CN103004859A - Preparation method and application of sustained-release nanoparticle preparation for preventing and treating grape ulcer - Google Patents
Preparation method and application of sustained-release nanoparticle preparation for preventing and treating grape ulcer Download PDFInfo
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- CN103004859A CN103004859A CN2011102876613A CN201110287661A CN103004859A CN 103004859 A CN103004859 A CN 103004859A CN 2011102876613 A CN2011102876613 A CN 2011102876613A CN 201110287661 A CN201110287661 A CN 201110287661A CN 103004859 A CN103004859 A CN 103004859A
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Abstract
The invention relates to a preparation method and application of a sustained-release nanoparticle preparation for preventing and treating grape ulcer, belonging to the technical field of pesticides.
Description
Technical field
The present invention relates to a kind of preparation and application thereof that prevents and treats the sustained-release nano microsphere preparations of grape canker, belong to technical field of pesticide.
Technical background
The grape canker is by the fungus-caused disease of Botryosphaeria (Botryosphaeria spp.), and this disease is the important grape disease that worldwide exists of discovered in recent years.Mainly cause harm grape newly slightly, fruit ear, limb, cause newly slightly withered or can not be ripe, withered top, mashed fringe, ulceration appears in limb, the xylem brown stain causes tree vigo(u)r weak, fruit abscission; Directly cause plant dead when disease is serious, affect vintage and quality.
At present, the method for preventing and treating of grape canker mainly comprises cultural control and chemical control, and cultural control comprises control output, and branch is pruned the methods such as post processing wound; The medicament of chemical control grape canker mainly is Flusilazole and fludioxonil, but because medicament is to grape limb poor permeability, medicament is only effective to the pathogen of limb epidermis, and is invalid to the pathogen that is deep into xylem, thereby causes the problem of the difficult radical cure of grape canker.
Summary of the invention
The objective of the invention is for above-mentioned existing technology drawback, a kind of preparation method and application thereof of adopting the medicines such as biodegradable macromolecular material CS-co-PLA and Flusilazole, imazalil to prepare sustained-release nano microsphere preparations is provided.
Can take following technical scheme to realize purpose.
The preparation method of a kind of Flusilazole, fludioxonil sustained-release nano microsphere preparations.Its processing step is:
1, the medicines such as Flusilazole (a.i.) of 0.01%-1% are joined the shell that contains 1%-5% poly--dichloromethane solution of sugared copolymer of poly lactic acid (CS-co-PLA) in (medicine such as Flusilazole and CS-co-PLA mass ratio 1: 5,1: 10,1: 50 or 1: 100), ultrasonic fully dissolving makes solution A.
2,1% PVA is dissolved in the water, makes solution B.
3, B is added drop-wise to (A and B volume ratio are 1: 10) among the A, rotating speed with 500r/min stirs 10min, fast mixed liquor ultrasonication 5min is obtained the emulsion of O/W, the emulsion rotary evaporation is removed the medicament nano microball preparations such as 150-300nm Flusilazole that organic solvent makes medicine carrying amount 10%-30%, and encapsulation ratio reaches more than 75%.
The medicament nano microball preparations such as prepared Flusilazole, microsphere supported material are the amphipathic graft copolymer chitosan-polylactic acids.
The medicament nano microball preparations such as prepared Flusilazole, the medicine such as Flusilazole and CS-co-PLA mass ratio 1: 5,1: 10,1: 50 or 1: 100.
The medicament nano microball preparations such as prepared Flusilazole, Nano microsphere medicine carrying amount 10-30%, particle diameter are below 300nm, and encapsulation ratio reaches 75%.
The medicament nano microball preparations such as prepared Flusilazole are used for control grape canker.
The usage amount of the medicament nano microball preparations such as prepared Flusilazole can change in certain scope, depends on the object and the content of this medicine in Nano microsphere that are applied.
The medicament nano microball preparations such as prepared Flusilazole use with conventional method when reality is used, and for example use by spraying.
The medicament nano microball preparations such as prepared Flusilazole are compared with conventional art, and obtained technological progress is:
1, particle diameter is very little, and surface tension is low, has fabulous permeability, wetability, levelability and rheological characteristic; The equal particle diameter 150-300nm of its microballoon can make the medicine high degree of dispersion.
2, solvent is water, pollutes littlely, has reduced cost.
3, have the function that control discharges, prolong the lasting period of same dose medicine, improved the availability of medicine, reduced dosage, thereby reduced cost.
4, suppress medicine decomposition and loss that environmental factor causes, improved the stability of medicament itself, be conducive to ecotope.The medicament sustained-release nano microsphere preparations such as Flusilazole are used for control grape canker, have and improve plant osmosis, prolong drug effect, control discharges in soil, reduces and pollutes, and shelters bad smell, improve stability, reduce control or application times and the total consumption of agricultural chemicals.Economy, safety, environmental friendliness, difficult by environmental factor and microbial destruction and loss significantly improve the bioavilability of its agricultural chemicals.Solve the situation of selling well control problem of medicament, increased duration of efficacy, reduced cost, slowed down the ecological environment of soil problem, enlarged the scope of application.
The key technical indexes of the medicament nano microball preparations such as Flusilazole:
1, carrier material is Biodegradable polymer material, and environmental friendliness has good biocompatibility.
2, the medicine carrying amount of the medicament nano microball preparation such as Flusilazole reaches 10%-30%, and encapsulation ratio reaches more than 75%.
3, the medicament nano microball preparation such as Flusilazole has the control release function, prolongs the lasting period of same dose medicine, improves the availability of medicine, has reduced dosage, thereby has reduced cost.
4, the medicines such as Flusilazole are carried into Nano microsphere with the CS-co-PLA bag.By selecting the polymerization single polymerization monomer of different proportionings, the active ingredient of medicine microspheres can be controlled at 15-30 days release time, require to select prolongation to control release time according to difference.
5, HPLC method (Acta Pharmaceutica Sinica, 2003,38 (4) are adopted in the drug release rate test, 302), detection range is from more than the 0.1 μ g/L-200 μ g/L, trace detection different time burst size, and its rate of release meets First order reaction.
Embodiment:
The medicament sustained-release nano microsphere preparations preparation methods such as Flusilazole are described further with representative instance.
The preparation method of Flusilazole, fludioxonil sustained-release nano microsphere preparations, processing step is:
Embodiment 1.
1,0.2% medicines such as Flusilazole (a.i.) are joined in the dichloromethane solution of the chitosan-polylactic acid copolymer (CS-co-PLA) that contains 1%-5% (medicine such as Flusilazole and CS-co-PLA mass ratio 1: 5), ultrasonic fully dissolving makes solution A.
2,1% PVA is dissolved in the water, makes solution B.
3, B is added drop-wise to (A and B volume ratio are 1: 10) among the A, rotating speed with 500r/min stirs 10min, fast mixed liquor ultrasonication 5min is obtained the emulsion of O/W, the emulsion rotary evaporation is removed the medicament nano microball preparations such as 280nm Flusilazole that organic solvent makes medicine carrying amount 30%.
Embodiment 2.
1,0.01% medicines such as Flusilazole (a.i.) are joined in the dichloromethane solution of the chitosan-polylactic acid copolymer (CS-co-PLA) that contains 1%-5% (medicine such as Flusilazole and CS-co-PLA mass ratio 1: 100), ultrasonic fully dissolving makes solution A.
2,1% PVA is dissolved in the water, makes solution B.
3, B is added drop-wise to (A and B volume ratio are 1: 10) among the A, rotating speed with 500r/min stirs 10min, fast mixed liquor ultrasonication 5min is obtained the emulsion of O/W, the emulsion rotary evaporation is removed the medicament nano microball preparations such as 180nm Flusilazole that organic solvent makes medicine carrying amount 10%.
Embodiment 3.
Flusilazole, fludioxonil sustained-release nano microsphere preparations under 200mg/L concentration to the inhibition of grape ulcer bacteria.
Flusilazole of the present invention, fludioxonil nano microsphere preparations are obvious to the inhibition of grape ulcer bacteria, after tested, inhibition is up to 90%, significantly is better than present conventional dose (the Flusilazole fungistatic effect 81% such as 40% and fludioxonil wetting powder fungistatic effect 85% of 50% etc.).
Embodiment 4.
Flusilazole, fludioxonil sustained-release nano microsphere preparations are to the osmotic effect of grape limb.
Flusilazole of the present invention, the fludioxonil nano microsphere preparations can obviously improve medicament to the permeability of grape limb and blade, after tested, the nano microsphere preparations of Flusilazole of the present invention and fludioxonil to grape branch dry treatment 24h after, medicament infiltration ratio reaches respectively 5.06% and 4.80%, the Flusilazole of contrast medicament 40% and 50% fludioxonil wetting powder permeate ratio and are respectively 2.24% and 2.21%, therefore, Flusilazole of the present invention, the fludioxonil sustained-release nano microsphere preparations can significantly improve the permeability of medicament, improves the control efficiency to the grape canker.
Claims (6)
1. preparation method who prevents and treats the sustained-release nano microsphere preparations of grape canker is characterized in that processing step is:
1) medicines such as Flusilazole (a.i.) with 0.01%-1% join in the dichloromethane solution of the chitosan-polylactic acid copolymer that contains 1%-5%, and ultrasonic fully dissolving makes solution A.
2) 1% PVA is dissolved in the water, makes solution B.
3) B is added drop-wise to (A and B volume ratio are 1: 10) among the A, rotating speed with 500r/min stirs 10min, fast mixed liquor ultrasonication 5min is obtained the emulsion of O/W, the emulsion rotary evaporation is removed the medicament nano microball preparations such as 150-300nm Flusilazole that organic solvent makes medicine carrying amount 10%-30%.
2. a kind of preparation method who prevents and treats the sustained-release nano microsphere preparations of grape canker according to claim 1 is characterized in that the medicine that wraps up is the medicament that the grape Pathogenic Fungus of Canker is had inhibition, comprises Flusilazole, fludioxonil, imazalil etc.
3. a kind of preparation method who prevents and treats the sustained-release nano microsphere preparations of grape canker according to claim 1, the carrier material that it is characterized in that Nano microsphere is the amphipathic graft copolymer chitosan-polylactic acid.
4. a kind of preparation method who prevents and treats the sustained-release nano microsphere preparations of grape canker according to claim 1 is characterized in that the medicines such as Flusilazole and CS-co-PLA mass ratio 1: 5,1: 10, and 1: 50 or 1: 100.
5. a kind of preparation method who prevents and treats grape canker sustained-release nano microsphere preparations according to claim 1 is characterized in that particle diameter is below 300nm.
6. a kind of preparation method who prevents and treats the sustained-release nano microsphere preparations of grape canker according to claim 1 is characterized in that preventing and treating the grape canker.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2011102876613A CN103004859A (en) | 2011-09-26 | 2011-09-26 | Preparation method and application of sustained-release nanoparticle preparation for preventing and treating grape ulcer |
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| CN2011102876613A CN103004859A (en) | 2011-09-26 | 2011-09-26 | Preparation method and application of sustained-release nanoparticle preparation for preventing and treating grape ulcer |
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| CN103004859A true CN103004859A (en) | 2013-04-03 |
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| CN2011102876613A Pending CN103004859A (en) | 2011-09-26 | 2011-09-26 | Preparation method and application of sustained-release nanoparticle preparation for preventing and treating grape ulcer |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103783039A (en) * | 2013-12-27 | 2014-05-14 | 中国农业科学院植物保护研究所 | Azoxystrobin nanocapsule with shell-core structure and preparation method thereof |
| CN107279174A (en) * | 2016-07-25 | 2017-10-24 | 中国农业科学院植物保护研究所 | A kind of preparation method of gamma cyhalothrin nano pesticide |
| CN107593699A (en) * | 2017-09-01 | 2018-01-19 | 中国热带农业科学院环境与植物保护研究所 | A kind of sustained-release micro-spheres for being used to sterilize and preparation method thereof |
| CN108684688A (en) * | 2018-06-14 | 2018-10-23 | 国家纳米科学中心 | A kind of nano pesticide composition and preparation method thereof |
| CN108782570A (en) * | 2018-08-31 | 2018-11-13 | 中国热带农业科学院环境与植物保护研究所 | Triazolone propiconazole polylactic acid microsphere and preparation method thereof |
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| JPH07258087A (en) * | 1994-03-25 | 1995-10-09 | Toko Yakuhin Kogyo Kk | Allopurinol gargarisma |
| CN101352420A (en) * | 2008-09-08 | 2009-01-28 | 厦门大学 | Hydroxycamptothecin sustained-release microsphere and preparation method thereof |
| CN101637453A (en) * | 2009-08-14 | 2010-02-03 | 西北工业大学 | Method for preparing amifostine microspheres |
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2011
- 2011-09-26 CN CN2011102876613A patent/CN103004859A/en active Pending
Patent Citations (3)
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| JPH07258087A (en) * | 1994-03-25 | 1995-10-09 | Toko Yakuhin Kogyo Kk | Allopurinol gargarisma |
| CN101352420A (en) * | 2008-09-08 | 2009-01-28 | 厦门大学 | Hydroxycamptothecin sustained-release microsphere and preparation method thereof |
| CN101637453A (en) * | 2009-08-14 | 2010-02-03 | 西北工业大学 | Method for preparing amifostine microspheres |
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| MIN LI ETC.: ""A novel chitosan-poly(lactide) copolymer and its submicron particles as imidacloprid carriers"", 《PEST MANAGEMENT SCIENCE》 * |
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| 宋倩等: ""可控缓释纳米农药制剂及其研究进展"", 《植物保护科技创新与发展》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103783039A (en) * | 2013-12-27 | 2014-05-14 | 中国农业科学院植物保护研究所 | Azoxystrobin nanocapsule with shell-core structure and preparation method thereof |
| CN107279174A (en) * | 2016-07-25 | 2017-10-24 | 中国农业科学院植物保护研究所 | A kind of preparation method of gamma cyhalothrin nano pesticide |
| CN107279174B (en) * | 2016-07-25 | 2020-01-14 | 中国农业科学院植物保护研究所 | Preparation method of efficient cyhalothrin nano pesticide |
| CN107593699A (en) * | 2017-09-01 | 2018-01-19 | 中国热带农业科学院环境与植物保护研究所 | A kind of sustained-release micro-spheres for being used to sterilize and preparation method thereof |
| CN108684688A (en) * | 2018-06-14 | 2018-10-23 | 国家纳米科学中心 | A kind of nano pesticide composition and preparation method thereof |
| CN108782570A (en) * | 2018-08-31 | 2018-11-13 | 中国热带农业科学院环境与植物保护研究所 | Triazolone propiconazole polylactic acid microsphere and preparation method thereof |
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Application publication date: 20130403 |