CN105123789B - A kind of free anthraquinones extracted from rheum nano-emulsion preparation for being used to prevent and treat plant red spider disease - Google Patents
A kind of free anthraquinones extracted from rheum nano-emulsion preparation for being used to prevent and treat plant red spider disease Download PDFInfo
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- CN105123789B CN105123789B CN201510623246.9A CN201510623246A CN105123789B CN 105123789 B CN105123789 B CN 105123789B CN 201510623246 A CN201510623246 A CN 201510623246A CN 105123789 B CN105123789 B CN 105123789B
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- 239000007908 nanoemulsion Substances 0.000 title claims abstract description 53
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 52
- 241000219061 Rheum Species 0.000 title claims abstract description 46
- 241000488583 Panonychus ulmi Species 0.000 title claims abstract description 30
- 241000196324 Embryophyta Species 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 201000010099 disease Diseases 0.000 title claims abstract description 19
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 title claims abstract description 19
- 239000003814 drug Substances 0.000 claims abstract description 20
- 240000004980 Rheum officinale Species 0.000 claims abstract description 15
- 235000008081 Rheum officinale Nutrition 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000284 extract Substances 0.000 claims abstract description 7
- 239000003381 stabilizer Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 235000001018 Hibiscus sabdariffa Nutrition 0.000 claims abstract description 3
- 235000005291 Rumex acetosa Nutrition 0.000 claims abstract description 3
- 240000007001 Rumex acetosella Species 0.000 claims abstract description 3
- 235000003513 sheep sorrel Nutrition 0.000 claims abstract description 3
- -1 polyoxyethylene Polymers 0.000 claims description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- GHHURQMJLARIDK-UHFFFAOYSA-N 2-hydroxypropyl octanoate Chemical compound CCCCCCCC(=O)OCC(C)O GHHURQMJLARIDK-UHFFFAOYSA-N 0.000 claims description 5
- LVGKNOAMLMIIKO-UHFFFAOYSA-N Elaidinsaeure-aethylester Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC LVGKNOAMLMIIKO-UHFFFAOYSA-N 0.000 claims description 5
- 229940093471 ethyl oleate Drugs 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 5
- 235000010234 sodium benzoate Nutrition 0.000 claims description 5
- 239000004299 sodium benzoate Substances 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- NTQGILPNLZZOJH-UHFFFAOYSA-N disilicon Chemical compound [Si]#[Si] NTQGILPNLZZOJH-UHFFFAOYSA-N 0.000 claims description 4
- LVGKNOAMLMIIKO-QXMHVHEDSA-N ethyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC LVGKNOAMLMIIKO-QXMHVHEDSA-N 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000008213 purified water Substances 0.000 claims description 3
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- 235000019438 castor oil Nutrition 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
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- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 229940035423 ethyl ether Drugs 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 230000002045 lasting effect Effects 0.000 claims 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-M octanoate Chemical compound CCCCCCCC([O-])=O WWZKQHOCKIZLMA-UHFFFAOYSA-M 0.000 claims 1
- 239000003995 emulsifying agent Substances 0.000 abstract description 22
- 230000000694 effects Effects 0.000 abstract description 16
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- 241000239290 Araneae Species 0.000 description 2
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- 206010059866 Drug resistance Diseases 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- LQGUBLBATBMXHT-UHFFFAOYSA-N chrysophanol Chemical compound C1=CC=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O LQGUBLBATBMXHT-UHFFFAOYSA-N 0.000 description 2
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- FFWOKTFYGVYKIR-UHFFFAOYSA-N physcion Chemical compound C1=C(C)C=C2C(=O)C3=CC(OC)=CC(O)=C3C(=O)C2=C1O FFWOKTFYGVYKIR-UHFFFAOYSA-N 0.000 description 2
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- CTKXFMQHOOWWEB-UHFFFAOYSA-N Ethylene oxide/propylene oxide copolymer Chemical compound CCCOC(C)COCCO CTKXFMQHOOWWEB-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- UGNZSMZSJYOGNX-UHFFFAOYSA-N Isoviocristine Natural products O=C1C=C(C)C(=O)C2=CC3=CC(OC)=CC(O)=C3C(O)=C21 UGNZSMZSJYOGNX-UHFFFAOYSA-N 0.000 description 1
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical class CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
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- FHNINJWBTRXEBC-UHFFFAOYSA-N Sudan III Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 FHNINJWBTRXEBC-UHFFFAOYSA-N 0.000 description 1
- 241001454295 Tetranychidae Species 0.000 description 1
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- 241000607479 Yersinia pestis Species 0.000 description 1
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- WLXGUTUUWXVZNM-UHFFFAOYSA-N anthraglycoside A Natural products C1=C(C)C=C2C(=O)C3=CC(OC)=CC(O)=C3C(=O)C2=C1OC1OC(CO)C(O)C(O)C1O WLXGUTUUWXVZNM-UHFFFAOYSA-N 0.000 description 1
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- NZPQWZZXRKZCDU-UHFFFAOYSA-N chrysophanol Natural products Cc1cc(O)c2C(=O)c3c(O)cccc3Oc2c1 NZPQWZZXRKZCDU-UHFFFAOYSA-N 0.000 description 1
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- UOAMTSKGCBMZTC-UHFFFAOYSA-N dicofol Chemical compound C=1C=C(Cl)C=CC=1C(C(Cl)(Cl)Cl)(O)C1=CC=C(Cl)C=C1 UOAMTSKGCBMZTC-UHFFFAOYSA-N 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
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- 235000010228 ethyl p-hydroxybenzoate Nutrition 0.000 description 1
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- NUVBSKCKDOMJSU-UHFFFAOYSA-N ethylparaben Chemical compound CCOC(=O)C1=CC=C(O)C=C1 NUVBSKCKDOMJSU-UHFFFAOYSA-N 0.000 description 1
- NYPJDWWKZLNGGM-UHFFFAOYSA-N fenvalerate Chemical compound C=1C=C(Cl)C=CC=1C(C(C)C)C(=O)OC(C#N)C(C=1)=CC=CC=1OC1=CC=CC=C1 NYPJDWWKZLNGGM-UHFFFAOYSA-N 0.000 description 1
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- Medicinal Preparation (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to biological pesticide technical field, and in particular to the prescription and preparation technology of free anthraquinones extracted from rheum nano-emulsion preparation, and the application in preventing and treating plant red spider disease.The free anthraquinones extracted from rheum extracts from Chinese medicine sorrel, Rheum tanguticum Maxim or Rheum officinale.In terms of the mass percent of contained each component in nano-emulsion, free anthraquinones extracted from rheum content is 0.05~0.16% in nanoemulsion, and the oil phase in nano-emulsion accounts for 18~22%, emulsifying agent 16~20%, assistant for emulsifying agent 4~6%, water 50~61%, stabilizer 1.0%, preservative 0.1%, adhesive agent 0.1%.The free anthraquinones extracted from rheum nano-emulsion preparation can be used for preventing and treating plant red spider disease.Dissociated anthraquinone in free anthraquinones extracted from rheum nano-emulsion disclosed by the invention derives from Chinese herb rhubarb, extraction process strong applicability, the cost that raw material is obtained is low, prepared by nano-emulsion is simple, quality controllable by spontaneously form, technique, it is easy to large-scale production, and excellent prevention effect is showed to plant red spider disease.
Description
Technical field
The invention belongs to pesticide field, more particularly to a kind of free anthraquinones extracted from rheum for being used to prevent and treat plant red spider disease is received
Rice milk preparation.
Background technology
Plant red spider disease is widely present on the plant stem-leafs such as various crops, vegetables, flowers, trees, main harm eggplant
The crops such as section, Curcurbitaceae, pulse family, Liliaceae and grass family.The red spider species of China belongs to spider shape based on Tetranychus cinnabarinus
Guiding principle, Acarina, Tetranychidae, extensively, feeding habits are miscellaneous, can endanger 110 various plants for distributed areas.Red spider breeding amount is big, and polypide is small
It is difficult to find, when its harm is found, transfer velocity is fast, and insect pest area is big, and infection crops are repeated several times.Hazard approach
It is to be pierced into blade to suck juice with mouthpart, is destroyed chlorophyll, sallow point or patch is presented in blade, until whole blade
It is orange, come off, it is serious to hinder the normal growth and development of plant, and cause huge economic loss.The agricultural chemicals being currently mainly used
There is the preventing and treating plant red spider disease such as net, Belmark of propargite, dicofol, Rogor, pink bollworm.But with the length of chemical agent
Time uses, and the red spider resistance different degrees of to which creating, prevention effect is greatly lowered, and chemical agent environment is dirty
Dye and the drawback such as high residue increasingly show.Therefore, small toxicity is developed, pollution is small, remain less, be avoided that the biological agriculture of drug resistance
Medicine is the task of top priority.
Botanical fungicide has to person poultry safety, environment-friendly, can natural degradation and the advantages of noresidue.Rheum officinale [bag
Sorrel (Rheum palmatum) is included, secondary is Rheum tanguticum Maxim (Rheum palmatum var.tanguticum) and medicine
With rheum officinale (Rheum officinale)] be one of conventional plant source Chinese medicine, its extract has rush down under, anti-infective and nerve
Protection activity etc. is acted on, but has no its inhibitory or killing effect research to plant red spider.Pharmaceutical dosage form can to the prevention effect of medicine
Significant impact is produced, such as wettable powder and supensoid agent only pass through solid drug particles and the pathogenic microorganism on plant surface
Contact and suppression is presented and kills activity, it is poor to kill effect to the suppression of the pathogenic microorganisms of inside plants；Missible oil plant surface adhesiveness,
Ductility is not good, it is impossible to farthest plays the effect of medicine；The particle diameter of microemulsion is generally in micron order, it is impossible to effectively pass through
The epidermis of plant stem-leaf and press down the pathogenic microorganism for killing inside plants tissue.Nano-emulsion is smaller because playing particle diameter, with good stream
Dynamic property, can more effectively penetrate into plant base of leaf, play the bioactivity of medicine, and preparation technology it is simple, can with water with
Arbitrary proportion is mixed, and does not block shower nozzle, easy to use.So far, the anti-plant of free anthraquinones extracted from rheum nano-emulsion preparation is not found
The technology of red spider disease activity is disclosed.
The content of the invention
The purpose of the present invention is, in view of the shortcomings of the prior art there is provided one kind using Chinese medicine rheum officinale as raw material, to pass through
The free anthraquinones extracted from rheum that acidolysis, separation and purifying are obtained (mainly contains rheum emodin, aloe-emodin, Chrysophanol, Physcion
And Rhein) it is bulk drug, research and develop a kind of nano-emulsion preparation for being exclusively used in preventing and treating plant red spider disease.
Technical scheme：A kind of free anthraquinones extracted from rheum nano-emulsion preparation for being used to prevent and treat plant red spider disease, is used
The following raw material is made：In terms of the mass percent of contained each component in nano-emulsion, free anthraquinones extracted from rheum content is 0.05-
0.16%, the oil phase in nano-emulsion accounts for 18~22%, emulsifying agent 16~20%, assistant for emulsifying agent 4~6%, water 50~61%, stably
Agent 1.0%, preservative 0.1%, adhesive agent 0.1%.
The oil phase is selected from isopropyl myristate, Sefsol 218, ethyl oleate, isopropyl palmitate, octanoic acid
Triglyceride DDD, castor oil and combinations thereof.Wherein, further preferred Sefsol 218 and its mixed with ethyl oleate
Compound, oil phase concentration is less than 30%.It is sweet that the emulsifying agent is selected from polyoxyethylene -40- rilanit specials, caprylic capric polyethylene glycol
Grease, Gelucire 44/14, Tween-80, poloxamer-188 and combinations thereof.Wherein, further preferred polyoxy
Ethene -40- rilanit specials；The assistant for emulsifying agent be selected from TC, Macrogol 600, polyethylene glycol 400,
1,2- propane diols, glycerine and combinations thereof.Wherein further preferred TC, the amount of assistant for emulsifying agent is less than
20%；The mass ratio of emulsifying agent and assistant for emulsifying agent is 2：1.The water is solvent, and stabilizer is oleic acid or enuatrol or citron
Sour sodium, preferably oleic acid；Preservative is sodium benzoate and ethylparaben, preferred sodium benzoate；Adhesive agent is disilicon trioxide.
A kind of free anthraquinones extracted from rheum nano-emulsion preparation for being used to prevent and treat plant red spider disease of the present invention, its preparation side
Method is：Free anthraquinones extracted from rheum is dissolved in oil phase, stabilizer is added, emulsifying agent/assistant for emulsifying agent mixture stirs.By
It is added dropwise after water, stirring, the nano-emulsion preparation of self-emulsifying formation clear, ultrasonically treated 15-30min, is adjusted with 1mol/LNaOH
PH is to 6.0-7.0 for section system, then is proportionally added into preservative and adhesive agent.Before emulsifying agent use need in 35-40 DEG C of heating and melting,
Magnetic stirring speed 200-300rpm.Gained nano-emulsion preparation is directly filtered when dispensing with the water system miillpore filter in 0.22 μm of aperture
Into sterilized brown plastic containers.
The present invention nanoemulsion particle diameter between 20-100nm, ζ-potential between -20~-50mV, viscosity between 8-12cP,
PH is between 6.0-7.0.
The free anthraquinones extracted from rheum nano-emulsion of the present invention has the purposes of preventing and treating plant red spider disease, and excellent effect.
The beneficial effects of the invention are as follows：
One is the raw materials used medicine of product of the present invention is Chinese medicine free anthraquinones extracted from rheum extract, nothing in the range of dosage
Poison has no drug resistance, safe, financial cost is relatively low；
The second is product of the present invention can be rendered as the homogeneous system of transparent and stable with the water mixing of arbitrary proportion, prepare
Technique is simple, it is easy to produce in enormous quantities, and emulsion droplet size is small, and viscosity is small, and field sprinkling does not block sprayer, easy to use；
The third is product of the present invention has significant preventing and treating to the red spider disease of the crops such as cucumber, eggplant, corn and flowers
Effect, its effect is equivalent or net better than flowers pink bollworm.
Brief description of the drawings
Fig. 1 is the free anthraquinones extracted from rheum nano-emulsion transmission electron microscope photo (× 15000) of the embodiment of the present invention 2
Fig. 2 is the sick photo of preventing and treating plant red spider of embodiment 4.
Embodiment
The present invention will be further described with reference to embodiments, but not limited to this.Wherein emulsifier polyoxyethylene -40-
Rilanit special is on sale in BASF Chemical Co., Ltd.；The poly- second of Sefsol 218, TC, laurate
Glycol glyceride, Labraso are on sale in French Gattefosse companies；PLURONICS F87 is in Switzerland
Adamas companies are on sale.Other each raw material components can market buy.
Embodiment 1：The extraction of free anthraquinones extracted from rheum
Experiment condition
Rheum officinale is purchased from Li County Xin Sheng sources biotechnology development corporation, Ltd., takes the Rhubarb pulverized and sieved, adds 20%
Sulfuric acid heats acidolysis, and the dregs of a decoction are washed to after neutrality and dried.Rheum officinale hydrolysis dry powder presses bulk drug：90% ethanol=1：30 (w/v) are mixed
Close, ultrasonic extraction, while hot suction filtration, filtrate decompression is concentrated into no alcohol taste, extracted with chloroform, and chloroform extract is extracted with 5%NaOH again
, merging alkali extract colourless to upper liquid is taken, adjusts pH about to 2, centrifuging and taking is precipitated, and is washed to neutrality, produces free anthraquinones extracted from rheum
Crude product.After crude product is dried, by bulk drug：Methanol=1：10 add methanol ultrasonic dissolution, and the decompression of centrifuging and taking supernatant is spin-dried for, obtained greatly
Yellow dissociated anthraquinone (wherein five kinds dissociated anthraquinones account for more than the 98% of gross mass).
Embodiment 2：The prescription of free anthraquinones extracted from rheum nano-emulsion and preparation
Prescription one：
Free anthraquinones extracted from rheum 0.130g, oil phase 19.5g, emulsifying agent 16.5g, assistant for emulsifying agent 4.5g, stabilizer 1.0g, anti-corrosion
Agent 0.1g, adhesive agent 0.1g, purified water 58.4g, gross weight about 100.0g.
Prescription two：
Free anthraquinones extracted from rheum 0.098g, oil phase 18.4g, emulsifying agent 16.0g, assistant for emulsifying agent 4.0g, stabilizer 1.0g, anti-corrosion
Agent 0.1g, adhesive agent 0.1g, purified water 60.5g, gross weight about 100.0g.
In prescription：Free anthraquinones extracted from rheum is main ingredient, and oil phase is Sefsol 218 (prescription two) or itself and ethyl oleate
Mixture (prescription one), emulsifying agent be polyoxyethylene -40- rilanit specials, assistant for emulsifying agent is TC, surely
Agent is determined for oleic acid, and preservative is sodium benzoate, and adhesive agent is disilicon trioxide.
Preparation method is：
Free anthraquinones extracted from rheum and stabilizer are dissolved in oil phase, the mixture of emulsifying agent/assistant for emulsifying agent is added, stirring is equal
It is even.Add water, at the uniform velocity stir dropwise, the nano-emulsion of self-emulsifying formation clear, and regulating system pH 6.0-7.0, add anti-
Rotten agent and adhesive agent.Emulsifying agent is solid at room temperature, therefore using preceding needing 35-40 DEG C of heating and melting.Gained nano-emulsion preparation
During packing, directly filtered with the water system miillpore filter in 0.22 μm of aperture into sterilized brown plastic containers.
Embodiment 3：Type, property, assay and the stability of free anthraquinones extracted from rheum nano-emulsion
Experimental condition：The nano-emulsion obtained to the prescription one of embodiment 2, is tested as follows：
Nano-emulsion type identification：Nano-emulsion type is differentiated using decoration method, oil-soluble dyes tonyred and water solubility is utilized
The speed that dyestuff methylene blue spreads in nano-emulsion judges the type of nano-emulsion.
Nano-emulsion property：Mode of appearance, light transmittance, pH value, viscosity, particle diameter and Zeta potential.
Assay：Free anthraquinones extracted from rheum nano-emulsion 1ml is taken, 10ml methanol, ultrasonic emulsion breaking, 0.45 μm of micropore filter is added
Membrane filtration, high performance liquid chromatography instrument (HPLC) analysis, calculates total free anthraquinone content in free anthraquinones extracted from rheum nano-emulsion.
Study on the stability：(1) influence factor is tested：Nano-emulsion is distinguished under strong light, high temperature and hot conditions, in the 5th day,
Sample within 10th day, whether the property of observation free anthraquinones extracted from rheum nano-emulsion changes.(2) centrifugal acceleration test：By nano-emulsion
After 12000rpm centrifugations 30min, see whether to be layered or precipitated.(2) normal temperature keeps sample experiment：By free anthraquinones extracted from rheum nano-emulsion
Place 90 days at normal temperatures, sampled respectively at the 30th day, 60 days, 90 days, investigate nano-emulsion property and medicament contg.Experiment knot
Really：
Free anthraquinones extracted from rheum nano-emulsion type is O/W types, and observation emulsion droplet is rounded under transmission electron microscope, and light transmittance is
99.0-99.9%, pH are 6.4-6.7, and viscosity is 10.0-11.5cP, particle diameter between 20-100nm, ζ-potential is -25.0~-
35.0mV。
The anthraquinone content that dissociates in free anthraquinones extracted from rheum nano-emulsion is 0.122% (w/w).The rheum officinale trip that nano-emulsion preparation is determined
From each component proportion in the ratio and extract between anthraquinone each component substantially close to its error arises primarily at difference
The same treatment of batch rheum officinale, and this is acceptable for traditional Chinese medicine extract.
Stability test shows that free anthraquinones extracted from rheum nano-emulsion is placed under these conditions, form still clear, does not send out
The phenomenons such as layer estranged, flocculation.In centrifugal acceleration test, after nano-emulsion 12000rpm centrifugations 30min, still clear is homogeneous.Often
The temperature experiment that keeps sample shows that nano-emulsion room temperature is placed 90 days, and physical stability is good, the content of rhubarb free general anthraquinone and each monomer
It is held essentially constant.
The anti-plant red spider disease experiment of the free anthraquinones extracted from rheum nano-emulsion of embodiment 4
Major target disease：Eggplant red spider disease
Test field：* * vegetable fields
Experiment packet：Blank control group is without any reagent (being respectively labeled as E) in following table；Three dilutions of drug component
Group：Respectively 100 times, 250 times and 500 times dilutions (A, B, C are respectively labeled as in following table) of free anthraquinones extracted from rheum nano-emulsion；Sun
Property control group be the net 800 times of dilutions (D is respectively labeled as in following table) per 10g of flowers pink bollworm.
Testing program：Eggplant (cool eggplant No. 2, Wuwei Institute of agricultural sciences seed selection), the red spider onste phase, is often handled
3 repetitions, often repeat spray 5m2, often repeat to select 2 plants of eggplants at random before spraying, red spider selected in every plant of different parts before spray
2 intact leafs of moderate quatity occur for spider, hang label and look into several movable mite numbers.The 2nd after spray, 5 days investigative action mite numbers, meter
Calculate Revision insect recluced rate and prevention effect.Compared with blank control group, calculate Revision insect recluced rate and prevention effect.
Borer population living before Revision insect recluced rate rate %=[borer population living after borer population-dispenser living before dispenser] × 100/ dispenser
Prevention effect %=[treatment region decline rate-check plot decline rate] × 100/ [100- check plots Revision insect recluced rate]
Result of the test (table 1)：
Controlling experiment of the different agents of table 1 to eggplant red spider disease
As can be seen from the test results, in medicament used of participating in the experiment 100 times of dilutions of free anthraquinones extracted from rheum nano-emulsion to red
Spider prevention effect is best, and efficacy time is long, and the controling power to red spider is strong, is a kind of preferable medicine for preventing and treating red spider
Agent；The prevention effect that 250 times of free anthraquinones extracted from rheum nano-emulsion and the net 800 times of dilutions of pink bollworm handle 2 to 5 quite, exists
More than 85%, it can promote the use of in production.
Found in preventive effect fact-finding process, although 100 times of dilutions of free anthraquinones extracted from rheum nano-emulsion are to eggplant red spider disease
Prevention effect is fabulous, but it accelerates the withered of eggplant leaf, shows certain poisoning.And free anthraquinones extracted from rheum nano-emulsion 250
There is not obvious poisoning in times dilution, can use safely.Optimum control period about 5 days, optionally row sprays again afterwards.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
Without departing from the invention herein, some simple deduction or replace can also be made, the protection of the present invention should be all considered as belonging to
Scope.
Claims (4)
1. a kind of free anthraquinones extracted from rheum composition has the purposes of preventing and treating plant red spider disease, it is characterised in that the rheum officinale trip
From the extract that anthraquinone composition is derived from Chinese medicine sorrel, Rheum tanguticum Maxim or Rheum officinale.
2. a kind of free anthraquinones extracted from rheum nano-emulsion preparation has the purposes of preventing and treating plant red spider disease, it is characterised in that described big
Yellow dissociated anthraquinone nano-emulsion preparation is made up of each raw material of following mass percent：Free anthraquinones extracted from rheum 0.05~0.16%, third
Glycol list caprylate 13~16%, ethyl oleate 4~6%, polyoxyethylene -40- rilanit specials 16~20%, diethylene glycol list
Ethylether 4~6%, oleic acid 1.0%, sodium benzoate 0.1%, disilicon trioxide 0.1%, purified water 50~61%.
3. purposes as claimed in claim 2, it is characterised in that the free anthraquinones extracted from rheum nano-emulsion preparation is made as follows
It is standby：Free anthraquinones extracted from rheum and stabilizer are dissolved in Sefsol 218 and ethyl oleate, polyoxyethylene -40- hydrogen is added
Change castor oil, TC, stir, add water dropwise, lasting stirring, until the liquid of clear is formed,
NaOH regulating system pH 6.0-7.0 are used after ultrasonically treated 15-30min, sodium benzoate and disilicon trioxide is added.
4. purposes as claimed in claim 3, it is characterised in that the polyoxyethylene -40- rilanit specials are using preceding needing 35-
40 DEG C of heating and meltings, magnetic stirring speed 200-300rpm.
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| CN101347516A (en) * | 2008-08-01 | 2009-01-21 | 石任兵 | Method for preparing total free anthraquinones extract from rhubarb |
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| CN104586961A (en) * | 2014-12-29 | 2015-05-06 | 南通市第三人民医院 | Method for extracting total anthraquinones in rhubarb |
| CN104642312A (en) * | 2015-02-13 | 2015-05-27 | 兰州大学 | Rheum officinale free anthraquinone composition for preventing plant powdery mildew and nano emulsion preparation |
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| US4602004A (en) * | 1984-06-14 | 1986-07-22 | Maurice Cohen | Aloin and aloe-emodin containing pesticides |
| CN1345597A (en) * | 2000-09-26 | 2002-04-24 | 上海市中药研究所 | Extract of free anthraquinone extracted from rhubarb and preparation process thereof |
| CN101347516A (en) * | 2008-08-01 | 2009-01-21 | 石任兵 | Method for preparing total free anthraquinones extract from rhubarb |
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