CN105145563B - A kind of composition pesticide and application thereof - Google Patents
A kind of composition pesticide and application thereof Download PDFInfo
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- CN105145563B CN105145563B CN201510667070.7A CN201510667070A CN105145563B CN 105145563 B CN105145563 B CN 105145563B CN 201510667070 A CN201510667070 A CN 201510667070A CN 105145563 B CN105145563 B CN 105145563B
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Abstract
The present invention relates to a kind of composition pesticide.It includes limonene, linalool, α terpinols, citral and beta pinene.The present invention is not only that the utilization of active material in citrus provide new way, also for the active material in citrus is provided into foundation applied to agricultural chemicals research and development.
Description
Technical field
The present invention relates to application of the composition pesticide in terms of pest control, more particularly to a kind of composition pesticide and its use
On the way.
Background technology
In recent years, domestic and foreign scholars have done substantial amounts of research work to the screening of antibacterial Insecticidal Plant Resource, it was found that many
Plant resources with antimicrobial and insecticidal activity.For example, Wilson etc. filters out 13 kinds from 345 kinds of plants and 49 kinds of plants essential oils
Plant and 4 kinds of essential oils have stronger bacteriostatic activity.And for example, navel orange and the essential oil pair of lemon peel extraction are pointed out in the research such as Ezeonu
Mosquito, cockroach and housefly fumigating effect are preferable, it is found that sweet orange oil has preferable desinsection potentiality, particularly sensitive to cockroach, are
Further the newtype drug of exploitation preventing and treating cockroach has certain directive significance.
Citrus is perennial evergreen dungarunga, and aboundresources, improved seeds are various, is gone through with the cultivation of more than 4,000 years
History, it is currently the maximum fruit of China's production area.However, the processing of citrus can produce largely discarded skin slag during producing.
Skin slag is discarded for these, recycling and the major way of processing have at present:Sanitary landfills, extraction effective active matter,
Produce organic fertilizer etc..Desinsection and Substance therein are researched and developed, is the preferable approach of citrus peel residue comprehensive utilization.Closely
Over a little years, the active material in citrus is increasingly paid attention in the effect of preventing and treating agricultural pests etc., but its desinsection is main
Composition and mechanism is not also fully aware of at present.
At present, although being related to the correlative study of the desinsection and bacteriostatic activity of active material in citrus, these grind
Active material mentioned in studying carefully, which can play application and mode of insecticidal action etc., still certain limitation, while these
It is what respectively that research, which does not all specify contained desinsection and antibacterial active material in its extract, yet, therefore has further research
Necessity.
The content of the invention
The first object of the present invention is to provide a kind of composition pesticide, and the composition pesticide can be used as efficiently killing citrus
The insecticide pesticide of Panonychus citri.
Technical scheme is specific as follows:
A kind of composition pesticide, it is characterised in that:It includes limonene, linalool, alpha-terpineol, citral and β-pinane
Alkene.
Limited as further, above-mentioned composition pesticide specifically can by limonene, linalool, alpha-terpineol, citral and
Nopinene forms.
As further clearly, the amount ranges of above-mentioned each material, in parts by weight meter be respectively limonene 30~
0.01~2 part of 60 parts, 0.5~5 part of linalool, 0.05~3 part of alpha-terpineol, 0.2~5 part of citral and nopinene.
As still more preferably, the dosage of above-mentioned each material, in parts by weight meter are respectively 55 parts of limonene, fragrant camphor tree
1 part of 5 parts of alcohol, 3 parts of alpha-terpineol, 5 parts of citral and nopinene.
Above-mentioned composition pesticide in the present invention, it can be used as killing the insecticide pesticide of panonychus citri.
The invention has the advantages that:
The invention discloses a kind of composition pesticide, and it can be used as a kind of agricultural chemical insecticide, have to panonychus citri good
Good killing action, its corrected mortality to 3 kinds of worm states of panonychus citri is respectively greater than 83%, 86%, 89%, complete to citrus
The female of pawl mite has excellent contact toxicity into mite, deutonymph, ovum.It is not only in citrus the utilization of active material provide
New way, also for the active material in citrus is provided into foundation applied to agricultural chemicals research and development.
Embodiment
The present invention is specifically described below by specific embodiment, it is pointed out here that following examples are served only for this hair
It is bright to be further described, it is impossible to be interpreted as limiting the scope of the invention, the person skilled in the art of this area can root
Some nonessential modifications and adaptations are made to the present invention according to foregoing invention content.
Embodiment 1
A kind of composition pesticide, it is by limonene, linalool, alpha-terpineol, citral, nopinene, hendecane, adjacent diformazan
Benzene and n-nonyl alcohol composition;The dosage of its each material, in parts by weight meter are respectively 55 parts of limonene, 5 parts of linalool, α-pine tar
1 part of 3 parts of alcohol, 5 parts of citral, 1 part of nopinene, 2 parts of hendecane, 2 parts of ortho-xylene and n-nonyl alcohol.
To draw the composition of above-mentioned composition pesticide, this example has also specifically carried out following 3 kinds and probed into:
Dry, pulverized and sieved after 50 DEG C of drying, afterwards according to solid-liquid ratio 1. the pericarp of northern a word used in place name 447 and seed are cleaned respectively
Petroleum ether, absolute ethyl alcohol, acetone, ethyl acetate, preservative film sealing, 50 DEG C of ultrasonic extractions are separately added into for 12.5mL/g
40min, it is filtered under diminished pressure, in triplicate, then the paste by the filtrate decompression concentration gained of collection;2. tangerine oil (red tangerine pericarp
Extract);3. orange oil (Citrus sinensis Osbeck pericarp extract).
The northern pericarp of a word used in place name 447,4 kinds of solvent extractable matters of seed and tangerine oil, orange oil are ground to the contact toxicity of citrus red mite (crm)
Study carefully:
Determined using slide infusion process:4 kinds of solvent extractable matter 1mL of the northern pericarp of a word used in place name 447, seed, tangerine oil are taken respectively
1mL, orange oil 1mL, 1mL Tween-80s and 8mL absolute ethyl alcohols are added, be configured to 10% compound decoction, be diluted to 50 times
Liquid.Under anatomical lens by it is female into mite, deutonymph foot towards day, the back of the body it is directed downwardly be pasted onto on the slide with double faced adhesive tape, every 40,
Every kind of medicament repeats 3, after mite body is stable, rejects dead and injured individual, after slide is impregnated in every kind of decoction 5 respectively
Second, unnecessary decoction is drawn, is compareed with clear water, dead number is checked after 24 hours, is touched with writing brush, motionless person is death.Adopt
Examined with T and Duncan methods analyze contact toxicity of each extract to citrus red mite (crm), P < 0.05 represent significant difference, and it is tied
Fruit sees below Tables 1 and 2:
The northern pericarp of a word used in place name 447 of table 1, the acaricidal activity of 4 kinds of solvent extractable matters of seed
It can be seen from table 1:4 kinds of northern pericarp of a word used in place name 447, seed solvent extractable matters all show preferable contact toxicity, wherein,
The acaricidal activity highest of ethanol extract, pericarp ethanol extract kill it is female into mite rate up to 76.23%, it is reachable to kill deutonymph effect
82.15%, the hatching inhibiting rate to ovum is up to 90.21%.
The tangerine oil of table 2, orange oil are to the contact toxicity of citrus red mite (crm)
It can be seen from table 2:Tangerine oil, orange oil all show good contact toxicity to 3 kinds of worm states of citrus red mite (crm), right
Young mite, the activity of ovum are all more than 50%.
Research is understood more than:Contain all there are 3 kinds of worm states of citrus red mite (crm) in citrus extracts and well tag
The active material of activity.
In order to which which active material clear and definite wherein acaricidal activity composition mainly includes, then need by citrus extracts
Middle active component carries out GC-MS analyses and determined, is also to have carried out analysis below in this this example:
(1) material to be tested:The pericarp ethanol extract of northern a word used in place name 447, seed ethanol extract, the extraction of pericarp ethyl acetate
Thing, seed ethyl acetate extract;
(2) key instrument:7890A/5975C gas chromatograph-mass spectrometers (GC-MS)
(3) the GC-MS analyses of the pericarp of northern a word used in place name 447, seed extract:4 kinds of extractions in 3mL materials to be tested are weighed respectively
Thing, it is put in 20mL screw socket sample bottles, adds 3.0g sodium chloride, is sealed with polytetrafluoroethylene (PTFE) dottle pin, in 40 DEG C of magnetic stirring apparatus
Upper balance heating 15 minutes, with DVB/CAR/PDMS50/30um extracting heads headspace absorption 40 minutes, extracting head insertion GC is entered
Sample, parse 5 minutes;The amount of internal standard compound:2uL cyclohexanone;Chromatographic condition:Chromatographic column:HP-5MS;Carrier gas:Helium 1mL/min:Enter
Sample mouth temperature:250 DEG C, Splitless injecting samples;Temperature programming:35 DEG C are kept for 5 minutes, and rising to 180 DEG C with 3 DEG C/min is kept for 2 minutes,
240 DEG C are risen to 5 DEG C/min again, is kept for 2 minutes;Mass Spectrometry Conditions:Interface temperature:280℃:Ion source temperature:230 DEG C of quadrupole rods
Temperature:150℃;Ionization mode:EI;Electron energy:70eV;Mass range:35-400;Chemical substance analysis software:
7890A/5975C gas chromatograph-mass spectrometers (GC-MS), 7683B automatic sampling instruments, NIST08 spectrums storehouse.
Constituent analysis, equal major diagnostic are carried out to above-mentioned citrus extracts by gas chromatography-mass spectrography (GC-MS) respectively
36 kinds of compounds are gone out, its content meter by mass percentage, using limonene as main component, and by monoterpene and sequiterpene olefinic carbon
Hydrogen compound and its containing oxygen derivative such as material composition such as higher alcohols, aldehydes, acids, esters, also containing a small amount of aldehyde, alcohol and
The oxygenatedchemicals such as ketone.In view of other chemical composition contents are relatively low, 24 kinds of derived essential oils therein are mainly determined in this example
Action of contace poison, screening have preferable contact toxicity and the derived essential oil compared with strong virus force, are laid the foundation for its application:
Main component in the ethanol of citrus, ethyl acetate extract is female to panonychus citri to tag into mite, deutonymph, ovum
Activity and toxicity test research:
1. to the female into mite, the contact toxicity of deutonymph and toxicity test of panonychus citri:
Under anatomical lens, it is pasted onto facing downward on the slide with double faced adhesive tape towards day, the back of the body into mite, young mite foot female, often
Piece 40, every kind of extract is repeated 3 times, and after mite body is stable, rejects dead and injured individual.With beaker by every kind of extract
A series of concentration gradients are diluted to, then slide is impregnated in wherein 5 seconds, unnecessary decoction is drawn, is compareed with clear water, 24 is small
When after check dead number, touched with writing brush, motionless person for death.Data statistic analysis is carried out with DPS softwares, calculates virulence time
Return straight line, coefficient correlation (R2) and median effective concentration (LC50);
2. to the contact toxicity and toxicity test of the ovum of panonychus citri:
The thick sponges of 0.7cm are spread on clean pallet, the height of sponge is added water to, then spreads filter paper, formed every
Water platform, complete, smooth, fresh blade is chosen as on water proof platform, then blade edge is surrounded with cotton, is chosen with No. zero writing brush
It is female into mite that body colour is bright-coloured, volume is larger, is transferred on blade and is cultivated, every leaf is inoculated with 60, in 25 degree of temperature, humidity
85%th, cultivated one day under the incubator of illumination L: D=16: 8H, make its spawning, be diluted to every kind of extract with beaker a series of
Concentration gradient, the blade with ovum is then impregnated in decoction 5 seconds, draws unnecessary decoction, compareed with clear water, seen day by day after 5 days
The hatching situation of ovum is examined, does not hatch and is considered as death.Data statistic analysis is carried out with DPS softwares, calculates toxicity regression straight line, correlation
Coefficient (R2) and median effective concentration (LC50)。
24 kinds of derived essential oils in the citrus extracts of table 3 to panonychus citri it is female into mite, deutonymph, ovum contact toxicity
It can be seen from table 3:Some in 24 kinds of derived essential oils in citrus extracts shows preferable contact toxicity.
To in the female contact toxicity research into mite of panonychus citri, limonene, citral, the corrected mortality of nopinene are more than
60%, kill female high into mite activity;The corrected mortality of alpha-terpineol, linalool etc. is killed in the female activity into mite 30%~60%
Deng;Killing for remaining chemical composition is female poor into mite activity.In contact toxicity research to the deutonymph of panonychus citri, limonene
Corrected mortality it is maximum, be 80.70%, kill deutonymph activity highest;Citral, the corrected mortality of nopinene are more than 60%,
It is high to kill deutonymph activity;It is medium to kill deutonymph activity 30%~60% for the corrected mortality of alpha-terpineol, linalool etc.;Remaining is changed
Polymer component kills that deutonymph activity is poor, and effect is not notable.To in the research of the contact toxicity of panonychus citri ovum, limonene ovicidal
Active highest, it is 84.45%, alpha-terpineol takes second place, and is 81.20%, and citral ovicidal activity is 61.26%, and nopinene is
68.48%, linalool 51.29%, remaining composition ovicidal activity is poor.Accordingly, it is determined that limonene, linalool, alpha-terpineol,
Citral and nopinene are the main active ingredient that citrus extracts kill panonychus citri.
To verify said determination result, in this example with reference in the ethanol of above-mentioned citrus, ethyl acetate extract it is main into
Point the female research method into mite, deutonymph, the contact toxicity of ovum and toxicity test of panonychus citri is determined respectively limonene,
Linalool, nopinene, alpha-terpineol and the single derived essential oil of 5 kinds of citral grab the female into mite, deutonymph, ovum of mite to citrus entirely
Toxicity test, and also it is additionally arranged 15% pyridaben missible oil as a comparison, its measurement result see the table below shown in 4-6:
45 kinds of derived essential oil virulence regression equations into mite female to citrus red mite (crm) of table
It can be seen from table 4:Female LC into mite of the above-mentioned 5 kinds of derived essential oils to panonychus citri500.0592~
0.1412mg/mL, it is close with 15% pyridaben missible oil activity, wherein, limonene virulence is most strong, next be followed successively by citral, β-
Firpene, alpha-terpineol, linalool.
Virulence regression equation of the 55 kinds of derived essential oils of table to the deutonymph of citrus red mite (crm)
It can be seen from table 5:LC of the above-mentioned 5 kinds of derived essential oils to panonychus citri deutonymph50In 0.2301~0.6054mg/
ML, it is close with 15% pyridaben missible oil activity, wherein, the virulence of limonene is most strong, next be followed successively by citral, nopinene, α-
Terpinol, linalool.
Virulence regression equation of the 65 kinds of derived essential oils of table to the ovum of citrus red mite (crm)
It can be seen from table 6:LC of the above-mentioned 5 kinds of derived essential oils to panonychus citri ovum50In 0.0658~0.1385mg/ml,
Wherein, the virulence of limonene is most strong, and next is followed successively by alpha-terpineol, citral, linalool, nopinene.
It can confirm that by above checking test:If in the active component of citrus extracts to citrus red mite (crm) it is female into mite,
Mite, ovum contact toxicity in, limonene, linalool, nopinene, alpha-terpineol and citral show preferable contact toxicity,
The main active ingredient of panonychus citri is killed for citrus extracts.
Probed into more than, should for ease of production after the main 5 kinds of active ingredients for panonychus citri of tagging are determined
With and further improve the corrected mortality of panonychus citri of tagging simultaneously, this example also by further probing into, has been drawn by upper
The composition pesticide that five kinds of active ingredients form according to optimum ratio is stated, and has been carried out according to the method described above to panonychus citri
Female contact toxicity and toxicity test into mite, deutonymph and ovum:
In composition pesticide in this example of table 7 and its composition each individually active material to panonychus citri it is female into
Mite, deutonymph, the contact toxicity of ovum
Embodiment 2
A kind of composition pesticide, it is by limonene, linalool, alpha-terpineol, citral, nopinene, hendecane, adjacent diformazan
Benzene, n-nonyl alcohol, dipentene, geranyl acetate, vanillic aldehyde and citronellal composition;The dosage of its each material, is counted in parts by weight
Respectively 65 parts of limonene, 6 parts of linalool, 5 parts of alpha-terpineol, 6 parts of citral, 2 parts of nopinene, 3 parts of hendecane, ortho-xylene
0.5 part of 3 parts, 2 parts of n-nonyl alcohol, 1 part of dipentene, 1 part of geranyl acetate, 0.5 part of vanillic aldehyde and citronellal.
Embodiment 3-9
A kind of composition pesticide, it is made up of limonene, linalool, alpha-terpineol, citral and nopinene;Its each thing
The dosage of matter, is counted in parts by weight, as shown in the table respectively:
Embodiment | Limonene | Linalool | Alpha-terpineol | Citral | Nopinene |
3 | 29.20 | 5.57 | 0.05 | 0.27 | 2.01 |
4 | 58.70 | 0.70 | 0.80 | 0.15 | 0.47 |
5 | 45.26 | 2.98 | 1.16 | 1.71 | 1.42 |
6 | 34.48 | 1.59 | 0.34 | 3.38 | 1.06 |
7 | 61.02 | 2.86 | 2.14 | 4.14 | 0.50 |
8 | 35.16 | 4.11 | 3.19 | 5.03 | 2.22 |
9 | 54.71 | 4.89 | 3.02 | 2.98 | 0.43 |
According to the method described in embodiment 1, the composition pesticide of gained in embodiment 2-9 is respectively adopted to the full pawl of citrus
The female contact toxicity and toxicity test into mite, deutonymph and ovum of mite:
Composition pesticide in the embodiment 2-9 of table 8 to panonychus citri it is female into mite, deutonymph, ovum contact toxicity
Claims (4)
- A kind of 1. composition pesticide, it is characterised in that:Meter includes 30~60 parts of limonene, linalool 0.5~5 in parts by weight Part, 0.05~3 part of alpha-terpineol, 0.2~5 part of citral and 0.01~2 part of nopinene.
- 2. composition pesticide as claimed in claim 1, it is characterised in that:Count in parts by weight by 30~60 parts of limonene, fragrant camphor tree 0.01~2 part of 0.5~5 part of alcohol, 0.05~3 part of alpha-terpineol, 0.2~5 part of citral and nopinene composition.
- 3. composition pesticide as claimed in claim 1 or 2, it is characterised in that:The dosage of each material, is counted in parts by weight Respectively 1 part of 55 parts of limonene, 5 parts of linalool, 3 parts of alpha-terpineol, 5 parts of citral and nopinene.
- 4. application of the composition pesticide in as the insecticide pesticide for killing panonychus citri as described in claim 1-3 is any.
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