%
Surfactant 8%~25% (chrysanthemum ester class emulsifier special, commercially available, farming breast 0203)
Bleeding agent (azone, thiophene ketone, soon ooze T) 1%~20%
Supplementing solvent to 100%
Complex preparation prescription (5) (cream preparation)
Juglone 0.1%~2.0% (cubage by juglone in the mother liquor goes out the mother liquor consumption)
Eliminate 2%~6% (commercially available, the product that the former medicine of import is produced)
Surfactant 6%~20% (with single agent prescription)
Bleeding agent (the same) 1%~20%
Supplementing solvent to 100%
Complex preparation prescription (6) (wetting powder)
Juglone 0.2%~2.0% (going out the mother liquor consumption) by juglone cubage in the mother liquor
Bacillus thuringiensis (B.t) 4000 tire (finally tire, by bacillus thuringiensis former
Powder is tired and is calculated the back adding)
Surfactant 6%~20% (with single agent prescription)
Bleeding agent (the same) 1%~20%
Be supplemented to 100% with lightweight calcium phosphate
Five, the insecticidal effect of juglone list agent
1, the insecticidal activity assay result of juglone
Leaf with Juglans mandshurica passes through conventional alcohol reflux, and the neutral alumina post separates, and preparation thin layer purifying obtains the orange-yellow acicular crystal of juglone, and its purity is 96%.With after the dissolve with methanol, thin up is surveyed its insecticidal activity to the various insects larva with this crystal, finds that juglone has stronger insecticidal activity to diamond-back moth, and aphid is had certain insecticidal activity.But to cotton bollworm, prodenia litura, three-spotted plusia, beet armyworm, cabbage white butterfly insecticidal activity all lower (as shown in table 1).
Table 1, juglone are to the insecticidal test result of several pest
The insect title Worm age Juglone concentration in the sample (μ g/ml) 48 hours corrected mortalities (%)
Prodenia litura beet armyworm bollworm eggplant red spider eggplant thrips vegetable aphid diamondback moth cabbage caterpillar If if 232 one-tenth Cheng Ruocheng 33 100 100 100 15 15 15 7.5 15 5.14 0 26.67 20.83 41.55 70.48 90.0 40.00
2, the diamond-back moth effect extremely of juglone insecticide list agent
Insecticidal activity assay result to the different length of times is as follows:
The indoor determination of activity result of diamond-back moth is killed in table 2, the agent of juglone insecticide list
Worm age 48 hours LC contaminate 50Value (mg/L) 95% confidence interval
Second instar larvae third-instar larvae four-age larva 1.4440 1.2062 3.4683 0.9534~2.1885 0.9645~1.5086 2.2833~5.2682
3, the effect of juglone insecticide field control diamond-back moth
Contain the concentration dispenser of juglone 20 μ g by every ml water, 60 liters of every mu of spray liquid medicine, the insect lethality surpassed 50% in 24 hours, and preventive effect is higher than 70% two days later.About 5 days of lasting period.
The complex preparation of above-mentioned juglone insecticide dilutes 1000 times or 2000 times, and the insect lethality was higher than 90%, lasting period 5-7 days above preventive effect after 70%, three day in 24 hours.
[embodiment]
The preparation of embodiment one, juglone mother liquor (0.4% and 4.0% juglone alcoholic solution)
Get Juglans mandshurica leaf, pericarp, branch skin dry powder (40-60 order) 600kg, add water 3000L, soak, adjusting pH is 5.0, spends the night, and puts into stainless steel column, soaks 8 hours, uses the ethanol drip washing of pH5.0 then lentamente.Being washed till in the leacheate juglone concentration≤0.001% o'clock stops.Receive leacheate (ethanol of juglone and the aqueous solution) 4500L.In vacuum concentration pan, eluent solution is concentrated into paste.Take out paste, dissolve repeatedly with methyl alcohol in dissolving tank, the solution filter and remove residue stays clear liquid, and clear liquid concentrates again, obtains concentrate 50kg, mother liquor (juglone content 0.398%).Concentrate again, become 4.0% mother liquor.
The preparation of embodiment two, the agent of juglone insecticide pesticide list (0.3% juglone cream preparation)
Get 0.4% mother liquor 40kg, add Tx-10 3kg, newborn 0203 2kg of farming, fast penetrant t 4kg, the abundant stirring and evenly mixing of Sodium Benzoate 0.8kg adds dimethylbenzene 1000ml at last, fully mixes once more.Obtain the about 49kg of juglone insecticide list agent emulsifiable solution at last.The content of juglone is 0.30% in the testing product.This kind trial product is diluted 500 times respectively, and 300 times, control field diamond-back moth, control efficiency was respectively 80% and 97% in 72 hours.
The preparation of embodiment three, 2.0% Ah 's missible oil (0.2% juglone+1.8% Avermectin)
Get Avermectin crystal 1.8kg (calculating), use the 25L dissolve with methanol, add and state 52.6 liters in 0.4% juglone mother liquor, stir evenly by Avermectin B1a component folding hundred.Add 12 liters of Avermectin emulsifier specials, 2 kilograms of thiophene ketone.Complement to 100 kilograms with dimethylbenzene at last, stir.2000 times, 3000 times of this product dilutions, control field diamond-back moth, control efficiency was respectively 92% and 84% in 72 hours.
Embodiment four, the 3.0% high preparation of missible oil (0.2% juglone+2.8% beta-cypermethrin) recklessly
Get 10.5 kilograms of the benzene oil of beta-cypermethrin 27%, add 20 liters of methyl alcohol, 12 liters of cypermethrin emulsifier specials, 3 kilograms of azones stir, and add 52.6 liters in juglone mother liquor again, complement to 100 kilograms with dimethylbenzene, stir.1500 times, 2000 times of this product dilutions, control field diamond-back moth, control efficiency was respectively about 95%, 85% in 72 hours.
The preparation of wetting powder (0.8% juglone+2.0% bacillus thuringiensis delta-endotoxin) recklessly of embodiment five, 2.8% gold medal
(the various auxiliary agents in this pulvis have been included in wherein to get the bacillus thuringiensis delta-endotoxin wetting powder of 16000IU, delta-endotoxin content 2.0%) the juglone mother liquor 25kg of 100kg absorption high-load (content 4%), air-dry, airslide disintegrating mill is crushed to 325 orders, gets product 105kg.
Control field diamond-back moth after this product dilutes 1000 times, preventive effect 90%~100% in 72 hours.
Embodiment six, 7.0% preparation that removes missible oil (1% juglone+6% capillary) recklessly
Get the former medicine 6kg of capillary (pure calculating) and add methyl alcohol 30L dissolving, add 0,203 7 kilogram, 8 kilograms of husky breasts stir, and add 4% juglone mother liquor 25kg again, azone 1.5kg, and fast penetrant t 10kg complements to 100kg with dimethylbenzene, fully stirs evenly once more.2000 times, 3000 times of product dilutions are to diamond-back moth field efficacy 95% and 100%.
Embodiment seven, 10.2% pacifies the preparation of missible oil (10% safety hit+0.2% juglone) recklessly
Get 30% safety hit 10kg and add 4% mother liquor 1.5kg, add farming breast 100 #3kg, dimethylbenzene 2kg, abundant mixing, altogether product 30kg.
1500 times, 2000 times of product dilutions, control field diamond-back moth preventive effect is more than 90%.
The preparation of embodiment eight, the many missible oil of 4.6% quinone (0.4% juglone+4.2% pleocidin)
Get the former medicine 2.1kg of pleocidin (pure, component A+D), with ethanol 15L dissolving, add Tx-10 5L, fast penetrant t 5L fully mixes, and gets content again and be 4% juglone mother liquor 5kg, complements to 50kg with dimethylbenzene.
1500 times, 2000 times of product dilutions, 72 hours effects of control diamond-back moth are up to 95% and 100%.
Embodiment nine, 2.4% preparation of Ah's granule (2.0% A Wei+0.4% juglone) recklessly
Get Avermectin 2kg (by the pure calculating of Avermectin B1a), use the 20L dissolve with methanol, add calcium dodecyl benzene sulfonate 6kg, Avermectin emulsifier special 6kg, 4% juglone mother liquor 10kg, fully mixing.Increase again and ooze T 10kg, fully mixing.With 60 kilograms of (NH 4) 2SO 4Crystallization is a carrier, and the rotary granulator of packing into is sprayed onto the solution of above-mentioned active substance on the carrier, rotates granulation while spraying.Sprayed after the above-mentioned active constituent, sprayed talcum powder (about 14 kilograms) again, granule coating is given in the spray while rotating.Drying room drying (40 ℃ of air-drying with warm wind, about 5 hours of time).Being packaged into pouch dispatches from the factory.
1000 times of controls of product dilution field diamond-back moth, preventive effect was 100% in 72 hours.
Embodiment ten, product of the present invention and biological and chemical kill the diamond-back moth pesticide efficacy relatively
With 0.3% juglone missible oil list agent of the embodiment of the invention two productions, the 2.4% Hu Ah granule that the 3.0% high missible oil recklessly that embodiment four produces, embodiment nine are produced has carried out the test of pesticide effectiveness of control diamond-back moth at suburb, Tonghai County, Yunnan Province vegetable field.Being blank with the clear water in the test, is the biopesticide contrast with the B.t wetting powder of 16000IU/mg, and 1.8% abamectin emulsifiable concentrate is the chemical pesticide contrast.Because the regional diamond-back moth of test shows the high resistance property of medicine to existing agricultural chemicals, so conventional B.t and Avermectin preparation as insecticiding effect are relatively poor, and significantly be better than above-mentioned two kinds of conventional dose (the results are shown in Table 3) with the diamond-back moth preparation effect of killing of walnut extract production.Test shows that product control diamond-back moth effect of the present invention is sure, and is a kind of effective weapon of subduing the resistance diamond-back moth.
Several Related product control of table 3 diamond-back moth field control effect relatively
The pesticidal preparations title Extension rate 48 hours control efficiency (%) behind the medicine 72 hours control efficiency (%) behind the medicine
0.3% juglone missible oil 600 79.3 93.8
3.0% high missible oil recklessly 1000 92.5 100
2.4% Hu Ah granule 1000 81.4 100
16000IU/mg 500 24.7 42.0
The B.t wetting powder
1.8% abamectin emulsifiable concentrate 1000 42.1 59.4
The clear water contrast - 0 0
Annotate: the amount of liquid medicine that every mu of ground sprays after the dilution is 60 kilograms.
Embodiment 11, utilize walnut tree to produce the juglone mother liquor
After the walnut tree result, gather its leaf, withe and pericarp be 500Kg altogether, adds 3 times of (w/w) water and takes advantage of fresh grinding pulping, uses plate compression, collects to obtain 1400Kg filtrate.95% ethanol (400Kg) of weight such as 400 kilograms of filter residues add soaked 24 hours, and plate compression is collected to such an extent that pure water mixes filtrate 400Kg once more.For the second time filter residue reclaim through double-cone dryer ethanol (55 ℃, vacuum-0.09MPa) afterwards as fertilizer.Merge twice filtrate (aqueous solution and ethanolic solution) 1800Kg altogether, with vacuum scraper plate inspissator filtrate is condensed into pulpous state, get slurry 220Kg at 60 ℃~65 ℃.Dissolve the pulpous state extract repeatedly with methyl alcohol, get the supernatant concentrating under reduced pressure (50 ℃~55 ℃ ,-0.09MPa) to thick juglone mother liquor.This embodiment obtains mother liquor 35Kg, and wherein juglone concentration 0.51%.
Embodiment 12, utilize black walnut tree to produce the juglone mother liquor
Production method is identical with embodiment 11 with operating process, but choice of tree species is the black walnut tree.Produce mother liquor 28Kg with the 500Kg plant tissue, wherein juglone concentration is 0.48%.

Claims (7)

1, a kind of purposes of walnut extract is characterized in that the walnut extract is prepared into the insecticide pesticide that is used to prevent and treat diamond-back moth.
2, purposes as claimed in claim 1 is characterized in that wherein said walnut extract prepares by the following method: treat after the walnut result, pluck its leaf, pericarp and branch skin.By plant fresh weight add clear water 1: 1~15 weight ratio, in the vegetable material of plucking, add clear water then, smash the back paste mill grinding to pieces, perhaps that leaf, withe is air-dry, be crushed to 40~200 purpose powder with beater disintegrating machine again.With cold water, methyl alcohol or the ethanol repeatedly extracting of above-mentioned powder with pH4.0~pH7.5, extract is paste or pulpous state through vacuum concentration at last.
3, purposes as claimed in claim 1 is characterized in that wherein said walnut comprises seeds and mutation such as English walnut, black walnut, Juglans mandshurica.
4,, it is characterized in that the main active insecticidal components in the wherein said walnut extract is a juglone as the arbitrary described purposes of claim 1-4.
5,, it is characterized in that wherein said walnut extract is made the juglone insecticide pesticide list agent that is used to prevent and treat diamond-back moth as the arbitrary described purposes of claim 1 to 4.
6, as the arbitrary described purposes of claim 1 to 4, it is characterized in that wherein said walnut extract and other agricultural insecticide are mixed, make the compound insecticidal agricultural chemicals that is used to prevent and treat diamond-back moth.
7, purposes as claimed in claim 6 is characterized in that wherein said other agricultural insecticide comprises: Avermectins, and the pleocidin class, the natural pyrethrin class, pyrethroid, the bacillus thuringiensis class eliminates, sharp strength spy, safety hit.
CNB2004100099653A 2004-12-03 2004-12-03 Use of walnut plant extract as pesticide in preventing and controlling diamondback moth Expired - Fee Related CN1314327C (en)

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CN101416644B (en) * 2008-01-21 2010-05-12 北京农学院 Walnut peel extract and new use thereof
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CN101416644B (en) * 2008-01-21 2010-05-12 北京农学院 Walnut peel extract and new use thereof
CN101274867B (en) * 2008-05-19 2011-03-23 中国农业大学 Anti-root-maggot medicinal organic fertilizer and fertilizing method thereof
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CN102577727A (en) * 2012-03-26 2012-07-18 王福 Methods for applying walnut green peel and leaf products to rice
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CN109042753A (en) * 2018-09-25 2018-12-21 河南科技大学 A kind of long-acting slow-release plant source compound Herbicidal combinations and preparation method thereof
CN115209732A (en) * 2019-11-15 2022-10-18 维氏化学有限责任公司 Agent for controlling plant diseases and special use thereof in treatment of plants infected with xylem-fastidious bacteria
JP2023507069A (en) * 2019-11-15 2023-02-21 ベクスタケム ソシエタ ア レスポンサビリタ リミタータ Phytosanitary agents and specific uses thereof in the treatment of plants infected with Pierce's fungus
JP7462042B2 (en) 2019-11-15 2024-04-04 ベクスタケム ソシエタ ア レスポンサビリタ リミタータ Phytosanitary agents and their specific use in the treatment of plants infected with Pierce's disease fungus - Patents.com
WO2024081610A1 (en) * 2022-10-13 2024-04-18 Ag Nutrients, LLC Compositions, systems, and methods for increased plant quality

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