CN107410382A - A kind of bactericide for tobacco black shank and its preparation method and application - Google Patents
A kind of bactericide for tobacco black shank and its preparation method and application Download PDFInfo
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- CN107410382A CN107410382A CN201710823564.9A CN201710823564A CN107410382A CN 107410382 A CN107410382 A CN 107410382A CN 201710823564 A CN201710823564 A CN 201710823564A CN 107410382 A CN107410382 A CN 107410382A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/20—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom three- or four-membered rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N55/00—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/36—Rutaceae [Rue family], e.g. lime, orange, lemon, corktree or pricklyash
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Abstract
The invention discloses a kind of bactericide for tobacco black shank, include phellodendron extract 90% 96%, methyl-silicone oil 3% 9% and epoxychloropropane no more than 1% by mass fraction, the phellodendron extract is made by golden cypress through ethanol reflux extraction.Through field test, to the prevention effect of tobacco black shank more than 80%, positive effect, in the balck shank of preventing and treating tobacco crop field efficiently, low toxicity and do not pollute the environment, for improving quality of tobacco, ensureing its security and keep ecological balance with highly important practice significance.Present invention also offers a kind of preparation method of the bactericide for tobacco black shank, the effect of twice extraction process is unique, has irreplaceability, and technique is simple, time saving and energy saving, easily production, possesses the possibility produced in enormous quantities.
Description
Technical field
The invention belongs to field of plant disease control, more particularly to a kind of bactericide and its preparation for tobacco black shank
Methods and applications.
Background technology
Tobacco black shank Phytophthoraparasitica var.nicotianae (Vann Breda de Haan) are
One of most destructive Major Diseases on tobacco leaf production, it is 5%-12% in Chinese tobacco average attack rate, serious field hair
Sick rate is up to 75%, and balck shank endangers cigarette strain health once occurring to spread rapidly, or even causes vega to have no harvest, serious shadow
Leaf tobacco production is rung, huge economic loss is caused to tobacco leaf production.
At present, tobacco black shank uses Agro-chemicals control more, the use of chemical pesticide, not only can be to cigarette strain strong in itself
Kang Zaocheng is had a strong impact on, and various harmful levels of pathogens can be caused to produce drug resistance, increases the follow-up difficulty of prevention and cure that disease occurs, more
The serious is a large amount of uses of chemical agent can make to contain chemical agent residue in tobacco leaf, further endanger health of people, dirty
Environment is contaminated, destroys the ecological balance.Important component of the botanical pesticide as biological pesticide, have efficient, degradable, not dirty
The advantages of contaminating environment, low-residual, high selectivity, therefore, is developed into efficient, less toxic, wide spectrum using plant extracts, is not likely to produce
The new type bactericide preventing and treating tobacco black shank of resistance is the new direction of those skilled in the art's research.However, currently used for tobacco
The plant source sterilization pesticide of balck shank still has following deficiency：1) pure Extracts from Plant Recourses medicament, its composition is by crop field ring
The influence in border and easily degrade, especially in natural crop field environment, meet that light is more degradable, i.e. failure is fast, and drug effect is unstable；2)
If rain washes away or dew dilution, effect are worse.
Therefore, it is badly in need of studying a kind of efficacy stability, while the adhesive force increase of medicament, is diluted by rain drop erosion or dew
Influence it is relatively fewer, and prevention effect multiplication the bactericide for tobacco black shank.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, there is provided one
Kind of efficacy stability, while the adhesive force increase of medicament, relatively fewer, and prevention effect is influenceed by rain drop erosion or dew dilution
Bactericide for tobacco black shank of multiplication and its preparation method and application.
In order to solve the above technical problems, technical scheme proposed by the present invention is a kind of sterilization for tobacco black shank of offer
Agent, by epoxy chloropropionate of the mass fraction including phellodendron extract 90%-96%, methyl-silicone oil 3%-9% and no more than 1%
Alkane.
Above-mentioned bactericide, it is preferred that by mass fraction by phellodendron extract 96%, methyl-silicone oil 3% and epoxy chlorine
Propane 1% is formed, and the phellodendron extract is made by golden cypress through ethanol reflux extraction.
Preferably, the phellodendron extract includes at least one of jamaicin, phellodendrine and obakunone.
The vegetal inspired of the main component medicinal plant golden cypress (Phellodendron chinense Schneid.) of the present invention
State feature is preferably：Rutaceae Phellodendron broad-leaved arbor, height of tree 10-25 rice, bark is khaki or light gray, has thick cork,
It is flexible, internal layer foresythia；Berry-like drupe spheroidal, atropurpureus when ripe, there are special aroma, the fruiting period 9-10 months.Golden cypress category is warm
Temperate plant, there is stronger cold tolerance, the speed of growth is fast, there is certain cold resistance, also more drought-resistant；Distribution is wide, production
In China Hunan, Hubei, Shaanxi, Henan, Guangdong, Guangxi, Sichuan and the Northeast and other places, it can also pass through seminal propagation or plant division
Or cutting propagation carries out artificial cultivation production, it is seen that its wide material sources, convenient material drawing.Modern medicine study proves that golden cypress has
A variety of pharmacological activity such as antibacterial, anti-trichomonal, anti-inflammatory, antiulcer, anti-oxidant, antiviral, have been widely used in field of medicaments, yellow
Cypress antibiotic effective ingredient is mainly the Flavonoid substances such as the alkaloids such as jamaicin, phellodendrine and obakunone, golden cypress decoction or leaching
Agent has different degrees of bacteriostasis to common pathogenic fungus, and based on this, the present inventor utilizes the antibacterial of golden cypress, anti-inflammatory etc.
Pharmacological action, using golden cypress ethanol extract as principal component, synergist methyl-silicone oil and stabilizer epoxychloropropane are added, to develop
The bactericide for tobacco black shank of the present invention.
Methyl-silicone oil have the function that insulation, it is dust-proof, mould proof, as a kind of additive, the guarantor that medicament of the present invention can be extended
Deposit the phase, meanwhile, penetrating power of the medicine to germ can be improved, improves drug effect, and a kind of synergist.
Epoxychloropropane is a kind of organic compound, and a kind of stabilizer of oxygen carrier, has that caking property is strong, chemistry
The good characteristic of stability, a kind of additive is used as in medicament of the present invention, can increase the adhesive force of medicament, strengthen agent stability,
It is a kind of stabilizer, because it has certain toxicity, therefore concentration control is within 1%.
Based on a total technical concept, the present invention correspondingly provides a kind of preparation of the bactericide for tobacco black shank
Method, comprise the following steps：
(1) golden cypress is dried in the shade, crushes, obtain golden cypress powder, pour into ethanol solution, heating carries out first time refluxing extraction, obtained
To an extract solution；
(2) after the extract solution obtained after step (1) is filtered, ethanol solution is poured into, heating carries out second of refluxing extraction,
Obtain secondary raffinate；
(3) secondary raffinate obtained after step (2) is subjected to decompression rotary evaporation, obtains paste phellodendron extract；
(4) the paste phellodendron extract low-concentration ethanol solution obtained after step (3) is dissolved, it is molten that saturation golden cypress is made
Liquid, mixing is shaken after adding methyl-silicone oil and epoxychloropropane, that is, obtains described bactericide.
Above-mentioned preparation method, it is preferred that in the step (1), every gram of golden cypress adds 10ml ethanol solutions, ethanol solution
Volumetric concentration be 75%, heating-up temperature be 60-95 DEG C, extraction time 30-60min；In the step (2), every gram of golden cypress
5ml ethanol solutions are added, the volumetric concentration of ethanol solution is 75%, and heating-up temperature is 60-95 DEG C, extraction time 30-
60min。
Preferably, extracted in electric jacket heating and refluxing extraction device.
Preferably, in the step (3), the rotating speed of rotation turns/min for 60-75, and the heating-up temperature of evaporation is 60-75 DEG C.
Preferably, in the step (3), decompression rotary evaporation, the cryogenic temperature of vavuum pump are carried out in Rotary Evaporators
For -2.0-10 DEG C.
Preferably, in the step (4), the volumetric concentration of low-concentration ethanol solution is 5%.
Based on a total technical concept, the present invention correspondingly provides a kind of above-mentioned bactericide and prevented in crop field tobacco black shank
The application in field is controlled, the application process of the bactericide is by every plant of cigarette pouring root 500ml after 100 times of dilutions, time of application difference
7 days and group's phase, co-administer twice after being transplanted for cigarette strain.
Compared with prior art, beneficial effects of the present invention are：
1st, the present invention is used for the bactericide of tobacco black shank, is a kind of bactericide based on phellodendron extract, and golden cypress is planted
Thing distribution is wide, and easy commerial growing production, material source is wide, and composition is simple, and cost is low, while with the addition of synergist methyl silicon
The adhesive force increase of oil and stabilizer epoxychloropropane, efficacy stability, while medicament, is influenceed by rain drop erosion or dew dilution
It is relatively fewer, prevention effect multiplication, it is easier to degrade relative to chemical agent, does not remain, while also reduce other metals
The application of class chemical agent, reduces Pesticide-Polluted Soil, can be directly used for the preventing and treating of tobacco crop field balck shank；Tried through field
Test, to the prevention effect of tobacco black shank more than 80%, positive effect, in the balck shank of preventing and treating tobacco crop field efficiently, low toxicity
And do not pollute the environment, for improving quality of tobacco, ensureing its security and keep ecological balance with highly important reality
Trample meaning.
2nd, preparation method of the invention, twice extraction process is carried out to golden cypress, golden cypress powder is poured into electric jacket and is heated to reflux
Extraction element, refluxing extraction is carried out, ensure that the principal component in golden cypress is unlikely to volatilization and is lost in, obtain golden cypress and more completely extract
Liquid, then the cortex phellodendri extract Jing Guo second extraction is poured into Rotary Evaporators, carry out decompression rotation, be evaporated to paste, obtain
To paste phellodendron extract, it is easy to preserve and the accurate of compound concentration quantifies, in a word, the effect of twice extraction process is unique, tool
There is irreplaceability, and technique is simple, it is time saving and energy saving, easily production, possess the possibility produced in enormous quantities.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are the present invention
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
These accompanying drawings obtain other accompanying drawings.
Fig. 1 is the test real object figure of electric jacket heating and refluxing extraction device in embodiment 1.
Fig. 2 is the test real object figure of Rotary Evaporators in embodiment 1.
Fig. 3 is that (left side is control to this bactericide, and the right side is originally to kill with compareing indoor flat plate experiment effect comparison diagram in embodiment 1
Microbial inoculum).
Fig. 4 be this bactericide in embodiment 1 crop field tobacco black shank controlling experiment scene photo (left lateral for control, that is, spray
Apply clear water；Right lateral sprays the bactericide of the present invention).
Embodiment
For the ease of understanding the present invention, the present invention is done below in conjunction with Figure of description and preferred embodiment more complete
Face, meticulously describe, but protection scope of the present invention is not limited to specific examples below.
Unless otherwise defined, all technical terms used hereinafter are generally understood that implication phase with those skilled in the art
Together.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of bactericide for tobacco black shank of the invention, include each component of following mass fraction：Golden cypress is extracted
Thing 96%, H201 methyl-silicone oils 3% and epoxychloropropane 1%, the phellodendron extract include jamaicin, phellodendrine and obakunone
At least one of.Its preparation method comprises the following steps：
(1) golden cypress is dried in the shade, crushes, obtain golden cypress powder 100g, pour into electric jacket heating and refluxing extraction device (such as Fig. 1 institutes
Show), then the ethanol solution 1000ml that volumetric concentration is 75% is poured into, temperature setting is 95 DEG C, carries out extraction 30min, obtains one
Secondary extract solution；
(2) after the extract solution obtained after step (1) is filtered, the ethanol solution that volumetric concentration is 75% is added
500ml, temperature setting are 95 DEG C, carry out second of extraction 30min, obtain secondary raffinate；
(3) secondary raffinate obtained after step (2) is poured into Rotary Evaporators (as shown in Figure 2), temperature control is
60-75 DEG C, the cryogenic temperature of vavuum pump is 4 DEG C or so, forms negative-pressure vacuum, carries out decompression rotation, the rotating speed of rotation for 75 turns/
Min, paste is evaporated to, obtaining phellodendron extract, (paste phellodendron extract is easy to preserve, and it is molten with 5% ethanol to also allow for the later stage
Solution controls dosage when saturation golden cypress solution is made)；
(4) ethanol that the paste phellodendron extract volumetric concentration obtained after step (3) is 5% is dissolved, saturation is made
Golden cypress solution, adds after methyl-silicone oil and epoxychloropropane to shake and mixes, phellodendron extract, methyl-silicone oil and epoxychloropropane
Mass percent is respectively 96%, 3% and 1%, that is, obtains described bactericide.
Bactericide obtained above is subjected to flat board bacteriostatic test, carried out using mycelial growth rate method biometric techniques
Measure.First the bactericide of the present invention is dissolved with sterilized water, it is standby to be configured to 500 times of strength solutions, and cigarette is being covered with card punch
Bacteria cake is cut on the culture medium of careless balck shank pathogen, bacteria cake is put into microbicide solution and soaked 5 minutes, is then transferred to sterile
In empty culture dish (diameter 90mn), it is placed in 25 DEG C of insulating boxs and cultivates, respectively behind 3 days and 5 days, blank pair is used as using sterilized water
According to, antibacterial circle diameter is determined with crossing method, to analyze influence of the bactericide (500 times of concentration) to balck shank germ, experiment
As a result as shown in table 1 and Fig. 3.
Table 1：Influence (cm) of the bactericide (500 times of concentration) to balck shank germ
(indicate：The large and small mother stock that writes of attached difference does not represent level of difference up to 0.01,0.05 level of signifiance after numeral, under
Together.)
As can be seen from Table 1, when cultivating 3 days and 5 days, compared with the control, the colony diameter of bactericide processing is smaller,
There is pole significant difference, illustrating 500 times of concentration liquid of bactericide of the present invention has good fungistatic effect to black shank bacterium.
Compared with chemical agent control (volumetric concentration is 72% first frost mancozeb wettable powder), at 5 days, the bacterium of bactericide processing
It is big to fall diameter, but is not significantly different, illustrates fungistatic effect and first frost mancozeb wettable powder of the bactericide to black shank bacterium
Quite.
As shown in figure 3, the figure left side is control, the right is the bactericide of the present invention, and the small black circle in 2 culture dishes is bacteria cake
With the mycelia of its growth, it is sterilization of the present invention to compare using the sterilized water after sterilization, the nearly 5.0cm of colony diameter, bactericide
Agent, colony diameter is less than 1.0cm, and in control (sterilized water) control, the hyphal diameter of bacteria cake is substantially than the bactericide of the present invention
Diameter is big.
To examine the indoor control effect of the bactericide of the present invention, following experiment has been carried out.12 formulas of experimental design
Preparation, the room effect biologicall test of 500 times of concentration, investigate colony growth diameter after 3d, be shown in Table 2.
Table 2：Influence (cm) of each biological agent (500 times of concentration) to balck shank germ
As seen from Table 2,1) at 3 days, compared with blank control (CK1), the colony diameter respectively handled is small, there is pole
Difference, illustrates the medicament of each formula, there is extremely significant fungistatic effect；2) at 3 days, with each extract solution stoste formula
(C100%, A100%, B100%, i.e., not adding synergist and stabilizer) is compared, and is formulated (phellodendron extract+methyl-silicone oil+ring
Oxygen chloropropane) processing colony diameter it is small, and there were significant differences, and this explanation with the addition of synergist methyl-silicone oil and stabilizer ring
The preparation fungistatic effect of the cortex phellodendri extract of oxygen chloropropane will be significantly better than cortex phellodendri extract (not adding synergist and stabilizer)；
3) at 3 days, compared with wintergreen barberry root and the formula of air potato, formula (phellodendron extract+methyl-silicone oil+epoxychloropropane) processing
Colony diameter is small, illustrates that the fungistatic effect for being formulated (phellodendron extract+methyl-silicone oil+epoxychloropropane) is better than Chinese medicine soil
The coptis and air potato extract solution；4) compared with positive control (CK2), i.e. 72% first frost mancozeb wettable powder (purchased in market), formula is (yellow
Cypress extract+methyl-silicone oil+epoxychloropropane) processing colony diameter it is small, especially inventive formulation (phellodendron extract
96%+ methyl-silicone oil 3%+ epoxychloropropane 1%) and there were significant differences, illustrates that medicament of the present invention has obvious fungistatic effect.
To examine the control in field effect of the bactericide of the present invention, tests below is carried out, testing ground is as shown in Figure 4.
1. experimental design：Experiment is carried out after field-transplanting, and experiment sets not dispenser (CK1), chemical pesticide (CK2：First frost-
MnZn), bactericide totally 3 processing of the present invention, totally 9 cells, more than 60 plants of each cell kind cigarette, cell is by the examination of random district's groups
Test design, 3 repetitions.Bactericide is made by the preparation method of the present invention, and positive control chemical pesticide is that 72% first frost MnZn can
WP (purchased in market), blank control are clear water.
2. test site：Test site is respectively provided at Hunan Province Longshan County great An towns tobacco base, the morbidity of last year balck shank
Heavier field.
3. experimental cultivar：Cloud and mist 87.
4. dispenser period and method
Tobacco seedlings transplanting on April 21.Dispenser period 7 days and group's phase after cigarette strain transplanting, common dispenser is twice.Application method：
After the bactericide of the present invention is diluted with water into 100 times, every plant of cigarette pouring root 500ml dilute liquid medicine.The bactericide of the present invention is held in
Lucifuge shady place, fully to be shaken up before.
5. observation and record
Control time：For the first time 7 days after a phase medication is rolled into a ball；Second of investigation is 7 days after topping；Third time investigation is in cigarette
Before the harvesting of leaf upper leaf；Investigation is three times, main to investigate the crop field cigarette strain incidence of disease and cigarette strain morbidity series altogether, calculates the state of an illness and refers to
Number.
6. severity Scaling
0 grade：Complete stool is disease-free.
1 grade：Stem's scab is no more than 1/3rd of stem girth, or 1/3rd is wilting with lower blade.
3 grades：Stem's scab is around stem girth 1/3rd to half, or 1/3rd slightly wither to half blade
Wither, or scab occurs in bottom minority blade.
5 grades：Stem's scab exceedes the half of stem girth, but not entirely around stem girth, or half is to 2/3rds
Blade is wilting.
7 grades：Stem's scab is entirely around stem girth, or 2/3rds wilting with blade.
9 grades：Diseased plant is substantially withered.
7. survey data and calculating
Drug effect computational methods are carried out with reference to following methods：
8. result of the test
Different disposal is shown in Table 3 to the prevention effect of tobacco black shank.
Table 3：Prevention effect of the different disposal to tobacco black shank
As shown in Table 3, medicine bactericide of the invention has good prevention effect to tobacco crop field balck shank, to balck shank
Prevention effect reached 81.77%.Understood with reference to table 1, the bactericide pair of the indoor flat plate bacteriostatic test result display present invention
The fungistatic effect of black shank bacterium is suitable with first frost mancozeb wettable powder, and shows the sterilization of the present invention in field experiment result
Agent has been higher by more than 70% to the prevention effect of black shank bacterium than the prevention effect of first frost mancozeb wettable powder, and this illustrates this hair
Bright bactericide efficacy stability, the adhesive force of medicament is stronger, and relatively fewer, preventing and treating effect is influenceed by rain drop erosion or dew dilution
Fruit becomes apparent from, and is particularly suited for the preventing and treating of tobacco crop field balck shank.
As shown in Figure 4, left lateral is control, i.e. spray clear water, it is apparent that tobacco cane is substantially black dead, and right lateral sprays
The bactericide of the present invention, adjacent with control treatment row but without the black dead phenomenon of tobacco stem bar, the present invention is to tobacco black shank for this explanation
Prevention effect it is obvious.
Embodiment 2：
A kind of bactericide for tobacco black shank of the invention, include each component of following mass fraction：Golden cypress is extracted
Thing 96%, H201 methyl-silicone oils 3% and epoxychloropropane 1%, the phellodendron extract include jamaicin, phellodendrine and obakunone
At least one of.Its preparation method comprises the following steps：
(1) golden cypress is dried in the shade, crushes, obtain golden cypress powder 150g, pour into electric jacket heating and refluxing extraction device, then pour into body
The ethanol solution 1200ml that product concentration is 75%, temperature setting are 60-95 DEG C, soak 120-180min, carry out extraction 30min,
Obtain an extract solution；
(2) after the extract solution obtained after step (1) is filtered, the ethanol solution that volumetric concentration is 75% is added
500ml, temperature control are 60-95 DEG C, carry out second of extraction 30min, obtain secondary raffinate；
(3) secondary raffinate obtained after step (2) is poured into Rotary Evaporators, temperature control is 60-75 DEG C, vacuum
The cryogenic temperature of pump is 4 DEG C or so, forms negative-pressure vacuum, carries out decompression rotation, the rotating speed of rotation is 75 turns/min, is evaporated to cream
Shape, obtain phellodendron extract (paste phellodendron extract is easy to preserve, also allow for the later stage with 5% ethanol dissolving be made saturation Huang
Dosage is controlled during cypress solution)；
(4) ethanol that the paste phellodendron extract volumetric concentration obtained after step (3) is 5% is dissolved, saturation is made
Golden cypress solution, adds after methyl-silicone oil and epoxychloropropane to shake and mixes, phellodendron extract, methyl-silicone oil and epoxychloropropane
Mass percent is respectively 96%, 3% and 1%, that is, obtains described bactericide.
To examine the control in field effect test of the bactericide of the present invention, tests below has been carried out.
1. experimental design：Experiment is carried out after field-transplanting, and experiment sets not dispenser (CK1), chemical pesticide (CK2：First frost-
MnZn), bactericide totally 3 processing of the present invention, totally 9 cells, more than 60 plants of each cell kind cigarette, cell is by the examination of random district's groups
Test design, 3 repetitions.Bactericide is made by the preparation method of the present invention, and positive control chemical pesticide is that 72% first frost MnZn can
WP (purchased in market), blank control are clear water.
2. test site：Test site is respectively provided at Hu-nan's agriculture living resources research on utilization institute's medicinal plant base and entered
OK.
3. experimental cultivar：Tobacco K326.
4. dispenser period and method
Tobacco seedlings transplanting on March 16.Dispenser period 7 days and group's phase after cigarette strain transplanting, common dispenser is twice.Application method：
After the bactericide of the present invention is diluted by 100 times, every plant of cigarette pouring root 500ml dilute liquid medicine.The bactericide of the present invention, which is held in, to be kept away
Light shady place, fully to be shaken up before.
5. observation and record
Control time：For the first time 7 days after a phase medication is rolled into a ball；Second of investigation is 7 days after topping；Third time investigation is in cigarette
Before the harvesting of leaf upper leaf；Investigation is three times, main to investigate the crop field cigarette strain incidence of disease and cigarette strain morbidity series altogether, calculates the state of an illness and refers to
Number.
6. severity Scaling
0 grade：Complete stool is disease-free.
1 grade：Stem's scab is no more than 1/3rd of stem girth, or 1/3rd is wilting with lower blade.
3 grades：Stem's scab is around stem girth 1/3rd to half, or 1/3rd slightly wither to half blade
Wither, or scab occurs in bottom minority blade.
5 grades：Stem's scab exceedes the half of stem girth, but not entirely around stem girth, or half is to 2/3rds
Blade is wilting.
7 grades：Stem's scab is entirely around stem girth, or 2/3rds wilting with blade.
9 grades：Diseased plant is substantially withered.
7. survey data and calculating
Drug effect computational methods are carried out with reference to following methods：
8. result of the test
Different disposal is shown in Table 4 to the prevention effect of tobacco black shank.
Table 4：Prevention effect of the different disposal to tobacco black shank
As shown in Table 4, medicine bactericide of the invention has good prevention effect to tobacco crop field balck shank, to balck shank
Prevention effect reached 80.79%.
Claims (10)
1. a kind of bactericide for tobacco black shank, it is characterised in that include phellodendron extract 90%- by mass fraction
96%th, methyl-silicone oil 3%-9% and the epoxychloropropane no more than 1%.
2. bactericide according to claim 1, it is characterised in that by mass fraction by phellodendron extract 96%, methyl silicon
Oil 3% and epoxychloropropane 1% are formed, and the phellodendron extract is made by golden cypress through ethanol reflux extraction.
3. bactericide according to claim 1 or 2, it is characterised in that the phellodendron extract includes jamaicin, phellodendrine
At least one of with obakunone.
4. a kind of preparation method of bactericide as any one of claim 1-3, comprises the following steps：
(1) golden cypress is dried in the shade, crushes, obtain golden cypress powder, pour into ethanol solution, heating carries out first time refluxing extraction, obtains one
Secondary extract solution；
(2) after the extract solution obtained after step (1) is filtered, ethanol solution is poured into, heating carries out second of refluxing extraction, obtained
Secondary raffinate；
(3) secondary raffinate obtained after step (2) is subjected to decompression rotary evaporation, obtains paste phellodendron extract；
(4) the paste phellodendron extract low-concentration ethanol solution obtained after step (3) is dissolved, saturation golden cypress solution is made,
Mixing is shaken after adding methyl-silicone oil and epoxychloropropane, that is, obtains described bactericide.
5. preparation method according to claim 4, it is characterised in that in the step (1), every gram of golden cypress adds 8-10ml
Ethanol solution, the volumetric concentration of ethanol solution is 75%, and heating-up temperature is 60-95 DEG C, extraction time 30-60min；The step
Suddenly in (2), every gram of golden cypress adds 3-5ml ethanol solutions, and the volumetric concentration of ethanol solution is 75%, and heating-up temperature is 60-95 DEG C,
Extraction time is 30-60min.
6. the preparation method according to claim 4 or 5, it is characterised in that enter in electric jacket heating and refluxing extraction device
Row extraction.
7. preparation method according to claim 4, it is characterised in that in the step (3), the rotating speed of rotation is 60-75
Turn/min, the heating-up temperature of evaporation is 60-75 DEG C.
8. the preparation method according to claim 4 or 7, it is characterised in that in the step (3), in Rotary Evaporators
Decompression rotary evaporation is carried out, the cryogenic temperature of vavuum pump is -2.0-10 DEG C.
9. preparation method according to claim 4, it is characterised in that in the step (4), the body of low-concentration ethanol solution
Product concentration is 5%.
10. one kind is as any one of claim 1-3 and made from the preparation method as any one of claim 4-9
Application of the bactericide in crop field tobacco black shank prevention and control field, it is characterised in that the application process of the bactericide is dilute with water
Every plant of cigarette pouring root 500ml after releasing 100 times, time of application are respectively 7-15 days and group's phase after cigarette strain transplanting, are co-administered twice.
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