CN111713514A - Medicament for citrus canker and preparation method thereof - Google Patents
Medicament for citrus canker and preparation method thereof Download PDFInfo
- Publication number
- CN111713514A CN111713514A CN202010645479.XA CN202010645479A CN111713514A CN 111713514 A CN111713514 A CN 111713514A CN 202010645479 A CN202010645479 A CN 202010645479A CN 111713514 A CN111713514 A CN 111713514A
- Authority
- CN
- China
- Prior art keywords
- medicament
- agent
- citrus canker
- parts
- copper
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003814 drug Substances 0.000 title claims abstract description 66
- 235000020971 citrus fruits Nutrition 0.000 title claims abstract description 45
- 241000207199 Citrus Species 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 241000196324 Embryophyta Species 0.000 claims abstract description 25
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 19
- 239000000341 volatile oil Substances 0.000 claims description 39
- 229910052802 copper Inorganic materials 0.000 claims description 23
- 239000010949 copper Substances 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- 239000002270 dispersing agent Substances 0.000 claims description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- 239000003995 emulsifying agent Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 238000000926 separation method Methods 0.000 claims description 16
- -1 Saisentong Chemical compound 0.000 claims description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 15
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 13
- 239000000284 extract Substances 0.000 claims description 12
- 239000000945 filler Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000605 extraction Methods 0.000 claims description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002518 antifoaming agent Substances 0.000 claims description 9
- 239000003899 bactericide agent Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
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- 239000002562 thickening agent Substances 0.000 claims description 8
- 230000002528 anti-freeze Effects 0.000 claims description 6
- MMUFAGXJPKNAHT-UHFFFAOYSA-N copper;quinolin-8-ol Chemical compound [Cu].C1=CN=C2C(O)=CC=CC2=C1 MMUFAGXJPKNAHT-UHFFFAOYSA-N 0.000 claims description 6
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- BCYMZMFCJMHEBD-JHZYRPMRSA-L copper;(1r,4ar,4br,10ar)-1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylate Chemical compound [Cu+2].C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C([O-])=O.C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C([O-])=O BCYMZMFCJMHEBD-JHZYRPMRSA-L 0.000 description 1
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- 210000003608 fece Anatomy 0.000 description 1
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- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
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Classifications
-
- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- 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
- 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
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
-
- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives thereof
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
- A01N43/42—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, 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
- A01N43/82—Biocides, 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
-
- 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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- 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
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- A01N65/08—Magnoliopsida [dicotyledons]
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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
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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Abstract
The invention provides a medicament for citrus canker and a preparation method thereof, which are characterized in that a plant-derived active antibacterial component is taken as a main component, and the traditional chemical medicament with high-efficiency bactericidal activity is matched to prepare a compound medicament, so that the effect of efficiently treating the citrus canker is realized.
Description
Technical Field
The invention belongs to the technical field of fruit tree pest control, and relates to a medicament for citrus canker and a preparation method thereof.
Background
China is a world large orange producing country, the orange industry is the agricultural support industry of China, plays an extremely important role in agricultural economy, and plays an extremely important role in promoting the income increase of farmers, increasing social employment and building new socialist rural areas. Citrus canker is a significant obstacle to the development of the citrus industry.
The citrus canker is a bacterial disease caused by Xanthomonas anoxopodispv.Citri belonging to Xanthomonas of the phylum of thin-walled bacterium, and the citrus canker can infect various Rutaceae plants, and is most susceptible to common sweet oranges, navel oranges, sour oranges and other varieties. The germs can be transmitted along with splashed raindrops and high-speed wind, and penetrate through skin holes, stomata and wounds to invade plants, so that leaves, fruits and stem parts are in crater scabs, and immature fruits are cracked, deformed, dropped and fallen leaves are caused. The citrus fruit disease is a very serious infectious disease, has long prevalence duration, wide disease incidence range and high disease incidence rate, causes short service life, low yield and high production cost of citrus fruit in most areas of China, and has serious troubles and restricts the development of citrus fruit industry in China and even in the world.
Aiming at the prevention and treatment of citrus canker, experts at home and abroad agree that the comprehensive treatment technology combining agricultural prevention and treatment and chemical prevention is the key for solving the citrus canker. At present, the medicines for preventing and treating the citrus canker pathogen mainly take copper preparation single agents and compound preparations as main materials, such as copper hydroxide, copper oxychloride, kasugao copper oxychloride, copper oxychloride-zineb, copper calcium sulfate, basic copper sulfate, kasugao quinoline copper, Zhongsheng copper acetate, copper abietate, cuaminosulfate and the like. However, the copper preparation has certain limitations such as poor crop safety, poor compatibility or serious drug resistance.
The long-term use of chemical pesticides not only increases the drug resistance of pathogenic bacteria and causes environmental pollution, but also often causes food safety problems, so that the selection of biogenic pesticides for controlling diseases is a hotspot in current research. In addition, the pesticide prepared by combining the effective components of different pesticides is an effective and quick way for developing and researching new pesticides and preventing and controlling resistant germs in agriculture at present. Pesticides of different species, when mixed, typically exhibit three types of action: additive action, synergistic action and antagonistic action. The compound synergistic formula is good, can obviously improve the actual prevention and treatment effect, and reduces the using amount of pesticide, thereby greatly delaying the generation speed of drug resistance of germs, and being an important means for comprehensively preventing and treating diseases.
Therefore, the development of drugs or compound combinations with high biological activity to citrus canker pathogens is urgent, and a medicament which can effectively improve the prevention and treatment effect and does not have adverse effects on the surrounding environment and human bodies is urgently needed.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a medicament for citrus canker and a preparation method thereof, which are characterized in that a plant-derived active antibacterial component is taken as a main component, and the conventional chemical medicament with high-efficiency bactericidal activity is matched to prepare a composite medicament, so that the effect of efficiently treating the citrus canker is realized.
In order to achieve the purpose, the invention adopts the following technical scheme that the medicament for the citrus canker consists of the following components in parts by weight: 10-15 parts of organic copper bactericide, 4-8 parts of nano silver sol and 5-10 parts of plant volatile oil.
The organic copper bactericide is selected from one or more of copper acetate, Saisentong, oxine-copper and thiediazole-copper;
the content of silver ions in the nano silver sol is 3000-5000ppm, and the particle size of the silver ions is 5-30 nm.
The plant volatile oil is selected from one or more of radix Asteris, cortex Cinnamomi, herba Schizonepetae, and fructus forsythiae, and is prepared by supercritical CO extraction2The preparation method comprises the following steps:
(1) selecting dried plant, pulverizing, sieving with 30-40 mesh sieve, placing into extraction kettle, and extracting with supercritical CO2Extracting the materials by extraction equipment, adding an entrainer in the extraction process, separating by using a first-stage separation kettle and a second-stage separation kettle, and collecting and combining extracts separated from the first-stage separation kettle and the second-stage separation kettle;
(2) adding 25-50 wt% of polyethylene glycol 300 and 25-50 wt% of monoglyceride into the extract obtained in the step (1), uniformly stirring, concentrating under reduced pressure in vacuum, drying to obtain a dry extract, and uniformly mixing the dry extract, 50-100 wt% of beta-cyclodextrin and 5-10 times of maltodextrin to obtain the plant volatile oil.
The entrainer is selected from one or more of ethanol, ethyl acetate and petroleum ether; the amount of the entrainer is 30-100% of the total feeding weight of the plant powder;
the pressure of the extraction kettle in the step (1): 25-32 MPa, temperature: 40-55 ℃; the pressure of the first-stage separation kettle is as follows: 7-9 MPa, temperature: 40-45 ℃; the pressure of the secondary separation kettle is as follows: 5-7 MPa, temperature: 30 to 38 ℃.
Further, the medicament for the citrus canker contains one or more than two of solvent, emulsifier, dispersant, wetting agent, thickener, antifreeze, disintegrant, defoamer, filler and binder;
the solvent is one or more than two of water, ethanol, glycerol, isopropanol and acetone;
the emulsifier is selected from one or more of alkylphenol polyoxyethylene ether, benzyl phenol polyoxyethylene ether, phenethyl phenol polyoxyethylene ether, castor oil polyoxyethylene ether, phenethyl phenol polyoxyethylene polyoxypropylene ether and the like;
the dispersant is one or more than two selected from polycarboxylate, lignosulfonate, alkylphenol polyoxyethylene pyrimidine formaldehyde condensate sulfate, alkylbenzene sulfonic acid calcium salt, naphthalene sulfonic acid formaldehyde condensate sodium salt, alkylphenol polyoxyethylene pyrimidine, fatty amine polyoxyethylene pyrimidine and fatty acid polyoxyethylene ester;
the wetting agent is selected from one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, nekal BX, wetting penetrant F, fructus Gleditsiae Abnormalis powder, faeces Bombycis, and fructus Sapindi Mukouossi powder;
the thickening agent is selected from one or more than two of xanthan gum, polyvinyl alcohol and polyethylene glycol;
the antifreezing agent is one or more than two of ethylene glycol, propylene glycol, glycerol and polyethylene glycol;
the disintegrating agent is one or more than two of bentonite, urea, ammonium sulfate and aluminum chloride;
the defoaming agent is one or more than two of silicone oil, silicone compounds, C10-20 saturated fatty acid compounds and C8-10 fatty alcohol compounds;
the filler is selected from one or more than two of kaolin, diatomite, bentonite, attapulgite, white carbon black, starch and light calcium carbonate;
the binder is selected from one or more of acacia, white dextrin, methylcellulose, sodium acrylate, polyvinylpyrrolidone, crosslinked polyvinylpyrrolidone, polyethylene glycol, and polyvinyl alcohol.
The invention also aims to provide a preparation method of the medicament for citrus canker, and the medicament can be prepared into any one dosage form suitable for agriculture by using a known method, such as water dispersible granules, suspending agents and wettable powder, wherein the mass percentage of the medicament in the preparation is 50-70%.
When the medicament for the citrus canker is a water dispersing agent, the medicament is 50-70%, the emulsifier is 2-4%, the dispersing agent is 4-6%, the disintegrating agent is 2-5%, the binder is 5-10%, the thickening agent is 2-6%, the defoaming agent is 1-3%, the antifreezing agent is 2-4%, and the rest is filler, and the components are uniformly mixed according to the proportion, crushed, granulated and dried.
When the medicament for the citrus canker is a suspending agent, the medicament is 50-70%, the emulsifier is 2-4%, the dispersant is 4-6%, the defoamer is 1-3%, the antifreeze is 2-4%, and the balance is water. The components are mixed evenly according to the proportion.
When the medicament for citrus canker is wettable powder, 50-70% of the medicament, 2-4% of an emulsifier, 4-6% of a dispersant, 2-4% of an antifreeze and the balance of a filler are uniformly mixed according to the proportion, crushed, granulated and dried.
The invention also aims to provide an application of the medicament in preventing and treating citrus canker, wherein the medicament consists of the following components in parts by weight: 10-15 parts of organic copper bactericide, 4-8 parts of nano silver sol and 5-10 parts of plant volatile oil.
The invention has the following beneficial effects:
(1) the invention takes the organic copper bactericide, the nano silver sol and the plant volatile oil as raw materials to prepare the medicament composition, makes full use of the synergistic interaction among the organic copper bactericide, the nano silver sol and the plant volatile oil, enlarges the sterilization spectrum, improves the sterilization capability, and overcomes and delays the generation of drug resistance of pathogenic bacteria. The dosage is reduced, the good sterilization effect is ensured, and the influence degree on the environment is reduced while the medication cost of farmers is reduced.
(2) According to the invention, the plant volatile oil is specially modified, so that the water solubility of the plant volatile oil is improved, the plant volatile oil is easier to be fully mixed with an organic copper bactericide and a nano silver sol, and the antibacterial effect of the plant volatile oil is greatly improved;
(3) the drug provided by the invention can well prevent and treat citrus canker, has the advantages of low cost, wide raw material source, environmental protection, no toxicity, no residue and the like, is easy to realize industrial production, and has wide market value.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the present invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the present invention and is not intended to limit the scope of the claims which follow. All of the starting materials of the present invention, without particular limitation as to their source, may be purchased commercially or prepared according to conventional methods well known to those skilled in the art.
1. Preparing the plant volatile oil, comprising the following steps:
(1) selecting dried radix asteris, cinnamon, schizonepeta and fructus forsythiae, respectively crushing, sieving with a 30-40-mesh sieve, putting into an extraction kettle, extracting materials by using supercritical CO2 extraction equipment, adding an entrainer in the extraction process, separating by using a first-stage separation kettle and a second-stage separation kettle, collecting and combining extracts separated from the first-stage separation kettle and the second-stage separation kettle;
pressure of the extraction kettle: 25-32 MPa, temperature: 40-55 ℃; the pressure of the first-stage separation kettle is as follows: 7-9 MPa, temperature: 40-45 ℃; the pressure of the secondary separation kettle is as follows: 5-7 MPa, temperature: 30-38 ℃;
the entrainer is selected from one or more of ethanol, ethyl acetate and petroleum ether; the amount of the entrainer is 30-100% of the total feeding weight of the plant powder;
(2) adding 25-50 wt% of polyethylene glycol 300 and 25-50 wt% of monoglyceride into the extract obtained in the step (1), uniformly stirring, concentrating under reduced pressure in vacuum, drying to obtain a dry extract, and uniformly mixing the dry extract, 50-100 wt% of beta-cyclodextrin and 5-10 times of maltodextrin to obtain plant volatile oil; respectively marked as aster volatile oil, cinnamon volatile oil, schizonepeta volatile oil and forsythia volatile oil.
2. Indoor activity test
Reference is made to the agricultural industry Standard NY/T1156.16-2008, turbidity method.
The citrus canker pathogen was streaked on top of LB solid medium and cultured at 28 ℃ until colonies were grown. Picking single colony of citrus canker pathogenic bacteria on LB solid culture medium, placing in liquid LB culture medium, shaking and culturing at 28 deg.C and 200rpm constant temperature shaking table to OD value of about 0.5, and reserving. The calculation method of the sterilization rate comprises the following steps: colony kill rate/% (number of control colonies-number of treated colonies)/number of control colonies x 100.
2.1 selecting the organic copper bactericide and the plant volatile oil with the weight ratio of 1:1 to prepare the medicament, preparing 50% of aqueous dispersion to test indoor bactericidal activity, and the results are shown in table 1:
TABLE 1
| Aster volatile oil | Cinnamon essential oil | Schizonepeta volatile oil | Fructus forsythiae volatile oil | |
| Cupric acetate | 88 | 92 | 85 | 84 |
| Thisen copper | 90 | 84 | 93 | 85 |
| Quinolinic copper | 92 | 94 | 89 | 93 |
| Thiodiazole copper | 94 | 90 | 84 | 90 |
As can be seen from the results in table 1, the combination of cinnamon volatile oil with copper acetate and oxine-copper, the combination of thiassen-copper with schizonepeta volatile oil, and the combination of thiabendazole-copper with aster volatile oil have higher bactericidal activity.
2.2 selecting the above combination to prepare medicaments with different proportions, selecting 60 parts of medicament, 2 parts of emulsifier, 4 parts of dispersant, 1 part of defoamer, 2 parts of antifreeze and the balance of water to prepare water dispersion with the mass fraction of 60 percent to test the indoor bactericidal activity, taking 30 percent by mass of copper acetate as a comparison example, and finding the results in table 2:
TABLE 2
As can be seen from the data in Table 2, the medicament prepared by the invention has obviously improved bactericidal activity compared with the commercial cupric acetate, and the three substances have synergistic bactericidal activity.
3. Field test
According to a field efficacy test design method, a random block method is adopted, the design is repeated for 3 times per treatment, and 3 plants of test trees are tested in each cell; spraying the first medicine at 14d after flower withering, and spraying the second medicine at intervals of 7 days for 2, 3, and 4 times. The pesticide is sprayed by a hand-operated knapsack compressed sprayer, so that no rain is produced 24 hours after each pesticide application, and timely supplement application is required if rain falls. Uniformly spraying 10kg of liquid medicine to the leaves and fruits till the liquid medicine is dripped. Before drug application, 3 trees are selected at fixed points in each cell, tender tips of each tree are marked in 4 directions, the disease condition of the citrus canker is investigated, the number of disease spots on 100 leaves and 50 fruits is investigated totally, grading is carried out, and the disease index is calculated. And 7d and 14d after the last application, respectively investigating the disease conditions of 100 leaves and 50 fruits marked on the tender tips, grading the diseased leaves (or fruits), and calculating the disease incidence, disease index and prevention effect.
Grading the disease condition: the disease grading standard is as follows by taking leaves (or fruits) as a unit: grade 0, no scab; grade 1, 1-5 scabs exist on each leaf (or fruit); grade 3, 6-10 lesions are formed on each leaf (or fruit); grade 5, 11-15 scabs exist on each leaf (or fruit); grade 7, each leaf (or fruit) has 16-20 scabs; grade 9, more than 21 scabs exist on each leaf (or fruit).
Example 1
Weighing 11 parts of Saisentong, 7 parts of schizonepeta volatile oil and 6 parts of nano silver sol, uniformly mixing to obtain a medicament, then weighing 50% of the medicament, 4% of an emulsifier, 6% of a dispersant, 3% of a disintegrant, 5% of a binder, 2% of a thickener, 1% of a defoaming agent, 2% of an antifreezing agent and the balance of a filler according to the following weight percentage, uniformly mixing the components according to the proportion, crushing, granulating, and drying to obtain the water dispersible granule.
Example 2
Weighing 13 parts of thiediazole copper, 6 parts of aster volatile oil and 5 parts of nano silver sol, uniformly mixing to obtain a medicament, then weighing 70% of the medicament, 2% of an emulsifier, 6% of a dispersant, 5% of a disintegrant, 8% of a binder, 2% of a thickener, 3% of a defoaming agent, 2% of an antifreezing agent and the balance of a filler according to the following weight percentage, uniformly mixing the components according to a ratio, crushing, granulating, and drying to obtain the water dispersible granule.
Example 3
Weighing 5 parts of copper acetate, 8 parts of oxine-copper, 5 parts of cinnamon volatile oil and 8 parts of nano silver sol, uniformly mixing to obtain a medicament, then weighing 60% of the medicament, 2% of an emulsifier, 4% of a dispersant, 2% of a disintegrant, 5% of a binder, 6% of a thickener, 1% of a defoaming agent, 2% of an antifreezing agent and the balance of a filler according to the following weight percentage, uniformly mixing the components according to the proportion, crushing, granulating, and drying to obtain the water dispersible granule.
Example 4
Weighing 5 parts of Saisentong, 7 parts of thiediazole copper, 6 parts of nano silver sol, 3 parts of Aster volatile oil and 5 parts of fructus forsythiae volatile oil, uniformly mixing to obtain a medicament, then weighing 50% of the medicament, 4% of an emulsifier, 6% of a dispersant, 1% of an antifoaming agent, 2% of an antifreezing agent and the balance of water according to the following weight percentage, and uniformly mixing the components in proportion to obtain the suspending agent.
Example 5
Weighing 6 parts of copper acetate, 8 parts of oxine-copper, 8 parts of nano silver sol, 4 parts of cinnamon volatile oil and 5 parts of fructus forsythiae volatile oil, uniformly mixing to obtain a medicament, then weighing 60% of the medicament, 3% of an emulsifier, 5% of a dispersant, 1% of a defoaming agent, 3% of an antifreezing agent and the balance of water according to the following weight percentage, and uniformly mixing the components in proportion to obtain the suspending agent.
Example 6
Weighing 7 parts of oxine-copper, 5 parts of thiediazole-copper, 6 parts of nano silver sol, 7 parts of cinnamon volatile oil and 3 parts of fructus forsythiae volatile oil, uniformly mixing to obtain a medicament, then weighing 70% of the medicament, 2% of an emulsifier, 4% of a dispersant, 2% of an anti-freezing agent and the balance of a filler according to the following weight percentage, uniformly mixing the components according to the proportion, crushing, granulating and drying to obtain the wettable powder.
Example 7
Weighing 12 parts of thiediazole copper, 6 parts of nano silver sol, 7 parts of cinnamon volatile oil and 3 parts of schizonepeta volatile oil, uniformly mixing to obtain a medicament, then weighing 60% of the medicament, 2% of an emulsifier, 4% of a dispersant, 2% of an anti-freezing agent and the balance of a filler according to the following weight percentage, uniformly mixing the components according to the ratio, crushing, granulating and drying to obtain the wettable powder.
Table 3 test of field control of Citrus canker by copper acetate of examples 1-7 and 30%
TABLE 3
| Numbering | Dilution factor | 7d control effect (%) | 14d control effect (%) |
| Example 1 | 4000 times of | 95.6 | 94.3 |
| Example 2 | 4000 times of | 95.3 | 94.8 |
| Example 3 | 4000 times of | 96.3 | 95.6 |
| Example 4 | 4000 times of | 94.2 | 93.6 |
| Example 5 | 4000 times of | 93.4 | 92.6 |
| Example 6 | 4000 times of | 94.8 | 93.4 |
| Example 7 | 4000 times of | 91.5 | 90.8 |
| 30% of copper acetate | 4000 times of | 49.3 | 47.6 |
As can be seen from the experimental data in Table 3, the medicament prepared by the invention has good effect of preventing and treating citrus canker and long-term preventing and treating effect.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A medicament for citrus canker, characterized in that: the composition comprises the following components in parts by weight: 10-15 parts of organic copper bactericide, 4-8 parts of nano silver sol and 5-10 parts of plant volatile oil.
2. A medicament for citrus canker as claimed in claim 1, wherein: the organic copper bactericide is selected from one or more than two of copper acetate, Saisentong, oxine-copper and thiediazole-copper; the content of silver ions in the nano silver sol is 3000-5000ppm, and the particle size of the silver ions is 5-30 nm; the plant volatile oil is selected from one or more of radix Asteris, cortex Cinnamomi, herba Schizonepetae, and fructus forsythiae.
3. A medicament for citrus canker as claimed in claim 2, wherein: the volatile oil is obtained by supercritical CO2The preparation method comprises the following steps:
(1) selecting dried plant, pulverizing, sieving with 30-40 mesh sieve, placing into extraction kettle, and extracting with supercritical CO2Extracting the materials by extraction equipment, adding an entrainer in the extraction process, separating by using a first-stage separation kettle and a second-stage separation kettle, and collecting and combining extracts separated from the first-stage separation kettle and the second-stage separation kettle;
(2) adding 25-50 wt% of polyethylene glycol 300 and 25-50 wt% of monoglyceride into the extract obtained in the step (1), uniformly stirring, concentrating under reduced pressure in vacuum, drying to obtain a dry extract, and uniformly mixing the dry extract, 50-100 wt% of beta-cyclodextrin and 5-10 times of maltodextrin to obtain the plant volatile oil.
4. A medicament for citrus canker as claimed in claim 3, wherein: the entrainer is selected from one or more of ethanol, ethyl acetate and petroleum ether; the dosage of the entrainer is 30-100% of the total feeding weight of the plant powder.
5. A medicament for citrus canker as claimed in claim 1, wherein: the medicament for the citrus canker contains one or more than two of solvent, emulsifier, dispersant, wetting agent, thickener, antifreeze, disintegrant, defoamer, filler and binder.
6. The agent for citrus canker according to any one of claims 1 to 5, characterized in that: the dosage form of the medicament is selected from one of water dispersible granules, suspending agents and wettable powder, and the mass percentage of the medicament in the preparation is 50-70%.
7. The agent for citrus canker according to claim 6, characterized in that: when the medicament for the citrus canker is an aqueous dispersing agent, 50-70% of the medicament, 2-4% of an emulsifier, 4-6% of a dispersing agent, 2-5% of a disintegrating agent, 5-10% of a binder, 2-6% of a thickening agent, 1-3% of a defoaming agent, 2-4% of an antifreezing agent and the balance of a filler are uniformly mixed according to a ratio, crushed, granulated and dried.
8. The agent for citrus canker according to claim 6, characterized in that: when the medicament for the citrus canker is a suspending agent, 50-70% of the medicament, 2-4% of an emulsifier, 4-6% of a dispersant, 1-3% of an antifoaming agent, 2-4% of an antifreezing agent and the balance of water. The components are mixed evenly according to the proportion.
9. The agent for citrus canker according to claim 6, characterized in that: when the medicament for the citrus canker is wettable powder, 50-70% of the medicament, 2-4% of an emulsifier, 4-6% of a dispersant, 2-4% of an antifreeze and the balance of a filler are uniformly mixed according to a ratio, crushed, granulated and dried.
10. Use of the agent of any one of claims 1-9 for the control of citrus canker.
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| CN110367019A (en) * | 2019-08-02 | 2019-10-25 | 中国农业科学院柑桔研究所 | A kind of antidote of citrus borism |
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| CN111109294A (en) * | 2020-01-16 | 2020-05-08 | 陕西麦可罗生物科技有限公司 | Nano-silver water dispersible granule and preparation method and application thereof |
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Application publication date: 20200929 |