CN104886163A - Botanical pesticide compound phytolacca acinosa and magnolia officinalis microemulsion and preparation method thereof - Google Patents
Botanical pesticide compound phytolacca acinosa and magnolia officinalis microemulsion and preparation method thereof Download PDFInfo
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Abstract
The invention relates to botanical pesticide compound phytolacca acinosa and magnolia officinalis microemulsion and a preparation method thereof. The microemulsion is prepared from, by weight, 0.5-5% of total saponins of phytolacca acinosa, 0.5-5% of magnolia officinalis extracts, 1-10% of xanthium sibiricum extracts, 5-15% of calcium dodecylben-zenesulfonate, 8-20% of styrylphenol polyoxyethylene ether, 10-25% of cyclohexanone and 20-75% of water. The preparation method includes: uniformly mixing the total saponins of phytolacca acinosa, the magnolia officinalis extracts and the xanthium sibiricum extracts, adding the calcium dodecylben-zenesulfonate, the styrylphenol polyoxyethylene ether and the cyclohexanone, uniformly stirring to prepare oil phase, adding water for diluting, and stirring to obtain homogeneous-phase O/W emulsion. Since main ingredients of the microemulsion are pure natural traditional Chinese medicines, the microemulsion is safe to human and livestock, less prone to causing drug resistance of insects and germs and easy to degrade and complies with the requirements of agricultural sustainable development and human physical health, thereby being an environment-friendly botanical pesticide preparation.
Description
Technical field
The present invention relates to field of pesticide preparation, be specifically related to botanical pesticide compound Lu Piao microemulsion and preparation method thereof.
Background technology
Ecological tobacco leaf is tobacco business reducing tar and reducing harm, makes the basic guarantee of be with Chinese characteristics " Chinese-style cigarette ".Current China tobacco infectious disease reaches 68 kinds, and wherein Alternaria alternate infects the disease that causes of tobacco by the brown spot pathogen of Dendrochium, be in tobacco leaf more generally, more serious disease.And the control aspect of China to Alternaria alternate is poor at present, so far also do not set up gratifying disease-resistant variety system and develop effectively preventing medicament, the control that current China takes mainly adopts chemical agent to prevent and treat, and chemical control generally uses easy contaminated environment, direct murder by poisoning non-target organism, the chemical pesticide that damage by disease and insect easily develops immunity to drugs, therefore chemical control also can produce residue of pesticide, have a strong impact on quality of tobacco, and to environment, larger harm is brought to health, do not meet " ecological tobacco leaf " and current environmental protection, healthy, the theory of sustainable development.And from Chinese medicine, filter out the active component these tobacco diseases to preventive and therapeutic effect, be developed into botanical pesticide, can be effectively addressed this problem.
Botanical pesticide is divided into plant insecticide, bactericide and antivirotic etc., and wherein the mechanism of action of bactericidal agent for preventing and treating disease mainly contains and suppresses pathogen spore germination, mycelial growth, suppresses infecting and synthesis etc. of pathogen.Botanical pesticide derives from nature, both to people, animal safety, free from environmental pollution, not easily causes insect germ pesticide resistance, is easy to degraded at occurring in nature, has complied with again the needs that agricultural sustainable development and the mankind improve own health requirement.So research and development botanical pesticide has become the Main way of current novel agrochemical research.
Botanical pesticide, with the superiority of above-mentioned uniqueness, has become the focus of Alternaria alternate pesticide control research.Therefore further investigate the Chinese medicine with remarkable antibacterial action, extract its main Antibacterial Constituents, be developed to the botanical pesticide of control Alternaria alternate, prospect is appreciable.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, there is provided a kind of to control Alternaria alternate Be very effective, botanical pesticide compound Lu Piao microemulsion of environmental friendliness, low-residual and preparation method thereof, needed for this agricultural chemicals compound Lu Piao microemulsion, primary raw material is by the dry root of Phytolacca acinosa (Phytolacca acinosa Roxb.), the dry root of the bark of official magnolia (Magnolia officinalis Rehd1et Wils), the fruit of Siberian cocklebur (Xanthium sibiricum Parr.et Widd.) obtains through extracting processing.
For solving the problems of the technologies described above, technical scheme provided by the invention is:
There is provided a kind of botanical pesticide compound Lu Piao microemulsion, each component of raw material and mass percent thereof are:
By such scheme, the preparation method of described Phytolacca acinosa total saposins is: extract 1-4 time with 5-10 quality alcohol solution dipping doubly after being pulverized by dry for Phytolacca acinosa root, each extraction 10-30h, gained leaching liquor will be extracted at every turn and merge filtration, concentrate to obtain medicinal extract, medicinal extract is scattered in water and is heated to fully dissolve obtain the aqueous solution, filter obtained aqueous solution and use extracting n-butyl alcohol, merge butanol extraction liquid, add hot reflux 5-30 minute after adding active carbon wherein, hold over night, cross and filter active carbon residue, collect filtrate, namely evaporate to dryness obtains Phytolacca acinosa total saposins.
By such scheme, the described aqueous solution is be heated to fully dissolve obtain in 60-80 DEG C by the water of the quality such as medicinal extract is scattered in.
By such scheme, described active carbon addition is the 0.1-1% of the dry root quality of Phytolacca acinosa.
By such scheme, the preparation method of described Magnolia cortex P.E is: extract 1-4 time with 5-10 quality alcohol heating reflux doubly after being pulverized by dry for bark of official magnolia root, each extraction 1-3 hour, by extracting the merging of gained filtrate at every turn, to be concentrated into relative density be 1.1-1.3, add NaOH solution adjust ph again to 10-11, filter after leaving standstill, filtrate hydrochloric acid solution adjust ph is 1 ~ 2, hold over night, filter to obtain precipitation, precipitation is washed to neutrality, dry, add 80-150 quality cyclohexane doubly again and add hot reflux 1-3h, after filtration, filtrate reduced in volume is dry, obtain Magnolia cortex P.E.
Preferably, described NaOH solution mass concentration is 2%, and the volume after NaOH solution volume concentrates with leaching liquor is identical.
Preferably, described hydrochloric acid solution mass concentration is 2%.
By such scheme, the preparation method of described xanthium sibiricum is: extract with 5-10 quality ethanolic solution doubly after being pulverized by the dry achene of Siberian cocklebur, add hot reflux in 70-100 DEG C and keep micro-boiling, each extraction 1-3h, extract 1-4 time, extract is merged after filtering and filtrate reduced in volume is drying to obtain xanthium sibiricum.
By such scheme, described volumes of aqueous ethanol concentration is 50-98%.
The present invention also provides the preparation method of above-mentioned botanical pesticide compound Lu Piao microemulsion: first by Phytolacca acinosa total saposins, Magnolia cortex P.E and xanthium sibiricum mixing mixing, add calcium dodecyl benzene sulfonate, styrylphenol polyoxyethylene ether and cyclohexanone again, stir and make oil phase, thin up again, stirring obtains homogeneous phase O/W type emulsion and botanical pesticide compound Lu Piao microemulsion, and wherein each material quality percentage is: Phytolacca acinosa total saposins 0.5-5%; Magnolia cortex P.E 0.5-5%; Xanthium sibiricum 1-10%; Calcium dodecyl benzene sulfonate 5-15%; Styrylphenol polyoxyethylene ether 8-20%; Cyclohexanone 10-25%; Water 20-75%.
The application of above-mentioned botanical pesticide compound Lu Piao microemulsion in control Alternaria alternate, comprising: described botanical pesticide compound Lu Piao microemulsion is diluted to less than 400 times and is sprayed on tobacco surface.
Beneficial effect of the present invention is: 1, this botanical pesticide compound Lu Piao microemulsion raw material (dry root of Phytolacca acinosa, the dried root of the bark of official magnolia, the fruit of Siberian cocklebur) abundance, three Plants related to are China's conventional Chinese medicine kinds, and recovery rate is high, cost is lower, and stable processing technique, preparation section are simple, not high to equipment requirement, simple and easy to get, handling safety is feasible, is suitable for suitability for industrialized production, 2, experimental studies have found that, Phytolacca acinosa is extracted with ethanolic solution, active insecticidal components effect in the bark of official magnolia and the achene of Siberian cocklebur is better, each extract all has efficient insecticidal activity to multiple kinds of crops insect, and there is synergistic function between three kinds of extract active insecticidal components, make prepared botanical pesticide compound Lu Piao microemulsion insecticidal better effects if, and not easily make insect develop immunity to drugs, show through repeatedly field experiment result, this botanical pesticide compound Lu Piao microemulsion all has inhibitory action significantly to the sprouting of tobacco brown spot pathogen spore and mycelial growth, and increase with drug concentration, sporulation quantity obviously reduces, mycelial growth is obviously suppressed, to Alternaria alternate, there is good control efficiency, speed of action is fast, 3, this botanical pesticide microemulsion energy natural degradation, environmentally friendly, to person poultry harmless, little to pest natural enemy injury, there is the feature of low toxicity, low-residual, meet modern times " ecological tobacco leaf " and environmental protection, health, sustainable development theory to the requirement of the botanical pesticide of new and effective control Alternaria alternate.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
The preparation of Phytolacca acinosa total saposins: the pokeberry root meal 10Kg taking pulverizing, with 8 quality 70% ethanolic solution (volumetric concentration) soak extraction doubly 3 times, each lixiviate 24h, merge leaching liquor to filter, concentrate to obtain medicinal extract, make it fully dissolve heating in the water of the quality such as medicinal extract is scattered in and obtain the aqueous solution, heating-up temperature is 80 DEG C, filtering solution is also with extracting n-butyl alcohol while hot, merges butanol extraction liquid, adds 50g heating activated carbon backflow about 10 minutes, hold over night, cross and filter active carbon residue, collect filtrate, namely evaporate to dryness obtains Phytolacca acinosa total saposins.
The preparation of Magnolia cortex P.E: take bark of official magnolia meal 10Kg, carries out extraction 3 times with 6 times amount 65% ethanolic solutions, each extraction 2 hours, it is 1.2 that extract is concentrated into relative density, adds isopyknic 2%NaOH solution adjust ph to 10-11, filters after leaving standstill 2h, the hydrochloric acid solution adjust pH that filtrate adds 2% is 1 ~ 2, hold over night, filters, must precipitate, be washed to neutrality, dry, add 100 quality cyclohexane doubly and add hot reflux 2h, filter, filtrate reduced in volume is dry, obtains Magnolia cortex P.E.
The preparation of xanthium sibiricum: the Siberian cocklebur dry fruit 10Kg taking pulverizing, extracts with 95% ethanol of 6 times amount, and add hot reflux and keep micro-boiling, extract 3 times, each 2h, filter, filtrate reduced in volume is dry, obtains xanthium sibiricum.
The pokeberry extract 0.01Kg of above-mentioned preparation, Magnolia cortex P.E 0.01Kg, xanthium sibiricum 0.02Kg are mixed, add emulsifier calcium dodecyl benzene sulfonate (DBS-Ca) 0.1Kg, styrylphenol polyoxyethylene ether 0.15Kg and cosolvent (cyclohexanone) 0.2Kg again to stir and make oil phase, add 0.51Kg water again, be stirred to homogeneous phase O/W type emulsion, obtain botanical pesticide compound Lu Piao microemulsion.
Embodiment 2
The preparation of Phytolacca acinosa total saposins: the pokeberry root meal 10Kg taking pulverizing, with 5 quality 50% ethanolic solution lixiviate doubly 1 time, lixiviate 30h, merge leaching liquor to filter, concentrate to obtain medicinal extract, make it fully dissolve heating in the water of the quality such as medicinal extract is scattered in and obtain the aqueous solution, heating-up temperature is 70 DEG C, filtering solution is also with extracting n-butyl alcohol while hot, merges butanol extraction liquid, adds 10g heating activated carbon backflow about 5 minutes, hold over night, cross and filter active carbon residue, collect filtrate, namely evaporate to dryness obtains Phytolacca acinosa total saposins.
The preparation of Magnolia cortex P.E: take bark of official magnolia meal 10Kg, carries out extraction 1 time with 5 quality, 50% ethanolic solution doubly, extracts 3 hours, it is 1.1 that extract is concentrated into relative density, adds isopyknic 2wt%NaOH solution adjust ph to 10-11, filters after leaving standstill 2h, the hydrochloric acid solution adjust pH that filtrate adds 2wt% is 1 ~ 2, hold over night, filters, must precipitate, be washed to neutrality, dry, add 80 quality cyclohexane doubly and add hot reflux 1h, filter, filtrate reduced in volume is dry, obtains Magnolia cortex P.E.
The preparation of xanthium sibiricum: the Siberian cocklebur dry fruit 10Kg taking pulverizing, extracts with 50% ethanol of 5 times amount, and add hot reflux and keep micro-boiling, extract 1 time, extraction time is 3h, filters, and filtrate reduced in volume is dry, obtains xanthium sibiricum.
The pokeberry extract 0.005Kg of above-mentioned preparation, Magnolia cortex P.E 0.005Kg, xanthium sibiricum 0.01Kg are mixed, add emulsifier DBS-Ca0.05Kg, styrylphenol polyoxyethylene ether 0.08Kg and cosolvent (cyclohexanone) 0.1Kg again to stir and make oil phase, add 0.75Kg water again, be stirred to homogeneous phase O/W type emulsion, obtain botanical pesticide compound Lu Piao microemulsion.
Embodiment 3
The preparation of Phytolacca acinosa total saposins: the pokeberry root meal 10Kg taking pulverizing, with 10 quality 95% ethanolic solution lixiviate doubly 4 times, each lixiviate 10h, merge leaching liquor to filter, concentrate to obtain medicinal extract, make it fully dissolve heating in the water of the quality such as medicinal extract is scattered in and obtain the aqueous solution, heating-up temperature is 60 DEG C, filtering solution is also with extracting n-butyl alcohol while hot, merges butanol extraction liquid, adds 100g heating activated carbon backflow about 30 minutes, hold over night, cross and filter active carbon residue, collect filtrate, namely evaporate to dryness obtains Phytolacca acinosa total saposins.
The preparation of Magnolia cortex P.E: take bark of official magnolia meal 10Kg, carries out extraction 4 times with 10 quality, 95% ethanolic solution doubly, each extraction 1 hour, it is 1.3 that extract is concentrated into relative density, adds isopyknic 2%NaOH solution adjust ph to 10-11, filters after leaving standstill 2h, the hydrochloric acid solution adjust pH that filtrate adds 2% is 1 ~ 2, hold over night, filters, must precipitate, be washed to neutrality, dry, add 150 quality cyclohexane doubly and add hot reflux 3h, filter, filtrate reduced in volume is dry, obtains Magnolia cortex P.E.
The preparation of xanthium sibiricum: the Siberian cocklebur dry fruit 10Kg taking pulverizing, extracts with 10 quality, 98% ethanol doubly, and add hot reflux and keep micro-boiling, extract 4 times, each 1h, filter, filtrate reduced in volume is dry, obtains xanthium sibiricum.
The pokeberry extract 0.05Kg of above-mentioned preparation, Magnolia cortex P.E 0.05Kg, xanthium sibiricum 0.1Kg are mixed, add emulsifier DBS-Ca 0.15Kg, styrylphenol polyoxyethylene ether 0.2Kg and cosolvent (cyclohexanone) 0.25Kg again to stir and make oil phase, add 0.20Kg water again, be stirred to homogeneous phase O/W type emulsion, obtain botanical pesticide compound Lu Piao microemulsion.
Embodiment 4
Botanical pesticide compound Lu Piao microemulsion embodiment 1 prepared carries out the determination of activity of suppression tobacco brown spot pathogen:
Examination Alternaria alternate bacterial strain is supplied to be No. Al (ward is planted by academy of agricultural sciences of Hubei Province to be provided).
Experimental technique and result
1. botanical pesticide compound Lu Piao microemulsion is to the activity test of tobacco brown spot pathogen spore germination
Filter paper enzyme is adopted to measure compound Lu Piao microemulsion to the activity of tobacco brown spot pathogen spore germination.With water, compound Lu Piao microemulsion is diluted to 200 of stoste respectively, 300, 400, 500, 1000 volumes doubly, after using sterilizing filter paper (diameter 4mm) to soak above-mentioned serial dilutions respectively, put into coat tobacco brown spot pathogen spore culture medium flat plate on, to soak sterile water filter paper for blank (CK), put 28 DEG C of cultivation 8d in incubator, each process conidium under aseptic washing, at each process sporulation quantity of the micro-lower mensuration of blood counting chamber, repeated test 3 times, according to formula: sporulation quantity inhibiting rate (%)=(CK) sporulation quantity-process sporulation quantity)/CK sporulation quantity x100%, calculate sporulation quantity inhibiting rate.The results are shown in Table 1.
Table 1 affects result (CK=22.73x10 to tobacco brown spot pathogen spore germination
6individual)
Result of the test shows, compound Lu Piao microemulsion has inhibitory action significantly to tobacco brown spot pathogen spore germination, and during to dilute 200 times, inhibit activities is the highest, reaches 91.23%, and with medicament by the increase of multiple of diluting, it produces spore rejection ability and can decline to some extent.
2. compound Lu Piao microemulsion is to the activity test of tobacco brown spot pathogen mycelial growth
Adopt the activity that mycelial growth rate method mensuration compound Lu Piao microemulsion grows Alternaria alternate mycelia.Mix after compound Lu Piao microemulsion dilute with water with medium, make the pastille flat board that concentration is respectively 200,300,400,500,1000 times of stoste dilution, in the access of dull and stereotyped central authorities with a collection of tobacco brown spot pathogen cake, with dull and stereotyped for blank (CK) without medicine, in incubator after 28 DEG C of cultivation 5d, measure antibacterial circle diameter by slide measure right-angled intersection method; Continue to cultivate after 8d, with process conidium each under aseptic washing, at the micro-lower mensuration of blood counting chamber sporulation quantity separately.Test repetition 3 times.According to formula: fungistatic effect (%)=(blank colony diameter-process colony diameter)/(blank bacterium colony size-bacterium cake diameter) x100%; Sporulation quantity inhibiting rate (%)=(blank sporulation quantity-process sporulation quantity)/blank sporulation quantity x 100%, calculates fungistatic effect and sporulation quantity inhibiting rate respectively.The results are shown in Table 2 and table 3.
Table 2 compound Lu Piao microemulsion is to tobacco brown spot pathogen bacteriostatic test result (CK=4.237)
Table 3 sporulation quantity inhibition test result (CK=22.75x10
6individual)
Botanical pesticide compound Lu Piao microemulsion prepared by embodiment 2 and 3 is carried out the determination of activity of suppression tobacco brown spot pathogen, and test result is similar to botanical pesticide compound Lu Piao microemulsion prepared by embodiment 1.
Result of the test shows, compound Lu Piao microemulsion of the present invention is obvious to tobacco brown spot pathogen mycelial growth inhibition, and also has obvious inhibitory action to brown spot pathogen bacterium colony sporulation quantity, and increases with drug concentration, mycelial growth is obviously suppressed, and sporulation quantity obviously reduces.Wherein during dilution 200 times, its fungistatic effect reaches 93.50%.By pharmacodynamics test, prove that this invention has preventive and therapeutic effect preferably to Alternaria alternate, be diluted to less than 400 times available.
Claims (7)
1. a botanical pesticide compound Lu Piao microemulsion, is characterized in that each component of raw material and mass percent thereof are:
2. botanical pesticide compound Lu Piao microemulsion according to claim 1, it is characterized in that, the preparation method of described Phytolacca acinosa total saposins is: extract 1-4 time with 5-10 quality alcohol solution dipping doubly after being pulverized by dry for Phytolacca acinosa root, each extraction 10-30h, gained leaching liquor will be extracted at every turn and merge filtration, concentrate to obtain medicinal extract, medicinal extract is scattered in water and is heated to fully dissolve obtain the aqueous solution, filter obtained aqueous solution and use extracting n-butyl alcohol, merge butanol extraction liquid, hot reflux 5-30 minute is added after adding active carbon wherein, hold over night, cross and filter active carbon residue, collect filtrate, namely evaporate to dryness obtains Phytolacca acinosa total saposins.
3. botanical pesticide compound Lu Piao microemulsion according to claim 1, it is characterized in that, the preparation method of described Magnolia cortex P.E is: extract 1-4 time with 5-10 quality alcohol heating reflux doubly after being pulverized by dry for bark of official magnolia root, each extraction 1-3 hour, by extracting the merging of gained filtrate at every turn, to be concentrated into relative density be 1.1-1.3, add NaOH solution adjust ph again to 10-11, filter after leaving standstill, filtrate hydrochloric acid solution adjust ph is 1-2, hold over night, filter to obtain precipitation, precipitation is washed to neutrality, dry, add 80-150 quality cyclohexane doubly again and add hot reflux 1-3h, after filtration, filtrate reduced in volume is dry, obtain Magnolia cortex P.E.
4. botanical pesticide compound Lu Piao microemulsion according to claim 1, it is characterized in that, the preparation method of described xanthium sibiricum is: extract with 5-10 quality ethanolic solution doubly after being pulverized by the dry achene of Siberian cocklebur, add hot reflux and keep micro-boiling, each extraction 1-3h, extract 1-4 time, extract is merged after filtering and filtrate reduced in volume is drying to obtain xanthium sibiricum.
5., according to the arbitrary described botanical pesticide compound Lu Piao microemulsion of claim 2-4, it is characterized in that, described volumes of aqueous ethanol concentration is 50-98%.
6. the preparation method according to the arbitrary described botanical pesticide compound Lu Piao microemulsion of claim 1-5, it is characterized in that: first by Phytolacca acinosa total saposins, Magnolia cortex P.E and xanthium sibiricum mixing mixing, add calcium dodecyl benzene sulfonate, styrylphenol polyoxyethylene ether and cyclohexanone again, stir and make oil phase, thin up again, stirring obtains homogeneous phase O/W type emulsion and botanical pesticide compound Lu Piao microemulsion, and wherein each material quality percentage is: Phytolacca acinosa total saposins 0.5-5%; Magnolia cortex P.E 0.5-5%; Xanthium sibiricum 1-10%; Calcium dodecyl benzene sulfonate 5-15%; Styrylphenol polyoxyethylene ether 8-20%; Cyclohexanone 10-25%; Water 20-75%.
7., according to the application of the arbitrary described botanical pesticide compound Lu Piao microemulsion of claim 1-5 in control Alternaria alternate, it is characterized in that: described botanical pesticide compound Lu Piao microemulsion is diluted to less than 400 times and is sprayed on tobacco surface.
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| CN105647285A (en) * | 2016-03-31 | 2016-06-08 | 黄山市古城歙砚有限公司 | Environment-friendly ink and preparation method thereof |
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| CN107787799A (en) * | 2017-11-01 | 2018-03-13 | 融安县飞腾中草药专业合作社 | A kind of coltsfoot implantation methods |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105580848A (en) * | 2016-03-11 | 2016-05-18 | 史运江 | Biopesticide for preventing and treating tobacco brown spot and preparation method |
| CN105647285A (en) * | 2016-03-31 | 2016-06-08 | 黄山市古城歙砚有限公司 | Environment-friendly ink and preparation method thereof |
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| CN107056418A (en) * | 2017-02-16 | 2017-08-18 | 梁慰爱 | A kind of mulch base manure and preparation method thereof |
| CN107787799A (en) * | 2017-11-01 | 2018-03-13 | 融安县飞腾中草药专业合作社 | A kind of coltsfoot implantation methods |
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Application publication date: 20150909 |
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