CN104304249A - Controlled release formulation for preventing and treating wheat scab and preparation method thereof - Google Patents
Controlled release formulation for preventing and treating wheat scab and preparation method thereof Download PDFInfo
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- CN104304249A CN104304249A CN201410584561.0A CN201410584561A CN104304249A CN 104304249 A CN104304249 A CN 104304249A CN 201410584561 A CN201410584561 A CN 201410584561A CN 104304249 A CN104304249 A CN 104304249A
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- jinggangmycin
- release agent
- sustained release
- chitosan oligosaccharide
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- 238000002360 preparation method Methods 0.000 title claims description 10
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- 238000013270 controlled release Methods 0.000 title abstract 6
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Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a controlled release formulation for preventing and treating wheat scab. Effective components of the controlled release formulation are chitosan oligosaccharide and jinggangmycin A. A method for preparing the controlled release formulation comprises the following steps: performing reaction on bentonite and organic cationic surface active agents at the temperature of 25-70 DEG C to obtain organic modified bentonite; mixing the organic modified bentonite with acetone solutions of the jinggangmycin A; performing pressure reduction evaporation for recycling solvents to obtain powder organic modified bentonite inner cores absorbed with the jinggangmycin A; uniformly dispersing the powder inner cores into sodium alga acid solutions with the mass percentage of 3 percent; adding chitosan oligosaccharide water solution for homogenizing for 1.5-2 hours at high speed; regulating pH to perform pressure reduction filtration or centrifugal separation on the obtained suspension liquid; drying a part of solids to obtain micro-particle shaped controlled release formulation. The controlled release formulation has an obvious microbe inhibition effect, and is environmentally friendly and free of residues.
Description
Technical field
The present invention relates to a kind of for sustained release agent preventing and treating wheat scab and preparation method thereof, being specifically related to the composite sustained release agent of chitosan oligosaccharide and jinggangmycin A for preventing and treating wheat scab, belonging to pesticide field.
Background technology
Wheat scab, mainly causes that seedling is withered, fringe is rotten, brown foot rot, stalk is rotten and fringe is rotten, all can be injured from seedling to heading.Wherein affect is the most seriously that fringe is rotten.Seedling corruption is caused by seed-borne fungi or soil, invalid body infects.Bud mutation was brown before this, and then root cap rots thereupon, and the sick seedling Huang of the lighter is thin, and severe one is dead, produces pink mustiness thing (germ conidium and stroma) during withered seedling high humidity.During fringe corruption wheat flowering, just on small ear and lepicena, produce the light brown spot of water soaking mode, be gradually extended to whole small ear, small ear is withered and yellow.During high humidity, scab place produces the gluey mould layer of pink.Later stage, it produced intensive black-and-blue granule (germ perithecium).Touch with hand, have projection to feel, can not erase, seed is shrivelled and mould to pink with white.Extend to cob after small ear morbidity, sick portion is withered brown, makes the above small ear in killed portion, forms withered dead ears.Brown foot rot all can occur from coming up to maturation, wheat strain base portion tissue be injured after browning rotten, cause complete stool withered.Stalk corruption to mostly occur under fringe first and second joint, on leaf sheath, just occur water stain shape chlorisis spot, after expand to filbert to the irregular shape spot of bronzing or expand in stem.When being in a bad way, cause more than disease portion withered and yellow, sometimes can not ear or extract out withered and yellow fringe.The visible pink mould layer in surface, disease portion when having a humid climate.
Chitosan oligosaccharide and Chitosan poly oligosaccharide, also claim chitin oligo saccharide, formal name used at school β-Isosorbide-5-Nitrae-oligosaccharides-gucosamine, and being a kind of product obtained through special biological enzyme technology process by shitosan, is a kind of good water solubility, and function is large, the low molecular weight product that biologically active is high.Chitosan oligosaccharide, by being adsorbed on bacterial cell surface, forming one deck polymeric membrane, thus plays restraining and sterilizing bacteria effect; Another kind of mechanism is that chitosan oligosaccharide passes through to penetrate in bacterial cell body, the cytoplasm with anion in cyton is flocculated, upsets the normal physiological activity of cell, thus kill bacteria.In general, molecular weight is larger, and the outer membrane formed is finer and close, nutriment more can be stoped to enter bacterial cell, thus antibacterial action successful; Molecular weight is less, more easily enters in the gap structure of cell wall, thus the metabolism of interference cell, bactericidal action is obvious.Chitosan oligosaccharide itself, containing abundant carbon and nitrogen, can be decomposed by the microorganisms and to utilize and as the nutrient of plant growth, chitosan oligosaccharide can promote that beneficial microorganism grows and suppresses some phytopathogens.Chitosan oligosaccharide also can stimulating plant growth and the disease resistance of inducing plant, has direct repression to a certain degree to various plants pathogen.
Jinggangmeisu comprises jinggangmycin A and jinggangmeisu (mixture of jinggangmycin A and its isomer B, C, D, E, F), at present by the single dose of national agriculture chemical registration, is mainly used in control crop banded sclerotial blight.Its compound formulation includes, composite with waxy Bacillus, for preventing and treating banded sclerotial blight, rice blast, head blight; Composite with carbendazim, for preventing and treating banded sclerotial blight, rice blast, head blight; Composite with tricyclazole, for preventing and treating banded sclerotial blight, rice blast, false smut; Composite with carbendazim, for preventing and treating rice blast, false smut; With olefin conversion or ucleosides antibiotic composite, for preventing and treating banded sclerotial blight, false smut; With own azoles alcohol or oxyenadenine composite, for preventing and treating banded sclerotial blight; Composite with bacillus subtilis, for preventing and treating false smut.Jinggangmeisu is to people and animals' low toxicity, and to birds fish safety, absorption farm antibiotics series bactericidal agent in belonging to, by disturbing and suppressing pathogen cell normal growth to be grown, plays therapeutic action.
In prior art, the usage amount of agricultural chemicals is increasing, not only makes crop produce resistance, also brings serious pollution to environment, for the problems referred to above, the invention provides a kind of for sustained release agent preventing and treating wheat scab and preparation method thereof.
Technical scheme of the present invention is as follows:
For preventing and treating a sustained release agent for wheat scab, active ingredient is chitosan oligosaccharide and jinggangmycin A.In the present invention, active ingredient content is by mass percentage 1%-3% chitosan oligosaccharide and 10%-20% jinggangmycin A; Preferably, active ingredient content is by mass percentage 1.5%-2.5% chitosan oligosaccharide and 12%-18% jinggangmycin A; Preferred, active ingredient content is by mass percentage 1.5% chitosan oligosaccharide and 14% jinggangmycin A.
Prepare the method for above-mentioned sustained release agent, comprise following concrete steps:
By the organic modified bentonite that bentonite and organic cation surfactant are obtained by reacting at 25-70 DEG C, mix with the acetone soln of jinggangmycin A, the mass ratio of organic modified bentonite and jinggangmycin A is 2-5:1, reduction vaporization recycling design, obtains pulverous organic modified bentonite kernel being adsorbed with jinggangmycin A; Then this Powdered kernel being evenly spread to mass fraction is in 3% sodium alginate soln, and wherein, the mass ratio of sodium alginate and jinggangmycin A is 3.5-4:1, then adds the chitosan oligosaccharide aqueous solution, high speed homogenisation process 1.5-2 hour; Regulate pH by gained suspension filtration under diminished pressure or centrifugation, solids portion after drying, obtains the microparticle shape sustained release agent that particle diameter is 50-600 micron.
Above-mentioned preparation method of organic modified bentonite is as follows:
Get 100g bentonite to add in 2L water, then add 20g softex kw, be heated to 70 DEG C, continue stirring 2 hours, centrifugation goes out solids, and after washing 4 times with distilled water, be placed in 110 DEG C of baking ovens and be dried to constant weight, cross 100 mesh sieves after pulverizing, obtain organic modified bentonite.
Sustained release agent tool of the present invention has the following advantages:
(1) utilize the suction-operated of organic modifiers bentonite strengthening to jinggangmycin A, and then utilize the coating function of sodium alginate and another active ingredient chitosan oligosaccharide of the present invention, obviously extend the release time of drug effect, significantly improve drugloading rate;
(2) prepared the micron order fine-grained agent of favorable dispersibility by high speed homogenisation, compared with bulky grain agent, can more effectively be uniformly distributed on paddy rice;
(3) the present invention is environmentally friendly, noresidue.
Summary of the invention
Embodiment
Further describe the present invention below in conjunction with specific embodiment, advantage and disadvantage of the present invention will be more clear along with description.But embodiment is only exemplary, does not form any restriction to scope of the present invention.It will be understood by those skilled in the art that and can modify to the details of technical solution of the present invention and form or replace down without departing from the spirit and scope of the present invention, but these amendments and replacement all fall within the scope of protection of the present invention.
Embodiment 1 one kinds is for preventing and treating the sustained release agent of wheat scab
Active ingredient is chitosan oligosaccharide and 14% jinggangmycin A of 1.5%.
Prepare the method for above-mentioned sustained release agent, comprise following concrete steps:
Mixed with the acetone soln of jinggangmycin A by machine modified alta-mud, the mass ratio of organic modified bentonite and jinggangmycin A is 3:1, reduction vaporization recycling design, obtains pulverous organic modified bentonite kernel being adsorbed with jinggangmycin A; Then this Powdered kernel being evenly spread to mass fraction is in 3% sodium alginate soln, and wherein, the mass ratio of sodium alginate and jinggangmycin A is 3.8:1, then adds the chitosan oligosaccharide aqueous solution, high speed homogenisation process 2 hours; Regulate pH by gained suspension filtration under diminished pressure or centrifugation, solids portion after drying, obtains the microparticle shape sustained release agent that particle diameter is 50-600 micron.
Above-mentioned preparation method of organic modified bentonite is as follows:
Get 100g bentonite to add in 2L water, then add 20g softex kw, be heated to 70 DEG C, continue stirring 2 hours, centrifugation goes out solids, and after washing 4 times with distilled water, be placed in 110 DEG C of baking ovens and be dried to constant weight, cross 100 mesh sieves after pulverizing, obtain organic modified bentonite.
Embodiment 2 one kinds is for preventing and treating the sustained release agent of wheat scab
Active ingredient is chitosan oligosaccharide and 18% jinggangmycin A of 1%.
Prepare the method for above-mentioned sustained release agent, comprise following concrete steps:
Mixed with the acetone soln of jinggangmycin A by machine modified alta-mud, the mass ratio of organic modified bentonite and jinggangmycin A is 4:1, reduction vaporization recycling design, obtains pulverous organic modified bentonite kernel being adsorbed with jinggangmycin A; Then this Powdered kernel being evenly spread to mass fraction is in 3% sodium alginate soln, and wherein, the mass ratio of sodium alginate and jinggangmycin A is 4:1, then adds the chitosan oligosaccharide aqueous solution, high speed homogenisation process 2 hours; Regulate pH by gained suspension filtration under diminished pressure or centrifugation, solids portion after drying, obtains the microparticle shape sustained release agent that particle diameter is 50-600 micron.
Above-mentioned preparation method of organic modified bentonite is with embodiment 1.
Embodiment 3 one kinds is for preventing and treating the sustained release agent of wheat scab
Active ingredient is chitosan oligosaccharide and 12% jinggangmycin A of 2.5%.
Prepare the method for above-mentioned sustained release agent, comprise following concrete steps:
Mixed with the acetone soln of jinggangmycin A by machine modified alta-mud, the mass ratio of organic modified bentonite and jinggangmycin A is 5:1, reduction vaporization recycling design, obtains pulverous organic modified bentonite kernel being adsorbed with jinggangmycin A; Then this Powdered kernel being evenly spread to mass fraction is in 3% sodium alginate soln, and wherein, the mass ratio of sodium alginate and jinggangmycin A is 3.5:1, then adds the chitosan oligosaccharide aqueous solution, high speed homogenisation process 2 hours; Regulate pH by gained suspension filtration under diminished pressure or centrifugation, solids portion after drying, obtains the microparticle shape sustained release agent that particle diameter is 50-600 micron.
Above-mentioned preparation method of organic modified bentonite is with embodiment 1.
Test example 1 field control effectiveness test of the present invention
The chitosan oligosaccharide utilizing the present invention to prepare and the composite sustained release agent of jinggangmycin A carry out the controlling experiment of wheat scab in Shandong, dispenser 1 time, observe control efficiency the 7th day and the 21st day.Result of the test is as shown in table 1, and result shows, the control efficiency of single dose to wheat scab of chitosan oligosaccharide and jinggangmycin A is poor, and the present invention not only preventive effect is good, and the lasting period is long.
Table 1
Claims (9)
1. for preventing and treating a sustained release agent for wheat scab, it is characterized in that, active ingredient is chitosan oligosaccharide and jinggangmycin A.
2. sustained release agent according to claim 1, is characterized in that, in described sustained release agent, active ingredient content is by mass percentage 1%-3% chitosan oligosaccharide and 10%-20% jinggangmycin A.
3. sustained release agent according to claim 1, is characterized in that, in described sustained release agent, active ingredient content is by mass percentage 1.5%-2.5% chitosan oligosaccharide and 12%-18% jinggangmycin A.
4. sustained release agent according to claim 1, is characterized in that, in described sustained release agent, active ingredient content is by mass percentage 1.5% chitosan oligosaccharide and 14% jinggangmycin A.
5. the method for the sustained release agent of preparation as described in any one of claim 1-4, concrete steps are:
By the organic modified bentonite that bentonite and organic cation surfactant are obtained by reacting at 25-70 DEG C, mix with the acetone soln of jinggangmycin A, the mass ratio of organic modified bentonite and jinggangmycin A is 2-5:1, reduction vaporization recycling design, obtains pulverous organic modified bentonite kernel being adsorbed with jinggangmycin A; Then this Powdered kernel being evenly spread to mass fraction is in 3% sodium alginate soln, and wherein, the mass ratio of sodium alginate and jinggangmycin A is 3.5-4:1, then adds the chitosan oligosaccharide aqueous solution, high speed homogenisation process 1.5-2 hour; Regulate pH by gained suspension filtration under diminished pressure or centrifugation, solids portion after drying, obtains the microparticle shape sustained release agent that particle diameter is 50-600 micron.
6. method according to claim 5, is characterized in that, described preparation method of organic modified bentonite is as follows:
Get 100g bentonite to add in 2L water, then add 20g softex kw, be heated to 70 DEG C, continue stirring 2 hours, centrifugation goes out solids, and after washing 4 times with distilled water, be placed in 110 DEG C of baking ovens and be dried to constant weight, cross 100 mesh sieves after pulverizing, obtain organic modified bentonite.
7. method according to claim 5, is characterized in that, the mass ratio of described machine modified alta-mud and jinggangmycin A is 3:1.
8. method according to claim 5, is characterized in that, the mass ratio of described sodium alginate and jinggangmycin A is 3.8:1.
9. method according to claim 5, is characterized in that, the particle diameter of described microparticle shape sustained release agent is 100-350 micron.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105660639A (en) * | 2015-12-31 | 2016-06-15 | 江苏邦盛生物科技有限责任公司 | Bactericide composition containing oligosaccharins and validamycin A, and application thereof |
| CN106804594A (en) * | 2015-12-02 | 2017-06-09 | 中国科学院大连化学物理研究所 | A kind of broad spectrum activity oligosaccharides composite bactericide and its application |
| CN108812669A (en) * | 2018-06-19 | 2018-11-16 | 西南大学 | A kind of multilayer package carried medicine sustained-release hydrogel and preparation method thereof |
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| CN102405908A (en) * | 2011-10-28 | 2012-04-11 | 海南正业中农高科股份有限公司 | Chitosan oligosaccharide composition for resisting wheat scab and application and method of chitosan oligosaccharide composition |
| CN102939960A (en) * | 2012-11-06 | 2013-02-27 | 绍兴文理学院 | Sustained-release herbicide microparticle preparation and preparation method thereof |
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| CN108812669A (en) * | 2018-06-19 | 2018-11-16 | 西南大学 | A kind of multilayer package carried medicine sustained-release hydrogel and preparation method thereof |
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| CN104304249B (en) | 2016-08-17 |
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