CN105638737A - Mongolian oak wood vinegar extract, preparation method and application thereof and harmless insecticide - Google Patents
Mongolian oak wood vinegar extract, preparation method and application thereof and harmless insecticide Download PDFInfo
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- CN105638737A CN105638737A CN201610048769.XA CN201610048769A CN105638737A CN 105638737 A CN105638737 A CN 105638737A CN 201610048769 A CN201610048769 A CN 201610048769A CN 105638737 A CN105638737 A CN 105638737A
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- A01N61/00—Biocides, pest repellants or attractants, or plant growth regulators containing substances of unknown or undetermined composition, e.g. substances characterised only by the mode of action
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Abstract
The invention discloses Mongolian oak wood vinegar extract and a preparation method thereof. The Mongolian oak wood vinegar extract is prepared from, by weight, 50-70% of phenols, 20-30% of ethers, 5-15% of aldehydes, 2-6% of ketone and the balance impurities. The method includes the steps that a Mongolian oak wood vinegar crude product is subjected to reduced pressure distillation to obtain first deep color liquid; the first deep color liquid is dissolved in water, insoluble particles are removed, and then second deep color liquid is obtained; the second deep color liquid is extracted with organic solvent, an organic solvent layer after extraction is collected, the organic solvent is removed through reduced pressure distillation, and then third deep color liquid is obtained; the third deep color liquid is dissolved in water, insoluble particles are removed, and fourth deep color liquid is obtained; selectively, water is removed from the fourth deep color liquid, and then fifth deep color liquid is obtained.
Description
Technical field
The application relates to, but are not limited to pesticide production technology field, is particularly, but not limited to a kind of Xylosmae japonici wood vinegar extract and its production and use and a kind of environmental-pollution insecticide.
Background technology
Pesticide is to ensure that the key factor that crops are had a good harvest. But chemical pesticide contaminated environment, seriously destroys ecosystem, and the high residue in agricultural byproducts causes direct threat to human life, chemical pesticide pollutes has become whole world public hazards, and therefore we must average out in agricultural development with environment and health. The organic agricultural chemicals of Non-polluted residue-free is an extraordinary selection.
Summary of the invention
This application provides a kind of Xylosmae japonici wood vinegar extract.
Xylosmae japonici wood vinegar extract provided herein includes the ketone of the phenols of 50��70 weight %, the ethers of 20��30 weight %, the aldehydes of 5��15 weight % and 2��6 weight %, and surplus is impurity.
In some embodiments, described phenols can include catechol, 4-methyl pyrocatechol, 6-methoxyl group catechol, 4-ethylo benzene phosphorus diphenol, desaspidinol; Described ethers can include pyrithiobacsodium, 1,2,4-benzene three methyl ether, 2-acetonyl-4-hydroxyanisol; Described aldehydes can include 5 hydroxymethyl furfural, 2,3-bis-dehydration galactan, Isosorbide-5-Nitrae: 3,6-bis-dehydration ��-D-Glucopyranose .s; Described ketone can include 6-hydroxyhexane-2-ketone.
Present invention also provides a kind of method preparing Xylosmae japonici wood vinegar extract.
The provided herein method preparing Xylosmae japonici wood vinegar extract includes:
By the decompression distillation of Xylosmae japonici wood vinegar crude product, obtain the first adopting dark liquid;
Described first adopting dark liquid is dissolved in water, removes insoluble particulates, obtain the second adopting dark liquid;
With the second adopting dark liquid described in organic solvent extraction, collecting the organic solvent layer after extracting, decompression is distilled off organic solvent, obtains the 3rd adopting dark liquid;
Described 3rd adopting dark liquid is dissolved in water, removes insoluble particulates, obtain the 4th adopting dark liquid;
Alternatively, described 4th adopting dark liquid is removed water, obtains the 5th adopting dark liquid.
In some embodiments, during by the decompression distillation of Xylosmae japonici wood vinegar crude product, described decompression distillation can carry out at the temperature of the pressure of-0.085MPa��-0.1MPa and 50 DEG C-60 DEG C, till the condensation tube wall of Rotary Evaporators does not have drop to drip; By collect after extracting organic solvent layer decompression distillation time, described decompression distillation can carry out at the temperature of the pressure of-0.085MPa��-0.1MPa and 30 DEG C-40 DEG C, till the condensation tube wall of Rotary Evaporators does not have drop to drip.
In some embodiments, during by the decompression distillation of Xylosmae japonici wood vinegar crude product, described decompression distillation can carry out at the temperature of the pressure of-0.1MPa and 60 DEG C; By collect after extracting organic solvent layer decompression distillation time, described decompression distillation can carry out at the temperature of the pressure of-0.1MPa and 30 DEG C.
In some embodiments, described organic solvent can be one or more in chloroform, ethyl acetate and dichloromethane, and alternatively, described organic solvent is chloroform.
In some embodiments, described organic solvent can be 1:1 with the volume ratio of described second adopting dark liquid.
Present invention also provides the Xylosmae japonici wood vinegar extract prepared by the described method preparing Xylosmae japonici wood vinegar extract.
Present invention also provides the above-mentioned Xylosmae japonici wood vinegar extract purposes as insecticide.
In some embodiments, described Xylosmae japonici wood vinegar extract may be used for the deinsectization preventing and treating of bollworm, beet armyworm, diamondback moth and Prodenia litura.
Present invention also provides a kind of environmental-pollution insecticide, described environmental-pollution insecticide contains above-mentioned Xylosmae japonici wood vinegar extract and water.
In some embodiments, the concentration of Xylosmae japonici wood vinegar extract described in described insecticide can be 10��20mg/mL.
The above-mentioned Xylosmae japonici wood vinegar extract that the application provides be a kind of efficiently, low toxicity, noresidue, free from environmental pollution, do not destroy the nuisanceless of ecological balance and plant source property insecticide, can effectively kill the multiple Field Pests including bollworm, beet armyworm, diamondback moth and Prodenia litura.
Accompanying drawing explanation
Fig. 1 is the GC-MS composition analysis collection of illustrative plates of the Xylosmae japonici wood vinegar extract of embodiment 1.
Fig. 2 be 2 age bollworm variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, the growth conditions figure after 4 days.
Fig. 3 be 2 age bollworm variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, bollworm body weight is over time.
Fig. 4 be 2 age bollworm variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, Helicoverpa armigera length is over time.
Fig. 5 be 2 age bollworm variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 2 Xylosmae japonici wood vinegar extract effect under, the growth conditions figure after 4 days.
Fig. 6 be 2 age bollworm variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 4 Xylosmae japonici wood vinegar extract effect under, the growth conditions figure after 4 days.
Fig. 7 be 3 age bollworm variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar insecticide effect under, the growth conditions figure after 4 days.
Fig. 8 be 2 age beet armyworm variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, the growth conditions figure after 4 days.
Fig. 9 be 2 age beet armyworm variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, beet armyworm body length is over time.
Figure 10 be 3 age diamondback moth variable concentrations (0,1.25,2.5,5,7.5,10mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, the growth conditions figure after 3 days.
Figure 11 be 3 age diamondback moth variable concentrations (0,1.25,2.5,5,7.5,10mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, diamondback moth body length is over time.
Figure 12 be 2 age Prodenia litura variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, the growth conditions figure after 4 days.
Figure 13 be 2 age Prodenia litura variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, Prodenia litura body length is over time.
Figure 14 be 2 age Prodenia litura variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 1 Xylosmae japonici wood vinegar extract effect under, Prodenia litura body weight is over time.
Figure 15 be 2 age Prodenia litura variable concentrations (0,2.5,5,10,15,20mg/mL) embodiment 3 Xylosmae japonici wood vinegar extract effect under, the growth conditions figure after 4 days.
Detailed description of the invention
Describe presently filed embodiment by the examples below, it will be appreciated by the person skilled in the art that these specific embodiments only indicate that to reach the purpose of the application and the enforcement technical scheme that selects, be not the restriction to technical scheme. According to teachings of the present application, it is obvious in conjunction with prior art to the improvement of technical scheme, belongs to the scope of the application protection.
The application embodiment provides a kind of Xylosmae japonici wood vinegar extract, and described Xylosmae japonici wood vinegar extract includes the ketone of the phenols of 50��70 weight %, the ethers of 20��30 weight %, the aldehydes of 5��15 weight % and 2��6 weight %, and surplus is impurity.
In the application embodiment, described Xylosmae japonici wood vinegar extract can include the ketone of the phenols of 55��60 weight %, the ethers of 25��30 weight %, the aldehydes of 5��10 weight % and 2��6 weight %, and surplus is impurity.
In the application embodiment, described phenols can include catechol, 4-methyl pyrocatechol, 6-methoxyl group catechol, 4-ethylo benzene phosphorus diphenol, desaspidinol; Described ethers can include pyrithiobacsodium, 1,2,4-benzene three methyl ether, 2-acetonyl-4-hydroxyanisol; Described aldehydes can include 5 hydroxymethyl furfural, 2,3-bis-dehydration galactan, Isosorbide-5-Nitrae: 3,6-bis-dehydration ��-D-Glucopyranose .s; Described ketone can include 6-hydroxyhexane-2-ketone.
In the application embodiment, described impurity potentially includes Ester and/or alcohols material.
The application embodiment further provides a kind of method preparing Xylosmae japonici wood vinegar extract, and described method includes:
By the decompression distillation of Xylosmae japonici wood vinegar crude product, obtain the first adopting dark liquid;
Described first adopting dark liquid is dissolved in water, removes insoluble particulates, obtain the second adopting dark liquid;
With the second adopting dark liquid described in organic solvent extraction, collecting the organic solvent layer after extracting, decompression is distilled off organic solvent, obtains the 3rd adopting dark liquid;
Described 3rd adopting dark liquid is dissolved in water, removes insoluble particulates, obtain the 4th adopting dark liquid;
Alternatively, described 4th adopting dark liquid is removed water, obtains the 5th adopting dark liquid.
In the application embodiment, during by the decompression distillation of Xylosmae japonici wood vinegar crude product, described decompression distillation can carry out at the temperature of the pressure of-0.085MPa��-0.1MPa and 50 DEG C-60 DEG C, till the condensation tube wall of Rotary Evaporators does not have drop to drip; By collect after extracting organic solvent layer decompression distillation time, described decompression distillation can carry out at the temperature of the pressure of-0.085MPa��-0.1MPa and 30 DEG C-40 DEG C, till the condensation tube wall of Rotary Evaporators does not have drop to drip.
In the application embodiment, during by the decompression distillation of Xylosmae japonici wood vinegar crude product, described decompression distillation can carry out at the temperature of the pressure of-0.1MPa and 60 DEG C; By collect after extracting organic solvent layer decompression distillation time, described decompression distillation can carry out at the temperature of the pressure of-0.1MPa and 30 DEG C.
In the application embodiment, described organic solvent can be one or more in chloroform, ethyl acetate and dichloromethane, and alternatively, described organic solvent is chloroform.
In the application embodiment, the volume ratio of described organic solvent and described second adopting dark liquid can be 1:1.
In the application embodiment, when using organic solvent extraction the second adopting dark liquid, extraction times can select according to actual needs; Alternatively, extract 3 times.
The application embodiment further provides the Xylosmae japonici wood vinegar extract prepared by the described method preparing Xylosmae japonici wood vinegar extract.
The application embodiment further provides the above-mentioned Xylosmae japonici wood vinegar extract purposes as insecticide.
In the application embodiment, described Xylosmae japonici wood vinegar extract may be used for the deinsectization preventing and treating of bollworm, beet armyworm, diamondback moth and Prodenia litura.
The application embodiment further provides a kind of environmental-pollution insecticide, and described environmental-pollution insecticide can contain above-mentioned Xylosmae japonici wood vinegar extract and water.
In the application embodiment, the concentration of Xylosmae japonici wood vinegar extract described in described insecticide can be 10��20mg/mL.
In the application embodiment, wood vinegar crude product can be usual sources well known by persons skilled in the art, such as, lumber is broken to 2cm square, put in retort and heat, condensing unit passes into cooling water, the gas produced during condensation dry distilling, it is collected by 90��150 DEG C, 150��310 DEG C, 310��550 DEG C 3 temperature sections, obtains wood vinegar crude product; Or, described wood vinegar crude product can be obtained by following approach: Xylosmae japonici sawdust is pressed into the batten of 40cm �� 5cm �� 5cm, carbonization under 200 DEG C��650 DEG C conditions in dry distilling axe, the steam produced in process is derived by conduit, after two grades cool down, through soda lye wash, collect liquid, be wood vinegar crude product.
The preparation of wood vinegar extract
Embodiment 1
1, Xylosmae japonici wood vinegar crude product is prepared
By the batten being pressed into 40cm �� 5cm �� 5cm by Xylosmae japonici sawdust of 200kg, the carbonization when 650 DEG C, the steam produced in process is derived by conduit, after 2 grades of coolings, through soda lye wash, collects liquid, obtains the Xylosmae japonici wood vinegar crude product of 40kg.
2, Xylosmae japonici wood vinegar extract is prepared
A, the Xylosmae japonici wood vinegar crude product that volume is 1L is reduced pressure under the pressure of-0.1MPa and the temperature of 60 DEG C distillation 120min, obtain the first dark liquid;
B, described first dark liquid is dissolved in water obtains the first troubled liquor, the first troubled liquor described in sucking filtration, remove the insoluble particulates in described first troubled liquor, obtain 500mL the second adopting dark liquid;
C, extract described second adopting dark liquid with chloroform, extract every time and use chloroform 500mL, extracts 3 times, collect chloroform layer, by decompression distillation 30min removing chloroform at the temperature of the described chloroform layer pressure at-0.1MPa and 30 DEG C, obtain the 3rd adopting dark liquid;
D, described 3rd adopting dark liquid is dissolved in water obtains the second troubled liquor, the second troubled liquor described in sucking filtration, remove the insoluble particulates in described second troubled liquor, obtain the 4th adopting dark liquid;
E, the distillation 120min that reduced pressure under the pressure of-0.1MPa and the temperature of 50 DEG C by described 4th adopting dark liquid remove water, obtain the 5th adopting dark liquid;
F, by described 5th adopting dark liquid vacuum drying 12h under the pressure of-0.1MPa and the temperature of 50 DEG C, namely obtain described Xylosmae japonici wood vinegar extract.
Described Xylosmae japonici wood vinegar extract include as shown in table 1 the aldehydes matter of 59.022 weight %, the ether material of 28.59 weight %, the 5 hydroxymethyl furfural of 2.187 weight %, 2.236 weight % 2,3-bis-dehydration galactan, 3.421 weight % 1,6-hydroxyhexane-2-the ketone of 4:3,6-bis-dehydration ��-D-Glucopyranose. and 4.543 weight %.
Embodiment 2
1, Xylosmae japonici wood vinegar crude product is prepared
By the batten being pressed into 40cm �� 5cm �� 5cm by Xylosmae japonici sawdust of 200kg, the carbonization when 650 DEG C, the steam produced in process is derived by conduit, after two grades cool down, through soda lye wash, collects liquid, obtains the Xylosmae japonici wood vinegar crude product of 40kg.
2, Xylosmae japonici wood vinegar extract is prepared
A, the Xylosmae japonici wood vinegar crude product that volume is 1L is reduced pressure under the pressure of-0.085MPa and the temperature of 55 DEG C distillation 180min, obtain the first adopting dark liquid;
B, described first adopting dark liquid is dissolved in water obtains the first troubled liquor, the first troubled liquor described in sucking filtration, remove the insoluble particulates in described first troubled liquor, obtain 500mL the second adopting dark liquid;
Second adopting dark liquid described in c, use dichloromethane extraction, extract every time and use 500mL dichloromethane, extract 3 times, collect dichloromethane layer, decompression distillation 30min at the temperature of the described dichloromethane layer pressure at-0.085MPa and 35 DEG C is removed dichloromethane, obtains the 3rd adopting dark liquid;
D, described 3rd adopting dark liquid is dissolved in water obtains the second troubled liquor, the second troubled liquor described in sucking filtration, remove the insoluble particulates in described second troubled liquor, obtain the 4th adopting dark liquid;
E, the distillation 120min that reduced pressure under the pressure of-0.1MPa and the temperature of 50 DEG C by described 4th adopting dark liquid remove water, obtain the 5th adopting dark liquid;
F, by described 5th adopting dark liquid vacuum drying 12h under the pressure of-0.09MPa and the temperature of 50 DEG C, namely obtain described Xylosmae japonici wood vinegar extract.
The composition of described Xylosmae japonici wood vinegar extract is similar with the extract of embodiment 1, including aldehydes matter, ether material, aldehyde material and letones.
Embodiment 3
1, Xylosmae japonici wood vinegar crude product is prepared
By the batten being pressed into 40cm �� 5cm �� 5cm by Xylosmae japonici sawdust of 200kg, the carbonization when 650 DEG C, the steam produced in process is derived by conduit, after 2 grades of coolings, through soda lye wash, collects liquid, obtains the Xylosmae japonici wood vinegar crude product of 40kg.
2, Xylosmae japonici wood vinegar extract is prepared
A, the Xylosmae japonici wood vinegar crude product that volume is 1L is reduced pressure under the pressure of-0.09MPa and the temperature of 50 DEG C distillation 200min, obtain the first adopting dark liquid;
B, described first adopting dark liquid is dissolved in water obtains the first troubled liquor, the first troubled liquor described in sucking filtration, remove the insoluble particulates in described first troubled liquor, obtain 500mL the second adopting dark liquid;
C, it is extracted with ethyl acetate described second adopting dark liquid, extract every time and use 500mL ethyl acetate, extract 3 times, collect ethyl acetate layer, decompression distillation 30min at the temperature of the described ethyl acetate layer pressure at-0.09MPa and 40 DEG C is removed ethyl acetate, obtains the 3rd adopting dark liquid;
D, described 3rd adopting dark liquid is dissolved in water obtains the second troubled liquor, the second troubled liquor described in sucking filtration, remove the insoluble particulates in described second troubled liquor, obtain the 4th adopting dark liquid;
E, the distillation 120min that reduced pressure under the pressure of-0.1MPa and the temperature of 50 DEG C by described 4th adopting dark liquid remove water, obtain the 5th adopting dark liquid;
F, by described 5th adopting dark liquid vacuum drying 12h under the pressure of-0.09MPa and the temperature of 50 DEG C, namely obtain described Xylosmae japonici wood vinegar extract.
The composition of described Xylosmae japonici wood vinegar extract is similar with the extract of embodiment 1, including aldehydes matter, ether material, aldehyde material and letones.
Embodiment 4
Adopt the preparation method identical with embodiment 1, the difference is that, described organic solvent is ether.
The composition of described Xylosmae japonici wood vinegar extract is similar with the extract of embodiment 1, including aldehydes matter, ether material, aldehyde material and letones.
The composition analysis of wood vinegar extract and insecticidal effect test
1, gas chromatograph-mass spectrometer (GC-MS) (VARIAN Oncology Systems, model L1200) commonly used in the art is utilized to analyze the composition of wood vinegar extract of embodiment 1-4: DB-WAX capillary column (30m �� 0.25mm �� 0.25 ��m); Injector temperature 220 DEG C, column temperature 60 DEG C, after constant temperature 2min, with 10 DEG C/min ramp to 240 DEG C, constant temperature 8min; Split sampling 80:1; Flow rate of carrier gas 1.0mL/min. Mass Spectrometry Conditions is: EI source, electron energy 70eV; Ion source temperature 250 DEG C; Quality of scanning 35��400amu. Mass spectrum java standard library is NIST storehouse.
Wherein, shown in the constituent of the wood vinegar extract of embodiment 1 and collection of illustrative plates such as table 1 and Fig. 1.
The constituent of table 1 wood vinegar extract
2, the killing effect to bollworm
(1) with the Xylosmae japonici wood vinegar extract of embodiment 1 for insecticide, worm culture medium is supported in configuration, in culture medium insecticide concentration respectively 0,2.5,5,10,15, the Xylosmae japonici wood vinegar crude product of 20mg/mL, 20mg/mL be comparison. With 2 age bollworm carry out insecticidal test for object, for examination bollworm and aseptic feed from Hubei Province biological pesticide Engineering Research Center, insectary temperature is 27 �� 2 DEG C, relative humidity 70%, photoperiod 14:10 (L:D); The experimental subject of Xylosmae japonici wood vinegar extract and Xylosmae japonici wood vinegar crude product and bollworm are same batch. Shown in experimental result such as table 2 and Fig. 2-4.
Table 2 bollworm experience table
From table 2 and Fig. 2-4 it can be seen that the concentration of wood vinegar extract respectively 2.5,5,10,15,20mg/mL time, all can suppress the growth of bollworm, and concentration is more big, it is suppressed that act on more strong. And the concentration of wood vinegar extract respectively 15 or can kill bollworm during 20mg/mL, wherein, when concentration is 20mg/mL, the mortality rate of bollworm is up to 100%. But the Xylosmae japonici wood vinegar crude product of un-extracted also cannot kill bollworm under the concentration of 20mg/mL, almost without killing effect.
(2) with the Xylosmae japonici wood vinegar extract of embodiment 2 for insecticide, worm culture medium is supported in configuration, in culture medium insecticide concentration respectively 0,2.5,5,10,15, the Xylosmae japonici wood vinegar crude product of 20mg/mL, 20mg/mL be comparison.With 2 age bollworm carry out insecticidal test for object, for examination bollworm and aseptic feed from Hubei Province biological pesticide Engineering Research Center, insectary temperature is 27 �� 2 DEG C, relative humidity 70%, photoperiod 14:10 (L:D); The experimental subject of Xylosmae japonici wood vinegar extract and Xylosmae japonici wood vinegar crude product and bollworm are same batch. Shown in experimental result such as table 3 and Fig. 5.
Table 3 bollworm experience table
From table 3 and Fig. 5 it can be seen that the concentration of wood vinegar extract respectively 5,10,15,20mg/mL time, all can suppress the growth of bollworm, and concentration is more big, it is suppressed that act on more strong. And the concentration of wood vinegar extract respectively 15 or can kill bollworm during 20mg/mL, when concentration is 20mg/mL, the mortality rate of bollworm is 50%. But the Xylosmae japonici wood vinegar crude product of un-extracted also cannot kill bollworm under the concentration of 20mg/mL, almost without killing effect.
(3) adopt with the identical method of aforesaid operations (2) with 2 age bollworm carry out insecticidal test for object, the difference is that, with the Xylosmae japonici wood vinegar extract of embodiment 4 for insecticide. Experimental result is as shown in Figure 6.
Comparison diagram 2 and Fig. 6 can be seen that, be only that the different embodiment 1 of organic solvent is different to the growth inhibited effect of bollworm with the Xylosmae japonici wood vinegar extract of 4: when the concentration of Xylosmae japonici wood vinegar extract be all 10,15,20mg/mL time, in with the addition of the culture medium of Xylosmae japonici wood vinegar extract of embodiment 1, the size of the bollworm of growth is significantly less than the bollworm grown in adding the culture medium of Xylosmae japonici wood vinegar extract of embodiment 4, illustrates to select the Xylosmae japonici wood vinegar extract that chloroform is prepared as organic solvent that the killing effect of insect is better.
(4) in order to investigate the wood vinegar extract killing effect to the insect of all ages and classes, with the Xylosmae japonici wood vinegar extract of embodiment 1 for insecticide, worm culture medium is supported in configuration, in culture medium insecticide concentration respectively 0,2.5,5,10,15,20mg/mL. With 3 age bollworm carry out insecticidal test for object. Experimental result is as shown in Figure 7. Comparison diagram 2 is known with Fig. 7, the wood vinegar extract killing effect slightly difference to the insect of all ages and classes, this is because the insect of all ages and classes is different to the resistance of insecticide, but the conclusion obtained is consistent: the wood vinegar extract of the application can suppress the growth of bollworm and kill bollworm, and the concentration of wood vinegar extract is more big, it is suppressed that act on more strong.
3, the killing effect to beet armyworm
With the Xylosmae japonici wood vinegar extract of embodiment 1 for insecticide, worm culture medium is supported in configuration, in culture medium insecticide concentration respectively 0,2.5,5,10,15, the Xylosmae japonici wood vinegar crude product of 20mg/mL, 20mg/mL be comparison. With 2 age beet armyworm carry out insecticidal test for object, for examination beet armyworm and aseptic feed from Hubei Province biological pesticide Engineering Research Center, insectary temperature is 27 �� 2 DEG C, relative humidity 70%, photoperiod 14:10 (L:D); The experimental subject of Xylosmae japonici wood vinegar extract and Xylosmae japonici wood vinegar crude product and beet armyworm are same batch. Shown in experimental result such as table 4 and Fig. 8-9.
Table 4 beet armyworm experience table
From table 4 and Fig. 8-9 it can be seen that the concentration of wood vinegar extract respectively 2.5,5,10,15,20mg/mL time, all can suppress the growth of beet armyworm, and concentration is more big, it is suppressed that act on more strong. And the concentration of wood vinegar extract respectively 15 or can kill beet armyworm during 20mg/mL, wherein, when concentration is 20mg/mL, the mortality rate of beet armyworm is up to 100%.But the Xylosmae japonici wood vinegar crude product of un-extracted also cannot kill beet armyworm under the concentration of 20mg/mL, almost without killing effect.
4, the killing effect to diamondback moth
With the Xylosmae japonici wood vinegar extract of embodiment 1 for insecticide, worm culture medium is supported in configuration, in culture medium insecticide concentration respectively 0,1.25,2.5,5,7.5, the Xylosmae japonici wood vinegar crude product of 10mg/mL, 10mg/mL be comparison. With 3 age diamondback moth carry out insecticidal test for object, for examination diamondback moth and aseptic feed from Hubei Province biological pesticide Engineering Research Center, insectary temperature is 27 �� 2 DEG C, relative humidity 70%, photoperiod 14:10 (L:D); The experimental subject of Xylosmae japonici wood vinegar extract and Xylosmae japonici wood vinegar crude product and diamondback moth are same batch. Shown in experimental result such as table 5 and Figure 10-11.
Table 5 diamondback moth experience table
From table 5 and Figure 10-11 it can be seen that the concentration of wood vinegar extract respectively 1.25,2.5,5,7.5,10mg/mL time, all can suppress the growth of diamondback moth, and concentration is more big, it is suppressed that act on more strong. And the concentration of wood vinegar extract respectively 7.5 or can kill diamondback moth during 10mg/mL, wherein, when concentration is 10mg/mL, the mortality rate of diamondback moth is up to 100%. But the killing rate of diamondback moth is only 6.25% by the Xylosmae japonici wood vinegar crude product of un-extracted under the concentration of 10mg/mL, and killing effect is poor.
5, the killing effect to Prodenia litura
(1) with the Xylosmae japonici wood vinegar extract of embodiment 1 for insecticide, worm culture medium is supported in configuration, in culture medium insecticide concentration respectively 0,2.5,5,10,15, the Xylosmae japonici wood vinegar crude product of 20mg/mL, 20mg/mL be comparison. With 2 age Prodenia litura carry out insecticidal test for object, for the Prodenia litura tried from Henan Jiyuan Baiyun Industry Co., Ltd., aseptic feed is from Hubei Province biological pesticide Engineering Research Center, and insectary temperature is 27 �� 2 DEG C, relative humidity 70%, photoperiod 14:10 (L:D). The experimental subject of Xylosmae japonici wood vinegar extract and Xylosmae japonici wood vinegar crude product and Prodenia litura are same batch. Shown in experimental result such as table 6 and Figure 12-14.
Table 6 Prodenia litura experience table
From table 6 and Figure 12-14 it can be seen that the concentration of wood vinegar extract respectively 2.5,5,10,15,20mg/mL time, all can suppress the growth of Prodenia litura, and concentration is more big, it is suppressed that act on more strong. And the concentration of wood vinegar extract respectively 15 or can kill Prodenia litura during 20mg/mL, wherein, when concentration is 20mg/mL, the mortality rate of Prodenia litura is up to 100%. But the Xylosmae japonici wood vinegar crude product of un-extracted also cannot kill Prodenia litura under the concentration of 20mg/mL, almost without killing effect.
(2) with the Xylosmae japonici wood vinegar extract of embodiment 3 for insecticide, worm culture medium is supported in configuration, in culture medium insecticide concentration respectively 0,2.5,5,10,15, the Xylosmae japonici wood vinegar crude product of 20mg/mL, 20mg/mL be comparison. With 2 age Prodenia litura carry out insecticidal test for object, for the Prodenia litura tried from Henan Jiyuan Baiyun Industry Co., Ltd., aseptic feed is from Hubei Province biological pesticide Engineering Research Center, and insectary temperature is 27 �� 2 DEG C, relative humidity 70%, photoperiod 14:10 (L:D); The experimental subject of Xylosmae japonici wood vinegar extract and Xylosmae japonici wood vinegar crude product and Prodenia litura are same batch. Shown in experimental result such as table 7 and Figure 15.
Table 7 Prodenia litura experience table
From table 7 and Figure 15 it can be seen that the concentration of wood vinegar extract respectively 5,10,15,20mg/mL time, all can suppress the growth of Prodenia litura, and concentration is more big, it is suppressed that act on more strong.And the concentration of wood vinegar extract respectively 15 or can kill Prodenia litura during 20mg/mL, wherein, when concentration is 20mg/mL, the mortality rate of Prodenia litura is 50%. But the Xylosmae japonici wood vinegar crude product of un-extracted also cannot kill Prodenia litura under the concentration of 20mg/mL, almost without killing effect.
Utilize the present processes can to insect without the Xylosmae japonici wood vinegar crude product of killing effect extracts the Xylosmae japonici wood vinegar extract that can prevent and treat and kill insect, and described Xylosmae japonici wood vinegar extract can effectively suppress to include the growth of the various pests of bollworm, beet armyworm, diamondback moth and Prodenia litura, and is killed.
It will be understood by those within the art that, without departing from the scope of technical scheme, the equivalent variations of a little change, modification and the differentiation made when available disclosed above technology contents is the Equivalent embodiments of the application; Meanwhile, above example is made by the substantial technological of all foundation the application the change of any equivalent variations, modification and differentiation etc. are all in the scope being defined by the claims of the application.
Claims (10)
1. an Xylosmae japonici wood vinegar extract, described Xylosmae japonici wood vinegar extract includes the ketone of the phenols of 50��70 weight %, the ethers of 20��30 weight %, the aldehydes of 5��15 weight % and 2��6 weight %, and surplus is impurity.
2. Xylosmae japonici wood vinegar extract according to claim 1, wherein, described phenols includes catechol, 4-methyl pyrocatechol, 6-methoxyl group catechol, 4-ethylo benzene phosphorus diphenol, desaspidinol; Described ethers includes pyrithiobacsodium, 1,2,4-benzene three methyl ether, 2-acetonyl-4-hydroxyanisol; Described aldehydes includes 5 hydroxymethyl furfural, 2,3-bis-dehydration galactan, Isosorbide-5-Nitrae: 3,6-bis-dehydration ��-D-Glucopyranose .s; Described ketone includes 6-hydroxyhexane-2-ketone.
3. the method preparing Xylosmae japonici wood vinegar extract, described method includes:
By the decompression distillation of Xylosmae japonici wood vinegar crude product, obtain the first adopting dark liquid;
Described first adopting dark liquid is dissolved in water, removes insoluble particulates, obtain the second adopting dark liquid;
With the second adopting dark liquid described in organic solvent extraction, collecting the organic solvent layer after extracting, decompression is distilled off organic solvent, obtains the 3rd adopting dark liquid;
Described 3rd adopting dark liquid is dissolved in water, removes insoluble particulates, obtain the 4th adopting dark liquid;
Alternatively, described 4th adopting dark liquid is removed water, obtains the 5th adopting dark liquid.
4. method according to claim 3, wherein, during by the decompression distillation of Xylosmae japonici wood vinegar crude product, described decompression distillation carries out under the pressure of-0.085MPa��-0.1MPa and the temperature of 50 DEG C-60 DEG C; When the organic solvent layer decompression collected after extracting being distilled, described decompression distillation carries out under the pressure of-0.085MPa��-0.1MPa and the temperature of 30 DEG C-40 DEG C.
5. method according to claim 4, wherein, during by the decompression distillation of Xylosmae japonici wood vinegar crude product, described decompression distillation carries out under the pressure of-0.1MPa and the temperature of 60 DEG C; When the organic solvent layer decompression collected after extracting being distilled, described decompression distillation carries out under the pressure of-0.1MPa and the temperature of 30 DEG C.
6. the method according to any one of claim 3-5, wherein, described organic solvent is one or more in chloroform, ethyl acetate and dichloromethane, and alternatively, described organic solvent is chloroform.
7. the method according to any one of claim 3-5, wherein, the volume ratio of described organic solvent and described second adopting dark liquid is 1:1.
8. the Xylosmae japonici wood vinegar extract prepared by the method preparing Xylosmae japonici wood vinegar extract according to any one of claim 3-7.
9. the Xylosmae japonici wood vinegar extract described in the Xylosmae japonici wood vinegar extract that prepared by the Xylosmae japonici wood vinegar extract described in claim 1 or 2, the method according to any one of claim 3-7 or claim 8 is as the purposes of insecticide; Alternatively, described Xylosmae japonici wood vinegar extract is for the deinsectization preventing and treating of bollworm, beet armyworm, diamondback moth and Prodenia litura.
10. Xylosmae japonici wood vinegar extract described in an environmental-pollution insecticide, described insecticide contains the Xylosmae japonici wood vinegar extract described in claim 1 or 2 or prepared by the method according to any one of claim 3-7 Xylosmae japonici wood vinegar extract or claim 8 and water; Alternatively, the concentration of Xylosmae japonici wood vinegar extract described in described insecticide is 10��20mg/mL.
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