CN103262849A - Agricultural phytosterol bactericide, and preparation method and application thereof - Google Patents
Agricultural phytosterol bactericide, and preparation method and application thereof Download PDFInfo
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- CN103262849A CN103262849A CN2013101671085A CN201310167108A CN103262849A CN 103262849 A CN103262849 A CN 103262849A CN 2013101671085 A CN2013101671085 A CN 2013101671085A CN 201310167108 A CN201310167108 A CN 201310167108A CN 103262849 A CN103262849 A CN 103262849A
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Abstract
The invention belongs to the pesticide field, and concretely relates to an agricultural phytosterol bactericide. The bactericide contains 3-70% of an effective active component. Phytosterol can be added into a wetting agent, a dispersant, a filler and the like to prepare a wettable pulvis, can be added into antifreeze agent, a wetting dispersant, a thickening agent, an antiseptic and water in proportion to prepare a suspending agent, can also be added into an emulsifier, a solvent and water in proportion to prepare an emulsion in water. The agricultural phytosterol bactericide can be used for controlling crop, fruit and vegetable diseases comprising Cytospora sp, Alternaria oleracea, Coniella diplodiella and the like. According to the invention, phytosterol is from plants, is well compatible to the environment and is easy to degrade, so the phytosterol bactericide is a botanical bactericide and has a wide market prospect.
Description
Technical field
The invention belongs to pesticide field, be specifically related to a kind of disinfectant use in agriculture.
Background technology
Come prevention and elimination of disease and pests to spray chemical pesticide in agricultural production management and storage, be still a kind of important means in the present plant protection, its advantage is that instant effect, handled easily, cost restriction low, that be subjected to envirment factor are less etc.But simple the dependence and the long-term chemical pesticide that uses will cause that disease worm fauna changes aggravation, and dangerous venereal disease worm is constantly taken place and be more and more serious." three R " problem is more and more outstanding.Along with rapid economy development and people's living standard improve constantly, food-safety problem becomes the focus that people pay close attention to, and has developed into worldwide problem.Residue of pesticide are to the mankind's threat in people's pay attention to day by day agricultural product, and food security has become the major criterion of weighing a national economic strength.Invention and the application of agricultural chemicals have improved crop yield, but because a large amount of unreasonable uses, the residue of pesticide in the food reveal day by day to the negative effect that human health causes.The product quality sampling result of State General Administration for Quality Supervision's announcement in 2000 shows that Multiple Pesticides is residual more general in the vegetables, and the residual quantity problem that exceeds standard is given prominence to, and organo-chlorine pesticide, organophosphorous pesticide, pyrethroid pesticide are the main causes that causes its residual contamination.Because " three R " problem of chemical pesticide, in recent years, country is to an organic solvent restriction increasingly stringent in the pesticidal preparations, and exploitation higher effective and lower toxic pesticide, eco-friendly novel agrochemical become the important development direction of pesticide field as the alternative kind of agricultural chemicals such as organic phosphor.Seeking bioactivator or directly develop botanical pesticide from plant, is the focus in current pesticide research field.Phytosterol has different physiological roles, and it has extensive use in fields such as medicine, cosmetics, growth of animal agent and sheet processing, printing, weaving, food, but does not still have the application report of phytosterol in the preparation disinfectant use in agriculture.
Summary of the invention
It is a kind of good to Environmental compatibility to the purpose of this invention is to provide, easily degraded, be a kind of be novel agricultural bactericide and preparation method thereof and the application in cereal class and fruit tree and vegetable disease control of effective active composition with the phytosterol.
For realizing purpose of the present invention, the present invention by the following technical solutions:
A kind of novel source agricultural bactericide is characterized in that, the effective active composition is phytosterol.
Novel agricultural bactericide of the present invention, described phytosterol are stigmasterol, the mixture of one or more compositions of cupreol and study on brassinolide.
Novel agricultural bactericide of the present invention, described effective active component content is 3～70%.
Novel agricultural bactericide of the present invention, described effective active component content is preferably 12～50%.
Novel agricultural bactericide of the present invention, described effective active component content is 20～40% (percentage by weights) more preferably.
The application of one plant sterols in the preparation of novel agricultural bactericide is characterized in that, adding wetting agent and filler are made wetting powder in the active ingredient.
The preparation of novel agricultural bactericide of the present invention, described phytosterol is stigmasterol, one or more mixtures of cupreol and study on brassinolide, wetting agent are one or more mixtures of lauryl sodium sulfate, neopelex, sodium alkyl sulfate, sodium alkyl benzene sulfonate, sldium lauryl sulfate and alkylphenol polyoxyethylene; Described filler is White Carbon black, diatomite, bentonite, talcum powder, precipitated calcium carbonate, zeolite and kaolinic a kind of.
The application of phytosterol of the present invention in the wetting powder preparation of novel agricultural bactericide is characterized in that described wetting agent content is 1～5% (percentage by weight), and filler content is 50～70% (percentage by weights).The application of one plant sterols in the preparation of novel agricultural bactericide is characterized in that, with phytosterol, emulsifier, solvent and water (percentage by weight) in proportion are made into aqueous emulsion.
The application of one plant sterols in the preparation of novel agricultural bactericide is characterized in that phytosterol, and antifreezing agent, wetting dispersing agent, thickener, preservative and water (percentage by weight) in proportion are made into suspending agent
Novel agricultural bactericide of the present invention is in the application of novel agricultural bactericide, and described phytosterol is one or more mixtures of stigmasterol, cupreol and study on brassinolide; Emulsifier is one or more mixtures of alkylphenol polyoxyethylene formaldehyde condensation products (700#), polyoxyethylene nonylphenol ether (OP-10), phenethyl phenol polyethenoxy ether (602#), phenethyl phenol polyoxyethylene poly-oxygen propylene aether (1601#, EPE type), castor oil polyoxyethylene ether (BY-125), tween series: Tween80, Tween60, castor oil ethylene oxide condensate (El-40); Solvent is benzinum, benzene, dimethylbenzene, toluene, ethanol, methyl alcohol, DMF, acetone, one or more mixtures of cyclohexanone and isopropyl alcohol; Described emulsifier is one or more mixtures of alkylphenol polyoxyethylene formaldehyde condensation products (700#), polyoxyethylene nonylphenol ether (OP-10), phenethyl phenol polyethenoxy ether (602#), phenethyl phenol polyoxyethylene poly-oxygen propylene aether (1601#, EPE type), castor oil polyoxyethylene ether (BY-125), tween series: Tween80, Tween60, castor oil ethylene oxide condensate (E1-40).
Preparation method on the one plant sterols disinfectant use in agriculture specifically may further comprise the steps:
(1) will contain sterol plant alcohol dipping, and use benzinum, ethyl acetate and extracting n-butyl alcohol respectively, and extract merging filtrate, decompression concentrates, and freeze drying is standby,
(2) active component in the benzinum phase medicinal extract is separated,
(3) with sterol material and auxiliary agent and auxiliary materials and mixing, make a kind of in wetting powder, aqueous emulsion, the suspending agent.
The invention has the beneficial effects as follows,
Phytosterol is from plant, and easily degraded is environmentally friendly, is developed as disinfectant use in agriculture market and has a bright future.
Embodiment
(1) phytosterol 20～40%, wetting agent 5%, and filler 55～75% is processed into wetting powder with above-mentioned raw materials according to common process, adopts spray method to carry out the control of plant disease.
(2) phytosterol 50～800g/L, wetting dispersing agent 20～60g/L, antifreezing agent 40～100g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
(3) phytosterol 20～40%, emulsifier 5～15%, and antifreeze 5～10%, all the other are water.Above-mentioned raw materials is processed into aqueous emulsion according to common process, adopts spray method to carry out the control of plant disease.
Adopt embodiment to make further explanation to technical scheme of the present invention below, but do not limit the scope of the invention, the used preparation raw material of the present invention is commercially available.
The extraction of embodiment 1, phytosterol
(1) gather twigs of the chaste tree flower, extract 3 times with an amount of 80% alcohol dipping, merge 3 times filtrate, decompression concentrates, and freeze drying is standby.Twigs of the chaste tree flower ethanol extract is made suspension with an amount of distilled water, uses benzinum, ethyl acetate and extracting n-butyl alcohol respectively, and gained extract and the decompression of remaining water concentrate, and freeze drying is standby.
(2) adopt silica gel column chromatography that the active component in the benzinum phase medicinal extract is separated.With 200-300 order silica white 1500g, adopt wet method dress post, with 72.3g benzinum phase extract with an amount of petroleum ether dissolution, add 200-300 purpose silica white 100g and mix sample, application of sample is in capital, use benzinum successively, benzinum and ethyl acetate mixture (100: 1,50: 1,25: 1,20: 1,10: 1,5: 1,2: 1,1: 1), ethyl acetate, carry out gradient elution, according to the silica gel thin-layer chromatography result, merge Rf value same section, obtain 19 cuts, follow the tracks of by activity, the good cut of bacteriostatic activity is carried out column chromatography 2 times, separate obtaining reactive compound.Be accredited as the sterol material through GC/MS.
The preparation of embodiment 2,5% stigmasterol wetting powder
(1) extraction of sterol is with embodiment 1
(3) stigmasterol 40% (percentage by weight), lauryl sodium sulfate 5% (percentage by weight), diatomite 55% (percentage by weight) with its mixing, is made wetting powder through airslide disintegrating mill.
(4) sterol formulations is made into concentration is 0.4,0.2,0.1,0.05, five concentration gradients of 0.025mg/mL, adopts growth rate method to measure the bacteriostatic activity of Valsa mali, Chinese cabbage alternaria and fruit white rot of grape bacterium.
The preparation of embodiment 3.3% stigmasterol wetting powder
Except step (3) sterol material is 3% (percentage by weight), all the other are identical with embodiment 2.
The preparation of embodiment 4.10% stigmasterol wetting powder
Except step (3) sterol material is 10% (percentage by weight), all the other are identical with embodiment 2.
The preparation of embodiment 5.20% stigmasterol wetting powder
Except step (3) sterol material is 20% (percentage by weight), all the other are identical with embodiment 2.
The preparation of embodiment 6.60% stigmasterol wetting powder
Except step (3) sterol material is 60% (percentage by weight), all the other are identical with embodiment 2.
The preparation of embodiment 7.70% stigmasterol wetting powder
Except step (3) sterol material is 70% (percentage by weight), all the other are identical with embodiment 2.
The preparation of embodiment 8.40% cupreol wetting powder
Except step (3) the stigmasterol substitution of materials was cupreol, all the other were identical with embodiment 2.
Embodiment 9.40% study on brassinolide wetting powder
Except step (3) the stigmasterol substitution of materials was study on brassinolide, all the other were identical with embodiment 2
Embodiment 10.40% mixed phytosterin wetting powder
Except step (3) the stigmasterol substitution of materials is stigmasterol, beyond cupreol and the study on brassinolide mixture, all the other are identical with embodiment 2.
The preparation of embodiment 11. stigmasterol wetting powders
Except step (3) replaces lauryl sodium sulfate with sodium alkyl sulfate, all the other are identical with embodiment 2
The preparation of embodiment 12. stigmasterol wetting powders
Except step (3) replaces lauryl sodium sulfate with sldium lauryl sulfate, all the other are identical with embodiment 1.
The preparation of embodiment 13. stigmasterol wetting powders
Except step (3) replaces lauryl sodium sulfate with alkylphenol polyoxyethylene, all the other are identical with embodiment 1.
The preparation of embodiment 14. stigmasterol wetting powders
Except step (3) replaces lauryl sodium sulfate with lauryl sodium sulfate and alkylphenol polyoxyethylene mixture, all the other are identical with embodiment 1.
The preparation of embodiment 15. stigmasterol wetting powders
Except step (3) replaces lauryl sodium sulfate with sodium alkyl sulfate, sodium alkyl benzene sulfonate, sldium lauryl sulfate mixture, all the other are identical with embodiment 2.
The preparation of embodiment 16. stigmasterol wetting powders
Except step (3) replaces diatomite with talcum powder, all the other are identical with embodiment 2.
The preparation of embodiment 17. stigmasterol wetting powders
Except step (3) replaces diatomite with White Carbon black, all the other are identical with embodiment 2.
The preparation of embodiment 18. stigmasterol wetting powders
Except step (3) replaces diatomite with precipitated calcium carbonate, all the other are identical with embodiment 2.
The preparation of embodiment 19. stigmasterol wetting powders
Except step (3) replaces diatomite with diatomite, bentonite, talcum powder mixture, all the other are identical with embodiment 2.
Embodiment 20. replaces diatomite except step (3) with calcium carbonate, zeolite and kaolin mixture, and all the other are identical with embodiment 2.
Embodiment 21. replaces 5% diatomite except step (3) with 1% diatomite, and all the other are identical with embodiment 2
Embodiment 22. replaces 5% diatomite except step (3) 3% diatomite, and all the other are identical with embodiment 2.
Embodiment 23. replaces 55% lauryl sodium sulfate except step (3) 60% lauryl sodium sulfate, and all the other are identical with embodiment 2.
Embodiment 24. replaces 55% lauryl sodium sulfate except step (3) 70% lauryl sodium sulfate, and all the other are identical with embodiment 2.
The application of embodiment 25. stigmasterol suspending agents
Stigmasterol 50～800g/L, wetting dispersing agent 20～60g/L, antifreezing agent 40～100g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
Embodiment 26. stigmasterol suspending agents
Stigmasterol 160～600g/L, wetting dispersing agent 20～60g/L, antifreezing agent 40～100g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
Embodiment 27. stigmasterol suspending agents
Stigmasterol 200～300g/L, wetting dispersing agent 20～60g/L, antifreezing agent 40～100g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
Embodiment 28. stigmasterol suspending agents
Stigmasterol 200～300g/L, wetting dispersing agent 30～45g/L, antifreezing agent 40～100g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
Embodiment 29. stigmasterol suspending agents
Stigmasterol 200～300g/L, wetting dispersing agent 35～38g/L, antifreezing agent 40～100g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
Embodiment 30. stigmasterol suspending agents
Stigmasterol 200～300g/L, wetting dispersing agent 35～40g/L, antifreezing agent 60～80g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
Embodiment 31. stigmasterol suspending agents
Stigmasterol 200～300g/L, wetting dispersing agent 35～40g/L, antifreezing agent 60～80g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
Embodiment 32. stigmasterol aqueous emulsions
Phytosterol 20～40%, emulsifier 5～15%, antifreeze 5～10%, all the other are water.Above-mentioned raw materials is processed into aqueous emulsion according to common process, adopts spray method to carry out the control of plant disease.
The mensuration of embodiment 33. phytosterol wetting powder bacteriostatic activities
Sterol formulations is made into concentration is 0.4,0.2,0.1,0.05, five concentration gradients of 0.025mg/mL, adopts growth rate method (NY/T1156.2-2006) to measure the bacteriostatic activity of Valsa mali, Chinese cabbage alternaria and fruit white rot of grape bacterium.The result is as follows
Table 1 phytosterol wetting powder is to the Valsa mali biologically active
Table 2 phytosterol wetting powder is to fruit white rot of grape bacterium biologically active
Table 3 phytosterol wetting powder is to Chinese cabbage alternaria biologically active
The mensuration of embodiment 34. phytosterol suspending agent bacteriostatic activities
Table 4 phytosterol suspending agent is to the Valsa mali biologically active
Table 5 phytosterol suspending agent is to fruit white rot of grape bacterium biologically active
Table 6 phytosterol suspending agent is to Chinese cabbage alternaria biologically active
The mensuration of embodiment 35. phytosterol aqueous emulsion bacteriostatic activities
Table 7 phytosterol aqueous emulsion is to the Valsa mali biologically active
Table 8 phytosterol aqueous emulsion is to fruit white rot of grape bacterium biologically active
Table 9 phytosterol aqueous emulsion is to Chinese cabbage alternaria biologically active
Experimental result shows that phytosterol is to the EC of Valsa mali, fruit white rot of grape bacterium and Chinese cabbage alternaria
50Be respectively 0.086～0.21,0.23～0.33,0.14～0.23mg/mL.
The preparation method of embodiment 36. phytosterol wettable powder formulation bactericide
(1) gather twigs of the chaste tree flower, extract 3 times with an amount of 80% alcohol dipping, merge 3 times filtrate, decompression concentrates, and freeze drying is standby.Twigs of the chaste tree flower ethanol extract is made suspension with an amount of distilled water, uses benzinum, ethyl acetate and extracting n-butyl alcohol respectively, and gained extract and the decompression of remaining water concentrate, and freeze drying is standby.
(2) adopt silica gel column chromatography that the active component in the benzinum phase medicinal extract is separated.With 200-300 order silica white 1500g, adopt wet method dress post, with 72.3g benzinum phase extract with an amount of petroleum ether dissolution, add 200-300 purpose silica white 100g and mix sample, application of sample is in capital, use benzinum successively, benzinum and ethyl acetate mixture (100: 1,50: 1,25: 1,20: 1,10: 1,5: 1,2: 1,1: 1), ethyl acetate, carry out gradient elution, according to the silica gel thin-layer chromatography result, merge Rf value same section, obtain 19 cuts, follow the tracks of by activity, the good cut of bacteriostatic activity is carried out column chromatography 2 times, separate obtaining reactive compound.Be accredited as the sterol material through GC/MS.
(3) the sterol material 40%, wetting agent 5%, and filler 55% with its mixing, is made wetting powder through airslide disintegrating mill.
The preparation method of embodiment 37. phytosterol suspending agent type bactericide
Step (1) (2) is with embodiment 36
(3) phytosterol 50～800g/L, wetting dispersing agent 20～60g/L, antifreezing agent 40～100g/L, thickener 0.55g/L, 0.1～0.5g/L, all the other are water.Above-mentioned raw materials is processed into suspending agent according to common process, adopts spray method to carry out the control of plant disease.
The preparation method of embodiment 38. phytosterol water and milk formulation bactericide
Step (1) (2) is with embodiment 36
(3) phytosterol 20～40%, emulsifier 5～15%, and antifreeze 5～10%, all the other are water.Above-mentioned raw materials is processed into aqueous emulsion according to common process, adopts spray method to carry out the control of plant disease.
Above-described embodiment is preferred embodiments of the present invention; but embodiments of the present invention are not limited by above-described embodiment, and the substitute mode that change, modification, combination, the simplification of making under other any spiritual essence that does not deviate from and the principle all should be equivalence all is contained within protection scope of the present invention.
Claims (11)
1. a novel agricultural bactericide is characterized in that, the effective active composition is phytosterol.
2. according to the novel agricultural bactericide of claim 1, it is characterized in that described phytosterol is stigmasterol, the mixture of one or more compositions of cupreol and study on brassinolide.
3. according to the novel agricultural bactericide of claim 1 or 2, it is characterized in that described effective active component content is 3～70% (percentage by weights).
4. according to the novel agricultural bactericide of claim 1 or 2, it is characterized in that described effective active component content is 12～50% (percentage by weights).
5. according to the novel agricultural bactericide of claim 1 or 2, it is characterized in that described effective active component content is 20～40% (percentage by weights).
6. the application of phytosterol each described novel agricultural bactericide in claim 1～5 is characterized in that, add in the phytosterol wetting agent, and filler make wetting powder.
7. according to the application in each described novel agricultural bactericide in claim 1～5 of claim 6 phytosterol, it is characterized in that described wetting agent content is 1～5% (percentage by weight), filler content is 50～70% (percentage by weights).
8. according to phytosterol application in each described novel agricultural bactericide in claim 1～5 of claim 6, it is characterized in that, the serve as reasons mixture of one or more compositions of being selected from lauryl sodium sulfate, neopelex, sodium alkyl sulfate, sodium alkyl benzene sulfonate, sldium lauryl sulfate and alkylphenol polyoxyethylene of described wetting agent, described filler is the mixture of White Carbon black, diatomite, bentonite, talcum powder, precipitated calcium carbonate, zeolite and kaolinic one or more compositions.
9. phytosterol application in each described novel agricultural bactericide in claim 1～5 is characterized in that phytosterol, antifreezing agent, and wetting dispersing agent, thickener, preservative and water are made into suspending agent in proportion.
10. the application of phytosterol each described novel agricultural bactericide in claim 1～5 is characterized in that phytosterol, and emulsifier, solvent and water are made into aqueous emulsion in proportion.
11. the preparation method on the plant sterols disinfectant use in agriculture specifically may further comprise the steps:
(1) will contain sterol plant alcohol dipping, and use benzinum, ethyl acetate and extracting n-butyl alcohol respectively, and extract merging filtrate, decompression concentrates, and freeze drying is standby.
(2) active component in the benzinum phase medicinal extract is separated.
(3) with sterol material and auxiliary agent and auxiliary materials and mixing, make a kind of in wetting powder, aqueous emulsion, the suspending agent.
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| CN107114386A (en) * | 2017-05-04 | 2017-09-01 | 四川农业大学 | The application of Sitosterolum and preparation |
| IT201700066508A1 (en) * | 2017-06-15 | 2018-12-15 | Isagro Spa | SUSPENSIONS CONCENTRATED OF PHYTOSTEROLS AND RELATIVE PREPARATION PROCESS |
| CN113575232A (en) * | 2021-07-30 | 2021-11-02 | 西北农林科技大学 | Application of brassinosteroids in prevention and treatment of apple tree canker |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107114386A (en) * | 2017-05-04 | 2017-09-01 | 四川农业大学 | The application of Sitosterolum and preparation |
| CN107114386B (en) * | 2017-05-04 | 2019-11-29 | 四川农业大学 | The application of cupreol and preparation |
| IT201700066508A1 (en) * | 2017-06-15 | 2018-12-15 | Isagro Spa | SUSPENSIONS CONCENTRATED OF PHYTOSTEROLS AND RELATIVE PREPARATION PROCESS |
| WO2018229710A1 (en) * | 2017-06-15 | 2018-12-20 | Isagro S.P.A. | Phitosterols suspension concentrates and process of preparation thereof |
| CN110719734A (en) * | 2017-06-15 | 2020-01-21 | 伊萨格罗股份公司 | Phytosterol suspension concentrate and preparation method thereof |
| US11291207B2 (en) | 2017-06-15 | 2022-04-05 | Isagro S.P.A. | Phitosterols suspension concentrates and process of preparation thereof |
| CN110719734B (en) * | 2017-06-15 | 2022-08-12 | 伊萨格罗股份公司 | Phytosterol suspension concentrate and preparation method thereof |
| CN113575232A (en) * | 2021-07-30 | 2021-11-02 | 西北农林科技大学 | Application of brassinosteroids in prevention and treatment of apple tree canker |
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Application publication date: 20130828 |