CN103416437A - Preparation method for modified cytidine antibiotic oil suspension - Google Patents
Preparation method for modified cytidine antibiotic oil suspension Download PDFInfo
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- CN103416437A CN103416437A CN2012101618996A CN201210161899A CN103416437A CN 103416437 A CN103416437 A CN 103416437A CN 2012101618996 A CN2012101618996 A CN 2012101618996A CN 201210161899 A CN201210161899 A CN 201210161899A CN 103416437 A CN103416437 A CN 103416437A
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- cytidine
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Abstract
Provided is a preparation method for a modified cytidine antibiotic oil suspension. Modified cytidine antibiotic is a bactericidal effective component. N-n-butyl caproyl lactone is a penetration enhancer. Others are auxiliary elements which are allowed for use and acceptable in pesticides. The oil suspension is mainly used for control of vegetable pests and diseases. The oil suspension has advantages of synergy, good penetrability, strong adhesion, anti-evaporation and the like, and has good industrialized application prospect.
Description
Technical field:
The invention belongs to the microbial pesticide technical field, relate to a kind of preparation method who modifies cytidine vegetable oil suspending agent.
Background technology:
Nucleoside antibiotic is the important antibiotic of a class, they are large class compounds to nucleosides and nucleotide structure modification, take nucleosides as its common parent nucleus, have antibacterium, antimycotic, anti-trypanosome, antitumor, hoe up weeds, the biologically active of the wider range such as desinsection, enhancing immunity.The difference of different nucleoside antibiotics is the side-chain radical beyond parent nucleus.On agricultural, the nucleoside antibiotic of application mainly contains blasticidin S (Blasticidin S) and Polyoxin (Polyoxins).Chemical modification cytidine element for side chain is-C
4H
8ClO
9Nitrogen replace the cytidine element.
Many important antibiotic, as chloramphenicol (chloramphenicol), 7-duomycin (7-chlotetracycline), vancomycin (vancomycin) etc. are all halide.Although the type of halogen atom, quantity and position are on compound, bioactive impact does not have specific rule, and some halide is compared with corresponding non-halide, and halogenation can strengthen its biologically active.As, the antifungal activity of 2-chlorine pyrrolnitrin only has 10% of pyrrolnitrin (containing two chlorine atoms); With it, containing chlorine derivative, compare, not chloride butterfly mycin does not have antibacterial activity.
N-normal-butyl caprolactam is a kind of novel penetrating agent, with a kind of novel, efficient, safe osmotic absorption promoter azone at present commonly used be the material of a series of structural similarities, but its facilitation that some agricultural chemicals is infiltrated to some insect has even surpassed azone, and its synthetic cost is much lower than azone, solved due to price restriction in the agricultural extension application to azone.It all has and significantly helps the effect of oozing hydrophily and lipophilicity compound, and outstanding feature is nontoxic, little to skin irritation.
Oil-suspending agent is the high dispersive that forms in non-water system dispersate of one or more pesticide active ingredients, stable suspension system.Compare with formulations such as aqueous suspension agent, wetting powder, water dispersible granules, there is the advantages such as good penetrability, adhesiveness are strong, anti-evaporating, storage endurance.
Summary of the invention:
The purpose of this invention is to provide a kind of modification cytidine element-N-normal-butyl hexanoyl lactone suspending agent preparation method and application thereof.
The present invention realizes by following method:
(1) modify the preparation of cytidine element:
With streptomyces hygroscopicus not for the bacterium that sets out, medium is: corn flour 15～25g, beancake powder 20～35g, glucose 15～25g, starch 8～12g, ammonium chloride 1～5g, calcium carbonate 1～5g, magnesium sulfate 0.1～0.5g, ferrous sulfate 0.1～0.5g, sodium chloride 0.1～0.5g, sodium hydrogen phosphate 0.1～0.5g, add running water to 1000mL, through 121 ℃ of high pressure moist heat sterilization 20min.
Training method is shaking table concussion cultivation and fermentation, fermentation temperature: 25～35 ℃.
Pass through FeCl
3The coordination catalysis halogenating reaction carries out chemical modification and obtains modifying cytidine element, i.e. side chain-C fermentation, separating-purifying product
4H
8ClO
9Nitrogen replace the cytidine element.
(2) modify the preparation of cytidine element-N-normal-butyl hexanoyl lactone oil-suspending agent
Press formula rate, in mixing kettle, add modification cytidine element and oil emulsion, by high-shear emulsion machine, carry out high-shear emulsifying stirring (8000r/min), 10～15min, fully mix material; By mixed product, add thickener and surfactant to proceed high-shear emulsifying in mixing kettle and stir (8000r/min), 10～15min, the product obtained adds N-normal-butyl hexanoyl lactone again, carry out last high-shear emulsifying and stir (8000r/min), 10～15min, obtain modifying cytidine element-N-normal-butyl hexanoyl lactone oil-suspending agent.
Each material mass percentage: modify the cytidine element: N-normal-butyl hexanoyl lactone: surfactant: thickener: solvent naphtha=1～10%:0.1～3%:0.3～7%:1～10%: complement to 100%.
Surfactant: neopelex, castor oil polyoxyethylene ether
Thickener: octenyl sodium starch, sodium carboxymethylcellulose
Solvent naphtha: rapeseed oil, soybean oil
Preparation technology of the present invention is simple, and product has the advantages such as synergy, good penetrability, adhesiveness are strong, anti-evaporating, has good industrial applications prospect.
Embodiment
Below in conjunction with specific embodiment, the invention will be further elaborated, but be not limited to these specific embodiments, and all embodiment are all by above-mentioned operating procedure operation.
Embodiment 1:
The present embodiment is the preparation of modifying the cytidine element.
Bacterial strain: the S510 bacterial strain that streptomyces hygroscopicus Hainan mutation S101 bacterial strain of take obtains after natural separation is starting strain.
Medium: corn flour 20g, beancake powder 25g, glucose 18g, starch 10g, ammonium chloride 3g, calcium carbonate 3g, magnesium sulfate 0.3, ferrous sulfate 0.3, sodium chloride 0.3g, sodium hydrogen phosphate 0.3g, add running water to 1000mL.Through 121 ℃ of high pressure moist heat sterilization 20min.
Fermented and cultured: the shaking table concussion is cultivated, and rotating speed is 220 rev/mins, fermentation temperature: 28 ℃, and tank pressure 0.12MPa, throughput 1:0.5, fermentation time 72h.
Tunning separates and purifying: the zymotic fluid extraction, with Sephadex G-25 column chromatography, water elution, eluent is (COSMOSIL C18 Econopak post after HPLC detects, mobile phase 0.03% trifluoroacetic acid aqueous solution, flow velocity 0.4mL/min, ultraviolet detects wavelength 220nm), the key component content that retention time wherein is about to 5.5min merges respectively in 75～85% and 60～75% part, then can obtain first separator after vacuum cooling drying.Content again through a normal pressure column chromatography, can bring up to 80～85% at 60～75% primary extract by purity, merges the content of twice gained at the sample more than 75%, with the HPLC semi-preparative column, is prepared, and finally can obtain the elaboration that purity is 90.12%.By elaboration solution cold dry after, the gained micro-yellow powder is side chain-C
4H
9O
9Nitrogen replace the cytidine element.
Chemical modification: with side chain-C
4H
9O
9Nitrogen replace the cytidine element and KCl is raw material, take n-butanol as solvent, FeCl
3For catalyzer, by the coordination catalysis halogenating reaction, prepare band side chain-C
4H
8ClO
9Nitrogen replace the cytidine element.Reaction condition is: side chain-C
4H
9O
9Nitrogen replace cytidine element: KCl:FeCl
3(mol ratio)=20:40:3, the consumption of solvent, n-butanol is every mole of side chain-C
4H
9O
9Nitrogen replace cytidine element 40ml, reaction temperature is 120 ℃.
Embodiment 2:
The present embodiment is the preparation of modifying cytidine element-N-normal-butyl hexanoyl lactone oil-suspending agent 1.
Press formula rate, in mixing kettle, add modification cytidine element and oil emulsion, by high-shear emulsion machine, carry out high-shear emulsifying stirring (8000r/min), 10～15min, fully mix material; By mixed product, add thickener and surfactant to proceed high-shear emulsifying in mixing kettle and stir (8000r/min), 10～15min, the product obtained adds N-normal-butyl hexanoyl lactone again, carry out last high-shear emulsifying and stir (8000r/min), 10～15min, obtain modifying cytidine element-N-normal-butyl hexanoyl lactone oil-suspending agent.
Each material mass percentage: modify the cytidine element: N-normal-butyl hexanoyl lactone: surfactant: thickener: solvent naphtha=2.5%:0.1%:6%:5%: complement to 100%.
Surfactant: neopelex
Thickener: octenyl sodium starch
Solvent naphtha: rapeseed oil
Embodiment 3:
The present embodiment is the preparation of modifying cytidine element-N-normal-butyl hexanoyl lactone oil-suspending agent 2.
Press formula rate, in mixing kettle, add modification cytidine element and oil emulsion, by high-shear emulsion machine, carry out high-shear emulsifying stirring (8000r/min), 10～15min, fully mix material; By mixed product, add thickener and surfactant to proceed high-shear emulsifying in mixing kettle and stir (8000r/min), 10～15min, the product obtained adds N-normal-butyl hexanoyl lactone again, carry out last high-shear emulsifying and stir (8000r/min), 10～15min, obtain modifying cytidine element-N-normal-butyl hexanoyl lactone oil-suspending agent.
Each material mass percentage: modify the cytidine element: N-normal-butyl hexanoyl lactone: surfactant: thickener: solvent naphtha=8%:3%:7%:9%: complement to 100%.
Surfactant: PEG-4000
Thickener: organobentonite
Solvent naphtha: paraffin oil
Embodiment 4:
The present embodiment is the application of modifying cytidine element-N-normal-butyl hexanoyl lactone oil-suspending agent 1.
(1) prevent and treat cladosporium leaf and fruit mould of tomato: leaf mold is one of common important disease of vegetable growing tomato, belong to the fungal disease that Deuteromycotina Fulvia fulva (Fulvia fulva (looke) cif) causes, have the advantages that intermittently break out, can have a strong impact on tomato yield and quality, cause income to descend.Use 350 g/acres of this mixtures to be watered spray even, after medicine, 7 days control efficiency reach 91%.
(2) watermelon blight is the destructive disease of watermelon, claims again dead arm, walks that rattan is dead, wilt disease etc., the melon-fruit-like vegetables such as main harm watermelon, muskmelon, cucumber.Do not adopt the field of graft technology, the general incidence of disease, in 5% left and right, can reach more than 50% when serious, even total crop failure.Use 400 g/acres of this mixtures to be watered spray even, after medicine, 5 days control efficiency reach 84.2%.
(3) grey speck of soybean ［ Cercosporidiumsojtnum(Hara.) LiuetGuo ］ is a typical epidemic disease, the Three River Plain and middle part Suihua Area at Eastern Heilongjiang Province occur serious, within popular year, cause Severe Reduction, be one of the maximum disease that causes harm in current Heilongjiang soybean production.Cercospora Sojina Hara infects soybean to be caused the underproduction except in leaf, stem, pod section, producing scab, more seriously causes Seed mottling.According to investigations, the time infected seed that is very popular can reach more than 50%, and the infected seed Oil content and Protein content descends respectively 2.9% and 1.2%.Use 500 g/acres of this mixtures to be watered spray even, after medicine, 8 days control efficiency reach 92.7%.
Claims (4)
1. modify cytidine vegetable oil suspending agent preparation method for one kind, it is characterized in that: chemical modification cytidine element is bactericidal active ingredient, N-normal-butyl hexanoyl lactone is penetration enhancer, and all the other are in agricultural chemicals, to allow to use and the acceptable auxiliary element, comprise surfactant, thickener and solvent naphtha.
2. method according to claim 1, is characterized in that each constituent mass percentage is: chemical modification cytidine element: N-normal-butyl hexanoyl lactone: surfactant: thickener: solvent naphtha=1～10%:0.1～3%:0.3～7%:1～10%: complement to 100%.
3. method according to claim 1 and 2, is characterized in that, each constituent mass percentage is preferred: chemical modification cytidine element: N-normal-butyl hexanoyl lactone: surfactant: thickener: solvent naphtha=2.5%:0.1%:6%:5%: complement to 100%.
4. method according to claim 1, is characterized in that chemical modification cytidine element is for side chain-C
4H
8ClO
9Nitrogen replace the cytidine element, its preparation method comprises:
(1) with streptomyces hygroscopicus not for the bacterium that sets out, fermented and cultured in medium,
(2) separation, purified fermentation broth,
(3) carry out chemical modification with the coordination catalysis halogenating reaction again after the separation of fermentative broth purifying, obtain chemical modification cytidine element.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101618996A CN103416437A (en) | 2012-05-23 | 2012-05-23 | Preparation method for modified cytidine antibiotic oil suspension |
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|---|---|---|---|
| CN2012101618996A CN103416437A (en) | 2012-05-23 | 2012-05-23 | Preparation method for modified cytidine antibiotic oil suspension |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436787A (en) * | 2002-02-04 | 2003-08-20 | 中国农业科学院植物保护研究所 | Antibiotic and its prepn and application |
| CN102373171A (en) * | 2011-11-01 | 2012-03-14 | 中国科学院南海海洋研究所 | Nucleoside antibiotic A201A superior strain and construction method thereof |
-
2012
- 2012-05-23 CN CN2012101618996A patent/CN103416437A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436787A (en) * | 2002-02-04 | 2003-08-20 | 中国农业科学院植物保护研究所 | Antibiotic and its prepn and application |
| CN102373171A (en) * | 2011-11-01 | 2012-03-14 | 中国科学院南海海洋研究所 | Nucleoside antibiotic A201A superior strain and construction method thereof |
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Application publication date: 20131204 |