CN108703157A - It the common fig leaf juice active constituent of inhibiting and killing plant pathogenic fungi and its produces and applies - Google Patents
It the common fig leaf juice active constituent of inhibiting and killing plant pathogenic fungi and its produces and applies Download PDFInfo
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- CN108703157A CN108703157A CN201810737989.2A CN201810737989A CN108703157A CN 108703157 A CN108703157 A CN 108703157A CN 201810737989 A CN201810737989 A CN 201810737989A CN 108703157 A CN108703157 A CN 108703157A
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- 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
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- 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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Abstract
The invention discloses a kind of common fig leaf juice active constituent of inhibiting and killing plant pathogenic fungi and its preparation and application, active constituent is the essence extract being further obtained by extraction as extractant using ethyl acetate or n-hexane again on the basis of using ethyl alcohol as the extract that extractant is obtained by extraction.The common fig leaf juice active constituent of inhibiting and killing plant pathogenic fungi of the present invention, the preparation that can be used for preparing inhibiting and killing plant pathogenic fungi and mushroom disease fungus kills Sclerotinia sclerotiorum, fusarium fungus particularly useful for making suppression, alternaric bacteria, the preparation of the disease fungus such as rhizopus oryzae.The common fig leaf juice active constituent that the present invention discloses has raw material sources extensive, nontoxic to human body, harmless to crop, it is degradable the features such as, can be developed into a kind of non-harmful plant source suppression Fungicidal formulations.
Description
Technical field
The present invention relates to plant pesticide technologies, are to be related to a kind of plant of inhibiting and killing plant pathogenic fungi to carry more specifically
Take object active constituent and the preparation method and application thereof.
Background technology
Plant disease is to influence a key factor of agricultural production, and different pathogens can result in various crop generation
Disease, this causes prodigious loss to agricultural economy.The fungi of Fusarium enough causes various plants to generate various diseases,
The whole world is rapidly developed, and prodigious harm is brought to the agricultural production security in the whole world.It can spend one in the soil
The four seasons in year, and various plants, including industrial crops, cereal crops, ornamental plant and medicinal plant can be infected.Plant can be caused to send out
Raw multiple diseases, such as root-rot, stem rot, spend corruption, the multiple diseases such as fringe corruption, host plant to be up to hundreds of, infect the dimension of plant
Tube bundle system destroys the tissue vascular bundle for being responsible for dredging.For inhibiting and killing plant pathogenic fungi, people have developed suppression and kill very early
The pesticide of plant pathogenic fungi just starts to commercially produce quickly, pesticide fast development the yield of agricultural product is brought it is rich
Thick benefit.The pesticide of early stage inhibiting and killing plant pathogenic fungi is all chemical pesticide, but constantly promoting the use of with chemical pesticide,
Harm caused by it is also that can not be ignored.Serious pollution largely can be caused to environment using chemical pesticide, it can be to non-target
Target biology damages, and the residue of pesticide also can generate harm to the health of the mankind.With carrying for people's lives quality
Height, it is food-safe also more to pay attention to.Therefore it in order to make agricultural obtain sustainable and healthy development, develops to environment and people
The novel pesticide that class health is safe from harm becomes the key task of pesticide research, and biological pesticide becomes grinding for modern agricultural development
Study carefully hot spot, and botanical pesticide is an important field in biological pesticide.Because botanical pesticide has the characteristics that：Ground
Ball plant resources are abundant, and type is various；Unlike chemical pesticide, the specific aim of the biological pesticide of plant source compares
By force, non-target biology will not be damaged；Extracts from Plant Recourses complicated component also has collaboration between each active constituent and makees
With, different activities ingredient is different to the target site of disease, so when using botanical biological pesticide relative to chemical pesticide, disease
Evil is not easy to develop immunity to drugs to pesticide；Because botanical pesticide itself be derived from naturally, can naturally clear up in
Naturally, not will produce has destructive substance to environment, therefore develop efficient biological pesticide for preserving the ecological environment,
Human and livestock health has important meaning.
Invention content
For the very few present situation of the preparation variety of existing plant inhibiting and killing plant pathogenic fungi, the present invention is intended to provide a kind of
It can be used for preparing the novel formulation of inhibiting and killing plant pathogenic fungi, and preparation bioactivity is high, compatible to non-target organism safety, environment
Preparation method and the application of the good common fig leaf juice active constituent and the active constituent of property.
The common fig leaf juice active constituent of inhibiting and killing plant pathogenic fungi provided by the invention, to first pass through ethyl alcohol by common fig leaf juice
Extraction passes through ethyl acetate or the obtained paste common fig leaf juice active constituent of n-hexane extraction again.That is common fig leaf juice active constituent
Can be extracted again by extractant of ethyl acetate to extracting the extract that common fig leaf juice obtains by extractant of ethyl alcohol
Obtained essence extract can also be to be carried by extractant of n-hexane to what the extraction common fig leaf juice by extractant of ethyl alcohol obtained
The essence extract that object is extracted again is taken, or even can also be and always carried using ethyl alcohol as what extractant extraction common fig leaf juice obtained
Take object.Total extract and essence extract may be used to prepare the active constituent of inhibiting and killing plant pathogenic fungi, preferentially select paste
Essence extract.
The common fig leaf juice active constituent of inhibiting and killing plant pathogenic fungi provided by the invention, can be by the side that includes the following steps
Method is produced：
(1) common fig leaf juice of drying and crushing is extracted 12-24 hours using ethyl alcohol as extractant in 18-24 DEG C, is then existed
45-50 DEG C of ultrasound extracts 4-8 hours, and the active constituent in common fig leaf juice is made fully to leach, and is separated by solid-liquid separation, and collects leaching liquor；
(2) leaching liquor being collected into is concentrated in 45-55 DEG C of water-bath, obtains paste common fig leaf juice total extract, and recycle work
For the ethyl alcohol of extractant；
(3) ethyl acetate or n-hexane is used to extract 12- in 18-24 DEG C again the paste common fig leaf juice total extract being concentrated to give
24 hours, the active constituent in common fig leaf juice is made fully to leach, be separated by solid-liquid separation, collects extract liquor；
(4) extract liquor of collection is obtained into pasta finished product common fig leaf juice active constituent in 30-40 DEG C of reduced under vacuum.
In the method for the above-mentioned common fig leaf juice active constituent for producing inhibiting and killing plant pathogenic fungi, step (1) is separated by solid-liquid separation
Obtained leaf slag preferably further continues extraction 4-8 hours with ethyl alcohol under ultrasonic wave, is separated by solid-liquid separation, isolated extraction
Liquid merges with the leaching liquor that step (1) obtains, and enters step (2).
In the method for the above-mentioned common fig leaf juice active constituent for producing inhibiting and killing plant pathogenic fungi, step (3) is separated by solid-liquid separation
Obtained solid slag preferably further continues extraction 12-24 hours with ethyl acetate or n-hexane, is separated by solid-liquid separation, is obtained after separation
Extract liquor merge with the leaching liquor that step (3) obtains, enter step (4).With ethyl acetate or n-hexane continue to solid slag into
The residue of resulting separation, can be washed colourless to cleaning solution with ethyl acetate or n-hexane after row extraction.
In the method for the above-mentioned common fig leaf juice active constituent for producing inhibiting and killing plant pathogenic fungi, step (2) is obtained
Paste common fig leaf juice total extract is not sent into before step (3) processing, is most better than under 1-10 DEG C of environment and is preserved.Step if (2) institute
Obtained paste common fig leaf juice total extract, which is connected to, to be fed to step (3) and is handled, then need not especially be preserved.
In the method for the above-mentioned common fig leaf juice active constituent for producing inhibiting and killing plant pathogenic fungi, extraction is molten in step (1)
The dosage of agent ethyl alcohol is preferably controlled to 5-10 times of common fig leaf juice raw material volume；In step (3) extractant ethyl acetate or just oneself
The dosage priority acccess control of alkane is 7-15 times of solid slag volume.
The method of the above-mentioned common fig leaf juice active constituent for producing inhibiting and killing plant pathogenic fungi, the ethyl alcohol as extractant are excellent
The ethyl alcohol that volume fraction is not less than 75% is selected in choosing；The ethyl alcohol of further preferred volume fraction 90-98%.
The common fig leaf juice active constituent of the inhibiting and killing plant pathogenic fungi provided by the invention can be used for preparing suppression and kill chain lattice
Spore bacterium, fusarium chlamydosporum, fusarium culmorum, Sclerotinia sclerotiorum, Fusarium graminearum, Fusarium oxysporum, fusarium tricinctum, anthracnose
Bacterium, the pathogen of Botrytis cinerea, rhizopus oryzae, the preparation of cladosporium sp.
After the medicinal extract shape common fig leaf juice total extract and extract that the present invention obtains can be used for N,N-dimethylformamide dissolving
It is directly used in the preparation for preparing inhibiting and killing plant pathogenic fungi.Only total extract inhibiting and killing plant pathogenic fungi effect is killed compared with extract suppression
Plant pathogenic fungi effect is lower.
The common fig leaf juice active constituent for the inhibiting and killing plant pathogenic fungi that the present invention discloses can be used for preparing inhibiting and killing plant pathogenic
Fungi and mushroom disease fungus preparation, Sclerotinia sclerotiorum, fusarium fungus, alternaric bacteria, rice are killed particularly useful for making suppression
The preparations such as rhizopus.
The common fig leaf juice active constituent for the inhibiting and killing plant pathogenic fungi that the present invention discloses, can be prepared into aqua, soluble powder
Preparation is killed in the plant pathogenic fungi suppression of the dosage forms such as agent, wettable powder, strong suspending agent and granula.The preparation method of various dosage forms is this
The conventional method in field, the adjuvant used usual auxiliaries in pesticide field in each dosage form manufacturing process.Each dosage form is when in use
The solution configured, the wherein concentration of fig leaf extract should be in the range of 0.1mg/mL-1000mg/mL.
For common fig leaf juice active constituent provided by the invention to alternaric bacteria, common fig leaf juice raw material sources are extensive, to human body without
Poison, it is harmless to crop, as plant source suppression fungicide have the characteristics that it is degradable, therefore be expected to exploitation be a kind of non-harmful plant
Material resource presses down Fungicidal formulations.
Description of the drawings
Fig. 1 is the inhibiting effect figure of three kinds of medicinal extract pair, three kinds of disease fungus.
Fig. 2 is bacteriostatic activity figure of the F1-F11 components to fusarium culmorum.
Specific implementation mode
The specific implementation mode for describing the present invention by the following examples is done present disclosure further detailed again
Explanation.But this should not be interpreted as protection scope of the present invention and be only limitted to example, on the contrary, being realized based on present disclosure
Technology application all belong to the scope of protection of the present invention.
Determination of activity is to measure prepared sample to the antibacterial of disease fungus using growth rate method under conditions of in vitro
Activity is alternaric bacteria (Alternaria alternate), fusarium chlamydosporum (Fusarium for examination bacterium
Chlamydosporum), fusarium culmorum (Fusarium culmorum), Sclerotinia sclerotiorum (Sclerotinia
Sclerotiorum), Fusarium graminearum (Fusarium graminearum), Fusarium oxysporum (Fusarium
Oxysporium), fusarium tricinctum (Fusarium tricinctum), anthrax bacteria (Colletotrichum
Higginsianum), the pathogen of Botrytis cinerea (Botrytis cinerea), rhizopus oryzae (Rhizopus oryzae), cladosporium sp
(Cladosporium cladosporioides)。
Embodiment 1：Common fig leaf juice total extract,
(1) dry common fig leaf juice is smashed it through into 40 mesh sieve, obtains common fig leaf juice powder.
(2) take 95% ethyl alcohol for being equivalent to about 7 times of material quality (ranging from 5-10 times of general control) volume in room temperature
About 20h (general control ranging from 12-24h) is extracted under (temperature is generally in 18-24 DEG C of range).
(3) ultrasonic wave 6h (the general control ranging from 4-8h) at about 50 DEG C.With Buchner funnel negative pressure filtration, remove residual
Slag obtains filtrate.
(4) by residue again with 95% second for being equivalent to about 6 times of material quality (ranging from 5-10 times of general control) volume
The further ultrasonic extraction 6h of alcohol (general control ranging from 4-8h), makes the active constituent in common fig leaf juice fully propose, uses Bu Shi
Funnel negative pressure filtration, removes residue, obtains filtrate.
(5) merging filtrate, filtrate are dense under about 50 DEG C of (ranging from 45-55 DEG C of general control) water-baths with Rotary Evaporators
Contracting obtains extraction condensed cream, 4 DEG C of preservations.
(6) a small amount of common fig leaf juice condensed cream is taken, being configured to a concentration of 0.05g/mL solution with n,N-Dimethylformamide makees
To test ready sample.
Embodiment 2：The preparation of N-hexane extract and Antibacterial Activity
(1) dry common fig leaf juice is smashed it through into 40 mesh sieve, obtains common fig leaf juice powder.
(2) take 95% ethyl alcohol for being equivalent to about 7 times of material quality (ranging from 5-10 times of general control) volume in room temperature
About 20h (general control ranging from 12-24h) is extracted under (temperature is generally in 18-24 DEG C of range).
(3) ultrasonic wave 6h (the general control ranging from 4-8h) at about 50 DEG C.With Buchner funnel negative pressure filtration, remove residual
Slag obtains filtrate.
(4) by residue again with 95% second for being equivalent to about 6 times of material quality (ranging from 5-10 times of general control) volume
The further ultrasonic extraction 6h of alcohol (general control ranging from 4-8h), makes the active constituent in common fig leaf juice fully propose, uses Bu Shi
Funnel negative pressure filtration, removes residue, obtains filtrate.
(5) merging filtrate, filtrate are dense under about 50 DEG C of (ranging from 45-55 DEG C of general control) water-baths with Rotary Evaporators
Contracting obtains extraction condensed cream, 4 DEG C of preservations.
(6) n-hexane extraction of its 10 times of volumes is added in common fig leaf juice alcohol leaching carries condensed cream, filter paper filters to get filtrate,
The n-hexane that proper volume is added again into remaining solid repeats to extract, and filter paper filters to get filtrate.Until extract liquor is to colourless
Until, then obtained filtrate is concentrated in vacuo with Rotary Evaporators at 35 DEG C to obtain common fig leaf juice alcohol extract just
Hexane extracts medicinal extract
(7) take a small amount of common fig leaf juice medicinal extract, use n,N-Dimethylformamide be configured to a concentration of 0.05g/mL solution as
Test ready sample.
3 acetic acid ethyl ester extract of embodiment
(1) dry common fig leaf juice is smashed it through into 40 mesh sieve, obtains common fig leaf juice powder.
(2) take 95% ethyl alcohol for being equivalent to about 7 times of material quality (ranging from 5-10 times of general control) volume in room temperature
About 20h (general control ranging from 12-24h) is extracted under (temperature is generally in 18-24 DEG C of range).
(3) ultrasonic wave 6h (the general control ranging from 4-8h) at about 50 DEG C.With Buchner funnel negative pressure filtration, remove residual
Slag obtains filtrate.
(4) by residue again with 95% second for being equivalent to about 6 times of material quality (ranging from 5-10 times of general control) volume
The further ultrasonic extraction 6h of alcohol (general control ranging from 4-8h), makes the active constituent in common fig leaf juice fully propose, uses Bu Shi
Funnel negative pressure filtration, removes residue, obtains filtrate.
(5) merging filtrate, filtrate are dense under about 50 DEG C of (ranging from 45-55 DEG C of general control) water-baths with Rotary Evaporators
Contracting obtains extraction condensed cream, 4 DEG C of preservations.
(6) ethyl acetate that its 10 times of volumes are added in common fig leaf juice alcohol leaching carries condensed cream is extracted, filter paper filtering
Filtrate is obtained, the ethyl acetate that proper volume is added again into remaining solid repeats to extract, and filter paper filters to get filtrate.Until extraction
Then all obtained filtrates are concentrated in vacuo with Rotary Evaporators at 35 DEG C until colourless and obtain common fig leaf juice alcohol extracting by liquid
The ethyl acetate of object extracts medicinal extract.
(7) take a small amount of common fig leaf juice medicinal extract, use n,N-Dimethylformamide be configured to a concentration of 0.05g/mL solution as
Test ready sample.
The Antibacterial Activity of three kinds of extracts
The measurement of bioactivity：In in vitro, the suppression of fig leaf extract is measured using mycelial growth rate method
Bacterium activity.Experiment ready sample (mass concentration 0.05g/mL) is taken to prepare culture medium, compound concentration 1.0mg/mL respectively.It waits for
After tablet solidification plant pathogenic fungi bacteria cake (fusarium culmorum, rape cultured, that growth is consistent are accessed in plate center
Sclerotium bacteria, alternaric bacteria), 3 repetitions are set as blank control (CK), each processing to be added after sterile aqueous media inoculation,
It is cultivated in constant incubator at 26 DEG C, until control culture dish bacterium colony records data when will cover with culture dish.Each bacterium colony according to
Crossing method measures twice, the size of its bacterium colony is represented with average, the calculation formula of bacteriostasis rate is as follows：
Colony diameter (mm)=bacterium colony average diameter-bacteria cake diameter (6.0mm)
Bacteriostasis rate (%)=(control colony diameter-processing colony diameter) ÷ compares colony diameter × 100%
Experimental result such as table 1, it is shown shown in Fig. 1：
The bacteriostasis rate of 1 common fig leaf juice of table, three kinds of medicinal extract pair, three kinds of disease fungus
E* represents common fig leaf juice alcohol extract, and E/A* represents common fig leaf juice alcohol extract acetic acid ethyl ester extract, and E/H* represents nothing
Flowers and fruits alcohol extracts from the leaves N-hexane extract.
Three kinds of medicinal extract of common fig leaf juice are to alternaric bacteria as can be seen from Table 1, fusarium culmorum, and Sclerotinia sclerotiorum has suppression
It makes and uses, but its inhibition level is different from.Wherein the inhibition of three kinds of disease fungus of common fig leaf juice acetic acid ethyl ester extract pair is made
With most by force, the inhibition of alcohol extract is taken second place, and fungistatic effect is shown in Fig. 1.As a concentration of 1.0mg/mL of medicine base, common fig leaf juice acetic acid
For ethyl ester extract extract to alternaric bacteria, the growth inhibition ratio of fusarium culmorum, Sclerotinia sclerotiorum is respectively 72.7%,
87.4%, 100%.Illustrate that the active ingredient of common fig leaf juice is present in acetic acid ethyl ester extract.
The biological activity determination of 4 common fig leaf juice acetic acid ethyl ester extract of embodiment
(1) take cream shape common fig leaf juice acetic acid ethyl ester extract is configured to a concentration of 0.05g/mL with N,N-dimethylformamide
Liquid is as experiment ready sample, with alternaric bacteria, fusarium chlamydosporum, and fusarium culmorum, Sclerotinia sclerotiorum, Fusarium graminearum,
Fusarium oxysporum, fusarium tricinctum, anthrax bacteria, the pathogen of Botrytis cinerea, rhizopus oryzae, cladosporium sp are for trying strain, measuring not
With the bacteriostatic activity under liquor strength.Antibacterial Activity method is the same as embodiment 1.
Experimental result is as shown in table 2：
The inhibiting effect of 2 11 kinds of disease fungus mycelia of common fig leaf juice acetic acid ethyl ester extract pair of table growth
Note：Bacteriostasis rate is that liquor strength is measured in 1.0mg/mL.
By table it can be seen that common fig leaf juice ethyl alcohol total extract 11 kinds of disease fungus of acetic acid ethyl ester extract pair all have centainly
Inhibition, wherein the inhibiting rate to Sclerotinia sclerotiorum has reached 100%,
5 common fig leaf juice acetic acid ethyl ester extract active constituent of embodiment detaches and determination of activity
1, grope the Optimum separation condition to common fig leaf juice acetic acid ethyl ester extract with thin-layer chromatography, by silica gel plate in baking oven
In activate 30min at 100 DEG C, with pencil gently retouching a filament away from 1 centimeters of silica gel plate bottom margin after cooling, using glass
Point sample capillary draws common fig leaf juice E/A extract mother liquors, then point uses ethyl acetate, ethyl acetate respectively on silica gel plate
With petroleum ether mixed liquor, the mixed liquor of ethyl acetate and methanol detects best separation scheme as solvent, waits until solvent
Forward position when going to about 1 centimetre away from silica gel plate top or so, take out silica gel plate, bands of a spectrum observed under 254nm ultraviolet lamps, analysis is most
Good separation condition.
2, the normal column pressure just separation of common fig leaf juice E/A extracts,
(1) column is filled：Suspension is made in silica white with petroleum ether to pour into pillar, is then eluted with petroleum ether always, directly
To after the silica white compacting in pillar, a small amount of quartz sand is added into column, keeps its evenly laid out on silica white, continuing to pillar
Middle addition petroleum ether closes pillar when liquid level is reduced to about 2cm higher than quartz sand surface in column.
(2) loading：Sample is uniformly added on quartz sand layer along chromatographic column tube wall, then uses petroleum ether on pillar
Residual sample is flushed into column, and a small amount of quartz sand is added into column, keeps its evenly laid out in sample, opening piston makes column internal solvent
Outflow, when liquid level is equal with cylinder, closure piston.
(3) it elutes：Using linear gradient elution method, ethyl acetate-light petrol (10 is first pressed:1,5:1) ratio sequentially adds column
Then son uses acetate-methanol (100:1,50:1,25:1,5:1,1:1) ratio sequentially adds pillar, finally uses methanol
The flow velocity of elution, elution is that 4-5 drops are per second, and a pipe is according to circumstances collected per 30-50mL.While elution, the liquid that will be collected into
Body is identified using thin-layered chromatography, and the liquid of the identical thin-layer chromatography mobility under 254nm ultraviolet irradiations is merged one
It rises, 11 components is finally obtained, are named as F1-F11.Finally 11 components are carried out with Rotary Evaporators under 50 DEG C of water-baths
It is concentrated to give medicinal extract.
(4) measurement of bioactivity：In in vitro, the antibacterial work of 11 components is measured using mycelial growth rate method
Property.11 components respectively take 0.4mg, are completely dissolved with n,N-Dimethylformamide and are made into 11 kinds of liquids.11 are measured with 24 well plate methods
The antifungal activity of kind of liquid, first empty to be added isometric n,N-Dimethylformamide, as negative control group, behind according to
11 kinds of liquids of secondary addition, are then separately added into the PDA culture medium also in liquid condition of 400 μ L into 12 holes, make its with
Liquid is sufficiently mixed.After culture medium cooled and solidified, fresh fusarium culmorum mycelia block, inoculation are intercepted using card punch (4mm)
To among the culture medium made.Until the mycelia of blank control group covers with tablet, the mycelia growth of observation medication processing group
Situation calculates bacteriostasis rate method such as embodiment 1.
Experimental result is as shown in Figure 2.F5 components are demonstrated by apparent inhibition to fusarium culmorum and make as can be seen from Figure 2
With.Illustrate that the compound with antifungal activity is in F5 components in common fig leaf juice.
6 common fig leaf juice acetic acid ethyl ester extract Active Components of embodiment
(1) method of gas chromatography-mass spectrum is used to analyze the F5 composition components with antifungal activity.Chromatostrip
Part is to be analyzed common fig leaf juice alcohol extract and E/A extract ingredients using the method for gas chromatography-mass spectrum[29].Post case temperature
Degree：40.0℃；Injector temperature：290.00℃；Sample introduction pattern：Shunting；Flow control mode：Pressure；Pressure：49.5kPa；Total stream
Amount：9.0mL/min；Column flow：1.00mL/min；Linear velocity：36.1cm/sec；Purge flow rate：3.0mL/min；Split ratio：
5.0；High pressure sample introduction pattern：It closes；Carrier gas saving device：It closes；Shunt Damping System is fixed：It closes；
Column oven temperature program(me)：
[GC Cheng Xus ]
[GCMS-QP2010Plus]
Ion source temperature：200.00℃；Interface temperature：220.00℃；The solvent delay time：3.00min；Detector gain
Mode：Relatively；Detector gain：0.00kV；Threshold values：0.Spectrum library is：NIST08.LIB.
Experimental result is as shown in table 3：
The GC/MS analysis results of table 3F5 components
F5 component analyses show that its main compound has 6 kinds (being shown in Table 2.3) as can be seen from Table 3.Wherein acetic acid lupeol
The content of ester (Lup-20 (29)-en-3-ol, acetate, (3b) -) is up to 27.02%, is secondly cupreol (β-
Sitosterol), content is 17.31%.The content of psoralen (Psoralen) also more a height of 8.11%.Remaining 3 kinds
The content of compound is relatively low, respectively bergapten (4-Methoxy-7H-furo[3,2-g]Chromen-7-one,
7.61%), Heptadecanoic acide (Margaric acid, 6.95%), 4-methyl-2-oxo-2H-chromene-7-
Carbaldehyde (5.05%).It can tentatively judge the main Active antifungal compound in common fig leaf juice acetic acid ethyl ester extract
May be psoralen, Lupeol acetate, cupreol.
Claims (10)
1. a kind of common fig leaf juice active constituent of inhibiting and killing plant pathogenic fungi, which is characterized in that first pass through second by common fig leaf juice
Alcohol extraction passes through ethyl acetate or the obtained paste common fig leaf juice active constituent of n-hexane extraction again.
2. the common fig leaf juice active constituent preparation method of inhibiting and killing plant pathogenic fungi described in claim 1, it is characterised in that including
Following steps：
(1) common fig leaf juice of drying and crushing is extracted 12-24 hours using ethyl alcohol as extractant in 18-24 DEG C, then in 45-50
DEG C ultrasound extraction 4-8 hour, so that the active constituent in common fig leaf juice is fully leached, be separated by solid-liquid separation, collection leaching liquor；
(2) leaching liquor being collected into is concentrated in 45-55 DEG C of water-bath, obtains paste common fig leaf juice total extract, and recycle as extraction
Take the ethyl alcohol of solvent；
(3) the paste common fig leaf juice total extract being concentrated to give is used again ethyl acetate or n-hexane small in 18-24 DEG C of extraction 12-24
When, so that the active constituent in common fig leaf juice is fully leached, be separated by solid-liquid separation, collects extract liquor；
(4) extract liquor of collection is obtained into pasta finished product common fig leaf juice active constituent in 30-40 DEG C of reduced under vacuum.
3. the common fig leaf juice active constituent preparation method of inhibiting and killing plant pathogenic fungi according to claim 2, which is characterized in that
Step (1) is separated by solid-liquid separation obtained leaf slag ethyl alcohol and continues extraction 4-8 hours under ultrasonic wave, is separated by solid-liquid separation, it is isolated
Leaching liquor merge with the leaching liquor that step (1) obtains, enter step (2).
4. the common fig leaf juice active constituent preparation method of inhibiting and killing plant pathogenic fungi according to claim 2, which is characterized in that
Step (3) is separated by solid-liquid separation obtained solid slag ethyl acetate or n-hexane continues extraction 12-24 hours, is separated by solid-liquid separation, separation
The extract liquor obtained afterwards merges with the leaching liquor that step (3) obtains, and enters step (4).
5. the common fig leaf juice active constituent preparation method of inhibiting and killing plant pathogenic fungi according to claim 4, which is characterized in that
Continue to extract through being separated by solid-liquid separation obtained residue, with ethyl acetate or n-hexane solid slag with ethyl acetate or n-hexane
Washing is colourless to cleaning solution.
6. special according to the common fig leaf juice active constituent preparation method of one of claim 2 to 5 inhibiting and killing plant pathogenic fungi
Sign is that the obtained paste common fig leaf juice total extract of step (2) is not sent into before step (3) processing, under 1-10 DEG C of environment
It preserves.
7. special according to the common fig leaf juice active constituent preparation method of one of claim 2 to 5 inhibiting and killing plant pathogenic fungi
Sign is, the dosage of extractant ethyl alcohol is 5-10 times of common fig leaf juice raw material volume in step (1)；Extractant in step (3)
The dosage of ethyl acetate or n-hexane is 7-15 times of solid slag volume.
8. special according to the common fig leaf juice active constituent preparation method of one of claim 2 to 5 inhibiting and killing plant pathogenic fungi
Sign is that the ethyl alcohol as extractant is the ethyl alcohol that volume fraction is not less than 75%.
9. the common fig leaf juice active constituent preparation method of inhibiting and killing plant pathogenic fungi according to claim 8, which is characterized in that
The ethyl alcohol that ethyl alcohol as extractant is volume fraction 90%-98%.
10. the common fig leaf juice active constituent of inhibiting and killing plant pathogenic fungi described in claim 1 kills alternaric bacteria, thick spore in preparation suppression
Sickle-like bacteria, fusarium culmorum, Sclerotinia sclerotiorum, Fusarium graminearum, Fusarium oxysporum, fusarium tricinctum, anthrax bacteria, grey grape
Spore bacterium, rhizopus oryzae, the application in cladosporium sp preparation.
Priority Applications (1)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1650918A (en) * | 2004-12-03 | 2005-08-10 | 山东大学 | Fig leaf extract and its use |
| CN101053332A (en) * | 2007-05-08 | 2007-10-17 | 四川大学 | Active constituent of curcuma longa for inhibiting and killing plant pathogenic fungi and its preparation and application |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1650918A (en) * | 2004-12-03 | 2005-08-10 | 山东大学 | Fig leaf extract and its use |
| CN101053332A (en) * | 2007-05-08 | 2007-10-17 | 四川大学 | Active constituent of curcuma longa for inhibiting and killing plant pathogenic fungi and its preparation and application |
Non-Patent Citations (6)
| Title |
|---|
| AFAF MOHAMMED WELI, AFAF ALI MOHAMMED AL-BLUSHI，MOHAMMAD AMZAD: "《Evaluation of antioxidant and antimicrobial potential of different leaves crude extracts of Omani Ficus carica against food borne pathogenic bacteria》", 《ASIAN PACIFIC JOURNAL OF TROPICAL DISEASE》 * |
| 张俐，欧晓明，张承来，等: "《几种有机溶剂对靶标病原菌生长影响的研究》", 《浙江化工》 * |
| 朱斌: "《5种植物提取物对植物病原真菌活性研究》", 《扬州大学硕士学位论文》 * |
| 李少华: "《植物农药》", 31 October 2012, 中国农业科学技术出版社 * |
| 赵爱云，吴神怡，杜桂彩: "《无花果叶抑菌活性成分的实验研究》", 《青岛大学学报（自然科学版）》 * |
| 齐建红，冯航: "《无花果叶中提取物的抑菌活性研究》", 《陕西农业科学》 * |
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Application publication date: 20181026 |