CN105104391A - Bactericidal composition containing berberine and oxine-copper - Google Patents
Bactericidal composition containing berberine and oxine-copper Download PDFInfo
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- CN105104391A CN105104391A CN201510530832.9A CN201510530832A CN105104391A CN 105104391 A CN105104391 A CN 105104391A CN 201510530832 A CN201510530832 A CN 201510530832A CN 105104391 A CN105104391 A CN 105104391A
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Abstract
The invention discloses a bactericidal composition containing berberine and oxine-copper. The bactericidal composition is prepared by compounding the active ingredients including berberine and oxine-copper in a mass ratio of (1 to 9)-(9 to 1). The bactericidal composition can be prepared into conventional dosage forms in the pesticide science, such as wettable powder, water dispersible granules, suspensions, microcapsule suspensions, granules or emulsion in water. The bactericidal composition has the advantages of high efficiency, little environmental pollution, capability of delaying the resistance of germs to drugs, and the like, and can be used for controlling diseases of various crops, especially rice bacterial leaf streak.
Description
Technical field
The invention belongs to technical field of pesticide, relate to composition pesticide, relate to a kind of bactericidal composition containing jamaicin and copper 8-hydroxyquinolinate specifically.
Background technology
In the whole process of growth of crop, be faced with the threat of the pests such as numerous such as disease, worm, grass, wherein disease, especially fungal disease, because it is of a great variety, complicated symptoms, propagation rapidly, the feature such as the serious and plyability generation of harm makes its difficulty of prevention and cure strengthen, and forms grave danger to crop yield and quality.In agricultural production process, in order to reduce the loss because fungal disease causes, chemical control is one of current comparatively significant means, but due to for a long time, unicity, continuity, repeatability etc. not Scientific Usage of Drugs means have caused many pathogens to produce resistance in various degree to the medicament of current use, and it is reported, due to this unscientific medication means, the resistance generation time of various medicament shortens year by year, causes the significantly increase of cost accounting, Environmental costs, medicament R&D costs.Based on this present situation, existing basis is improved effect of drugs for the comparatively cost-effective means that solve the problem.
Jamaicin is also known as berberine.A common morphinane alkaloid, molecular formula C
20h
18nO
4, its structure is as follows:
Jamaicin is present in many plants of four sections ten genus such as Berberidaceae.M.-E. Xia Waliai in 1826 and G. Pei Ertan obtain first from Xanthoxylonclava bark.Jamaicin is a kind of quartermary ammonium alkaloids.Yellow needle-like crystals can be separated out from ether; Fusing point 145 DEG C; Water-soluble, be insoluble in benzene, EC.Be mainly used in enteric infection such as treatment gastroenteritis, bacillary dysentery etc., eye conjunctivitis, otitis media suppurative etc. effectively.Recently also find that this product has blocking-up alpha-receptor, antiarrhythmic effect.
Jamaicin is to hemolytic streptococcus, staphylococcus aureus, gonococcus and Fu Shi, Shigella shigae etc. all have antibacterial action, and have the phagocytosis of enhancing leukocyte, also there is inhibitory action in various degree to tubercle bacillus, plague bacillus, also have suppression effectiveness to the amoeba bacterium of rat.Jamaicin has anti-curare effect in animals, and has peripheral step-down and refrigeration function.The hydrochloride (being commonly called as Halomine) of jamaicin has been widely used in treatment gastroenteritis, bacillary dysentery etc., also has certain curative effect to pulmonary tuberculosis, scarlet fever, acute tonsillitis and respiratory tract infection.The traditional Chinese medical science is commonly used the coptis, golden cypress, barberry and Chinese mahonia etc. and is made clearing heat and detoxicating medicine, wherein principle active component and jamaicin.
Copper 8-hydroxyquinolinate, for clamping together state organic copper bactericide, can be prevented and treated because of the disease caused by bacterium and all kinds of fungi; Registration crop and disease are the peronospora tabacinas of lichee, use extension rate for 1000-1500 times; Other disease that can prevent and treat: downy mildew of garpe and anthrachose of grape; The downy mildew of cucumber, anthracnose and bacterial angular leaf spot; The ocean downy mildew of muskmelon, anthracnose and bacterial angular leaf spot; The black spot of pears, scab and ring spot; The downy mildew of watermelon, pumpkin and muskmelon, anthracnose; The black rot of cabbage; The rot of lettuce, bacterial angular leaf spot, soft rot and downy mildew etc.
The combination of active principles of different agricultural chemicals is made agricultural chemicals, is current development novel pesticide and the one of preventing and treating agriculturally resistance germ effectively and efficiently mode.After the pestsides synthesis of different cultivars, usually show three kinds of type of action: summation action, synergistic effect and antagonism.Compound synergic is well filled a prescription, and can significantly improve actual control efficiency, and reducing the usage amount of agricultural chemicals, thus delay the drug-fast generation speed of germ widely, is the important means of integrated control disease.
Synergistic bactericidal composition not only can improve preventive effect greatly, reduces dosage, reduces costs, and phytopathogen can also be avoided to produce the generation speed of resistance and delaying drug resistance simultaneously, be solve current agricultural chemicals alone time resistance and a kind of effective means of Cost Problems.Therefore, develop and have the bactericidal composition of synergistic effect significant to plant disease.
The information being disclosed in this background technology part is only intended to increase the understanding to general background of the present invention, and should not be regarded as admitting or imply in any form that this information structure has been prior art that persons skilled in the art are known.
Summary of the invention
The object of the invention is to overcome the dosing that above-mentioned single bactericide exists large, environmental pollution is serious, germ resistance produces the shortcomings such as speed is fast and provide a kind of efficient, safe bactericidal composition containing jamaicin and copper 8-hydroxyquinolinate.Under optimal proportion, composition has notable synergistic effect, ensureing the usage amount reducing medicament under optimum preventive effect, reducing costs, reducing the harm to environment, and is of value to and delays the drug-fast generation of germ.
Technical scheme provided by the invention is:
Contain a bactericidal composition for jamaicin and copper 8-hydroxyquinolinate, it is that jamaicin and oxine-copper composite form by active ingredient.
As preferably, the mass ratio of described jamaicin and copper 8-hydroxyquinolinate is 1:9-9:1.
As preferably, the mass ratio of described jamaicin and copper 8-hydroxyquinolinate is 9:1.
As preferably, the mass ratio of described jamaicin and copper 8-hydroxyquinolinate is 7:3.
Present invention also offers a kind of pesticidal preparations comprising described bactericidal composition, the quality of described jamaicin and copper 8-hydroxyquinolinate accounts for the 1-90% of pesticidal preparations gross mass, and surplus is acceptable auxiliary element auxiliary agent, solvent or filler on agricultural chemicals.
As preferably, the formulation of described pesticidal preparations is wetting powder, water dispersible granules, suspending agent, microcapsule suspending agent, granule or aqueous emulsion.
The auxiliary agent used in described pesticidal preparations comprises solvent, dispersant, emulsifier, stabilizing agent, antifreezing agent, film forming agent, wetting agent etc. and other is of value to the known substance that active ingredient is stablized in the formulation and drug effect plays, all various compositions that are conventional in pesticidal preparations or permission use, be not particularly limited, concrete composition and consumption are determined by simple experiment according to recipe requirements.
Bactericidal composition of the present invention control paddy rice, wheat, vegetables, fruit tree etc. apply in multiple diseases on crop, be particularly useful for control bacterial leaf streak of rice disease.
Bactericidal composition of the present invention also can be used by common method, as cast, spraying, scatters, and its amount of application is with weather condition or crop condition change.
Compared with prior art, the present invention has following beneficial effect:
1. bactericidal composition of the present invention is made up of the active ingredient that two kinds of mechanism of action are different, has obvious synergistic function, improve control efficiency after mixture to Xanthomonas campestris pv. Oryzicola, is also conducive to overcoming and delay the drug-fast generation of germ simultaneously.
2. present composition medicament mixture decreases dosage, thus reduces cost and alleviate the pollution to environment, and safety is good, meets the security requirement of pesticidal preparations.
3. of the present invention provided bactericidal composition has good control efficiency to the disease that Xanthomonas campestris pv. Oryzicola causes.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described in detail, but is to be understood that protection scope of the present invention not by the restriction of embodiment.
Clearly represent unless otherwise other, otherwise in whole specification and claims, term " comprise " or its conversion as " comprising " or " including " etc. by be understood to include the element of stating or part, and do not get rid of other element or other part.
Inventor is by a large amount of screening tests, and discovery jamaicin and oxine-copper composite combine has synergistic function significantly to Xanthomonas campestris pv. Oryzicola, and is not only the simple addition of two kinds of medicaments, and this can know from following biologicall test example and find out.
biologicall test example 1: jamaicin and oxine-copper composite are to the Toxicity Determination of Xanthomonas campestris pv. Oryzicola
Subjects: the xanthomonas oryzae pv. oryzicola picking up from field
Test method: reagent agent is made into certain density mother liquor, then be mixed with 5 ~ 6 concentration in the ratio of setting with water dilution, if clear water is contrast, adding containing germ concentration is respectively 1 × 10
7in the NB culture fluid of cfu/mL, in 28 DEG C, in the constant-temperature table of 130r/m, cultivate after 24 hours, utilize UV detector to measure absorbance under 600nm wavelength, calculate bacteriostasis rate by formula 2-3.Drug concentration is converted into logarithm, and bacteriostasis rate is converted into probability value and carries out linear regression, calculates virulence regression equation and EC50 value (HalfMaximalEffectiveConcentration, EC50).
This test is carried out with reference to the way to the best synergistic formula screening of agriculture chemical compounding such as Chen Li (2000).
First, malicious factorization method is altogether used a large amount of compounded combination to be carried out to the qualitative screening of synergistic effect.Suppose that the antibacterial middle concentration through toxicity test A, B two single dose is respectively a and b, then select 9 proportionings with when malicious factorization method evaluates the synergistic effect of A+B mixture altogether, these 9 proportionings are ten Along ents of additive effect line in isoboles, can be expressed as a/9b, 2a/8b, 3a/7b, 4a/6b, 5a/5b, 6a/4b, 7a/3b, 8a/2b, 9a/b.By corresponding concentration gradient order by A, B two single dose by certain volume ratio 1:9,1:4,3:7,2:3,1:1,3:2,7:3,4:1,9:1 mixing, obtain the concentration gradient of whole proportioning mixture.Measure each matched proportion density gradient to the inhibitory action of bacterial leaf streak of rice by OD value method, find out antibacterial compatibility and enter next step screening preferably.
To the compounded combination having synergistic effect, then carry out quantitative analysis by the abundant method of Sun Yun, acquired results obtains co-toxicity coefficient and nitrate enhancement according to Sun & Johnson method.Processing method is: the concentration of single dose and mixture is converted into logarithm, and bacteriostasis rate is converted into probability value and carries out linear regression, obtains EC50 value.The co-toxicity coefficient (CTC) of mixed agent, according to following formulae discovery:
Mixed agent co-toxicity coefficient (CTC)=[actual measurement mixture toxicity index (ATI)/theoretical toxicity index (TTI)] × 100
Mixture actual measurement toxicity index (ATI)=(EC50 of the EC50/ reagent agent of standard agent) × 100
Theoretical toxicity index (the TTI)=A agent toxicity index × content of A agent in mixture (the %)+B agent toxicity index × content of B agent in mixture (%) of mixture
(CTC)≤120 are synergistic effect to the co-toxicity coefficient of mixture; CTC≤80 are antagonism; 80 ﹤ CTC ﹤ 120 are summation action.
Toxicity test the results are shown in following table 1 and table 2.
Table 1 jamaicin and copper 8-hydroxyquinolinate are to the virulence of xanthomonas oryzae pv. oryzicola
Table 2 jamaicin and oxine-copper composite are to the Toxicity Determination result of Xanthomonas campestris pv. Oryzicola
| Process | EC50(μg/ml) | ATI | TTI | CTC |
| Jamaicin | 2.9008 | 100.00 | —— | —— |
| Copper 8-hydroxyquinolinate | 0.9705 | 298.90 | —— | —— |
| Jamaicin 1: copper 8-hydroxyquinolinate 9 | 0.85 | 341.27 | 279.01 | 122.32 |
| Jamaicin 2: copper 8-hydroxyquinolinate 8 | 0.91 | 318.77 | 259.12 | 123.02 |
| Jamaicin 3: copper 8-hydroxyquinolinate 7 | 1.01 | 287.21 | 239.23 | 120.06 |
| Jamaicin 4: copper 8-hydroxyquinolinate 6 | 1.04 | 278.92 | 219.34 | 127.17 |
| Jamaicin 1: copper 8-hydroxyquinolinate 1 | 1.12 | 259.00 | 199.45 | 129.86 |
| Jamaicin 6: copper 8-hydroxyquinolinate 4 | 1.31 | 221.44 | 179.56 | 123.32 |
| Jamaicin 7: copper 8-hydroxyquinolinate 3 | 1.18 | 245.83 | 159.67 | 153.96 |
| Jamaicin 8: copper 8-hydroxyquinolinate 2 | 1.53 | 189.59 | 139.78 | 135.64 |
| Jamaicin 9: copper 8-hydroxyquinolinate 1 | 1.5 | 193.39 | 119.89 | 161.31 |
As shown in table 1, the mass ratio of bactericidal composition Berberine of the present invention and copper 8-hydroxyquinolinate is within the scope of 1:9-9:1, and co-toxicity coefficient is all greater than 120, and namely the biologically active of said composition to Xanthomonas campestris pv. Oryzicola all shows as synergistic effect; Especially, when the mass ratio of jamaicin and copper 8-hydroxyquinolinate is at 9:1 or 7:3, synergistic effect is more obvious.
Fungicidal composition of the present invention can be prepared into any one formulation of applicable agricultural use by known method, reasonable formulation is wetting powder, water dispersible granules, suspending agent, microcapsule suspending agent, granule or aqueous emulsion.
In order to make object of the present invention, technical scheme and advantage clearly understand, the following specific embodiment of the present invention is described, but the present invention is limited to absolutely not these examples.The following stated is only the good embodiment of the present invention, only in order to explain the present invention, therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.In all formulas, percentage is all weight percentage.The processing technology of each preparation of the present composition is prior art, can change to some extent according to different situations.
embodiment 1: 1% little Bo Jian ﹒ copper 8-hydroxyquinolinate granule
In jamaicin and copper 8-hydroxyquinolinate, add dimethylbenzene, then they are fully stirred, make them dissolve completely; Under agitation, in system, slowly add propane diols, fully stir 30 minutes, make them dissolve completely, form stable solution.
First 12-60 object zeolite is added in mixer, then the solution of aforementioned stable is added wherein, mix 30 minutes, through screening, detect qualified after can obtain 1% little Bo Jian ﹒ copper 8-hydroxyquinolinate granule.
embodiment 2: 10% little Bo Jian ﹒ copper 8-hydroxyquinolinate microcapsule suspending agent
By rosickyite bacterium ester 2%, copper 8-hydroxyquinolinate 8%, is dissolved in 5% dimethylbenzene, suction tributyl phosphate 0.3% again, carboxymethyl cellulose 2.4%, sodium alginate 2.7%, shears 30 minutes in high shear still high speed, add 20% urea resin prepolymer, 2000 revs/min are stirred lower elevated cure 60 minutes, add deionized water afterwards, 4.5% dinaphthylmethanedisulfonic acid sodium, 1.8% bentonite, stir to obtain 10% jamaicin copper 8-hydroxyquinolinate microcapsule suspending agent.
embodiment 3: 16% little Bo Jian ﹒ copper 8-hydroxyquinolinate aqueous emulsion
By above-mentioned formula Central Plains medicine, solvent, cosolvent emulsifiers dissolve uniformly oil phase; Mixed by the insecticides adjuvants such as part water, antifreezing agent, defoamer and form uniform aqueous phase, oil phase adds aqueous phase in clipper, carries out high speed shear, and adds remaining water, shears 30 minutes, mixes.Namely 16% little Bo Jian ﹒ copper 8-hydroxyquinolinate aqueous emulsion is made.
embodiment 4: 21% little Bo Jian ﹒ copper 8-hydroxyquinolinate suspending agent
A component such as active component, dispersant, thickener, wetting agent, antifreeze and water is mixed in the ratio of formula, after high speed shear, obtains 21% little Bo Jian ﹒ copper 8-hydroxyquinolinate suspending agent.
embodiment 5: 60% little Bo Jian ﹒ copper 8-hydroxyquinolinate wetting powder
Active component and various auxiliary agent and filler etc. are mixed in the ratio of formula, after ultra-fine pulverizer disintegrating, obtains 60% little Bo Jian ﹒ copper 8-hydroxyquinolinate wetting powder.
embodiment 6: 90% little Bo Jian ﹒ copper 8-hydroxyquinolinate water dispersible granules
Active component and various auxiliary agent and filler etc. are mixed in the ratio of formula, after air-flow crushing, obtains wetting powder, then add a certain amount of water mixing extruder grain, after drying screening, obtain 90% little Bo Jian ﹒ copper 8-hydroxyquinolinate water dispersible granules.
embodiment 7: 55% little Bo Jian ﹒ copper 8-hydroxyquinolinate wetting powder
Active component and various auxiliary agent and filler etc. are mixed in the ratio of formula, after ultra-fine pulverizer disintegrating, obtains 55% little Bo Jian ﹒ copper 8-hydroxyquinolinate wetting powder.
embodiment 8: 21% little Bo Jian ﹒ copper 8-hydroxyquinolinate microcapsule suspending agent
By rosickyite bacterium ester 20%, copper 8-hydroxyquinolinate 1%, is dissolved in 5% dimethylbenzene, suction tributyl phosphate 0.3% again, carboxymethyl cellulose 2.4%, sodium alginate 2.7%, shears 30 minutes in high shear still high speed, add 20% urea resin prepolymer, 2000 revs/min are stirred lower elevated cure 60 minutes, add deionized water afterwards, 4.5% dinaphthylmethanedisulfonic acid sodium, 1.8% bentonite, stir to obtain 21% jamaicin copper 8-hydroxyquinolinate microcapsule suspending agent.
embodiment 9: 41% little Bo Jian ﹒ copper 8-hydroxyquinolinate water dispersible granules
Active component and various auxiliary agent and filler etc. are mixed in the ratio of formula, after air-flow crushing, obtains wetting powder, then add a certain amount of water mixing extruder grain, after drying screening, obtain 41% little Bo Jian ﹒ copper 8-hydroxyquinolinate water dispersible granules.
embodiment 10: 61% little Bo Jian ﹒ copper 8-hydroxyquinolinate water dispersible granules
Active component and various auxiliary agent and filler etc. are mixed in the ratio of formula, after air-flow crushing, obtains wetting powder, then add a certain amount of water mixing extruder grain, after drying screening, obtain 61% little Bo Jian ﹒ copper 8-hydroxyquinolinate water dispersible granules.
embodiment 11: 81% little Bo Jian ﹒ copper 8-hydroxyquinolinate wetting powder
Active component and various auxiliary agent and filler etc. are mixed in the ratio of formula, after ultra-fine pulverizer disintegrating, obtains 81% little Bo Jian ﹒ copper 8-hydroxyquinolinate wetting powder.
embodiment 12: 6% little Bo Jian ﹒ copper 8-hydroxyquinolinate granule
In jamaicin and copper 8-hydroxyquinolinate, add dimethylbenzene, then they are fully stirred, make them dissolve completely; Under agitation, in system, slowly add propane diols, fully stir 30 minutes, make them dissolve completely, form stable solution.
First 12-60 object zeolite is added in mixer, then the solution of aforementioned stable is added wherein, mix 30 minutes, through screening, detect qualified after can obtain 6% little Bo Jian ﹒ copper 8-hydroxyquinolinate granule.
embodiment 13: 70% little Bo Jian ﹒ copper 8-hydroxyquinolinate water dispersible granules
Active component and various auxiliary agent and filler etc. are mixed in the ratio of formula, after air-flow crushing, obtains wetting powder, then add a certain amount of water mixing extruder grain, after drying screening, obtain 70% little Bo Jian ﹒ copper 8-hydroxyquinolinate water dispersible granules.
embodiment 14: 30% little Bo Jian ﹒ copper 8-hydroxyquinolinate suspending agent
A component such as active component, dispersant, thickener, wetting agent, antifreeze and water is mixed in the ratio of formula, after high speed shear, obtains 30% little Bo Jian ﹒ copper 8-hydroxyquinolinate suspending agent.
embodiment 15: 25% little Bo Jian ﹒ copper 8-hydroxyquinolinate aqueous emulsion
By above-mentioned formula Central Plains medicine, solvent, cosolvent emulsifiers dissolve uniformly oil phase; Mixed by the insecticides adjuvants such as part water, antifreezing agent, defoamer and form uniform aqueous phase, oil phase adds aqueous phase in clipper, carries out high speed shear, and adds remaining water, shears 30 minutes, mixes.Namely 25% little Bo Jian ﹒ copper 8-hydroxyquinolinate aqueous emulsion is made.
embodiment 15: 1% little Bo Jian ﹒ copper 8-hydroxyquinolinate microemulsion
Former medicine is dissolved in organic solvent and cosolvent, to be dissolved completely after, add emulsifier, stir, make it to form homogeneous mixed system, then in system, drip aqueous phase, stir and form transparent w/o type micro emulsion, stir in 55 DEG C of Water Under baths again, make it to form O/W type micro emulsion, namely make 1% little Bo Jian ﹒ copper 8-hydroxyquinolinate microemulsion.
field efficacy embodiment 1: 1% jamaicin copper 8-hydroxyquinolinate microemulsion (7:3) is to the control efficiency of bacterial leaf streak of rice
With agricultural chemicals single dose 1% jamaicin microemulsion and 33.5% copper 8-hydroxyquinolinate wetting powder as a comparison, by 1% jamaicin copper 8-hydroxyquinolinate microemulsion (7:3) dispenser process prepared by embodiment 15, in 15d " Invest, Then Investigate " control efficiency, the results are shown in Table 3.
Table 31% jamaicin copper 8-hydroxyquinolinate microemulsion is to the control efficiency of bacterial leaf streak of rice
As can be seen from Table 3, the control efficiency of built agent when 0.5g/L is best, but suitable with the preventive effect of 0.05g/L; The preventive effect of built agent 0.05g/L is suitable with the preventive effect contrasting medicament 20% Yekuzuo wetting powder active ingredient 0.44g/L, and is significantly higher than the preventive effect of copper 8-hydroxyquinolinate single dose.
In sum, have obvious synergistic function, improve control efficiency after bactericidal composition mixture of the present invention, be also conducive to overcoming and delay the drug-fast generation of germ, bactericidal composition of the present invention has good commercial promise simultaneously.
The aforementioned description to concrete exemplary of the present invention is to illustrate and the object of illustration.These descriptions not want the present invention to be defined as disclosed precise forms, and obviously, according to above-mentioned instruction, can much change and change.The object selected exemplary embodiment and describe is to explain certain principles of the present invention and practical application thereof, thus those skilled in the art can be realized and utilize various different exemplary of the present invention and various different selection and change.Scope of the present invention is intended to limited by claims and equivalents thereof.
Claims (6)
1. contain a bactericidal composition for jamaicin and copper 8-hydroxyquinolinate, it is characterized in that: it is that jamaicin and oxine-copper composite form by active ingredient.
2. bactericidal composition according to claim 1, is characterized in that: the mass ratio of described jamaicin and copper 8-hydroxyquinolinate is 1:9-9:1.
3. bactericidal composition according to claim 2, is characterized in that: the mass ratio of described jamaicin and copper 8-hydroxyquinolinate is 9:1.
4. bactericidal composition according to claim 2, is characterized in that: the mass ratio of described jamaicin and copper 8-hydroxyquinolinate is 7:3.
5. one kind comprises the pesticidal preparations of the arbitrary described bactericidal composition of Claims 1-4, it is characterized in that: the quality of described jamaicin and copper 8-hydroxyquinolinate accounts for the 1-90% of pesticidal preparations gross mass, surplus is acceptable auxiliary element auxiliary agent, solvent or filler on agricultural chemicals.
6. pesticidal preparations according to claim 5, is characterized in that: the formulation of described pesticidal preparations is wetting powder, water dispersible granules, suspending agent, microcapsule suspending agent, granule or aqueous emulsion.
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