CN103843838A - Plant source bactericidal synergist, extraction process and application thereof to agricultural bactericide - Google Patents
Plant source bactericidal synergist, extraction process and application thereof to agricultural bactericide Download PDFInfo
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- CN103843838A CN103843838A CN201210514141.6A CN201210514141A CN103843838A CN 103843838 A CN103843838 A CN 103843838A CN 201210514141 A CN201210514141 A CN 201210514141A CN 103843838 A CN103843838 A CN 103843838A
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- synergistic agent
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Abstract
The invention discloses a plant source bactericidal synergist, an extraction process of the plant source bactericidal synergist and application of the plant source bactericidal synergist to the agricultural sterilizing agent. The plant source bactericidal synergist is pericarp extract of citrus fruits, three-time extraction process is adopted, and the ultrasonic-assisted extraction is performed, the maximum extraction quantity of active ingredients is ensured, the process is simple and has little environmental influence, the plant source bactericidal synergist can be used as the synergist to be matched with the traditional chemical bactericide, the bactericidal effect is remarkably improved, the plant source bactericidal synergist can be added into liquid preparations and solid preparations and can be specifically used in the preparations such as microemulsions, suspending agents, wettable powder, and water dispersible granules.
Description
Technical field
The present invention relates to agricultural bacteriocide preparation technique field, particularly relate to a kind of plant resource sterilizing synergistic agent, its extraction process and this extract as synergist in the application aspect agricultural bacteriocide preparation technique.
Background technology
Oranges and tangerines, it is tangerine, mandarin orange, orange, gold mandarin orange, shaddock, the general name of trifoliate orange etc., in existing more than the 4000 year history of China's citriculture, many strains are formed, citrusfruit color, smell and taste are held concurrently excellent, fruit juice is abundant, local flavor grace, except containing multiple sugar, organic acid, outside mineral matter, also be rich in vitamin C, multiple glucoside material, nutritive value is high, therefore be often used as traditional Chinese medicine and health food is used, report the useful gas of oranges and tangerines, keep fit, aid digestion, strengthening the spleen and stomach, effect such as hypotensive grade, to preventing and treating suppurative sphagitis, tonsillitis, diabetes, virus flu has certain effect.
On market, there is at present the extract product of oranges and tangerines, but be various health medicines, equally, though have data to record for the extraction process of orange peel, as mentioned microwave method and extract the technical study of pectin from orange peel, take orange peel as raw material, under microwave condition, regulate the pH value of extract with nitration mixture, adopt the technique extraction pectin of absolute ethyl alcohol precipitation, but the extract of orange peel as the sterilizing synergistic agent in agricultural with and extraction process and the application in agricultural chemicals be not reported.
Agricultural disease prevent and treat process in be mainly adopt chemical bactericide process, although sterilization speed is fast, successful, but along with the long-term a large amount of irrational uses of various medicaments, germ has produced serious pesticide resistance, and drug effect reduces gradually, also day by day serious to the harm of environment, therefore good botanical fungicide becomes current main flow direction, to seek Environmental compatibility.
Summary of the invention
Object of the present invention is exactly to provide a kind of its extraction process of plant resource sterilizing synergistic agent and the application in agricultural bacteriocide thereof for the defect of above-mentioned existence, improve original preparation technique, for the control of agricultural disease, with the compatibility of environment, to person poultry harmless, alleviate the pollution to environment, little to natural biotic influence, environmental protection, can extensive use in agricultural bacteriocide, in liquid preparation and solid pharmaceutical preparation, all can add, be suitable for long-term use.
The pericarp extract that plant resource sterilizing synergistic agent of the present invention is citrus fruit, carries out the extraction of bactericidal active component take the pericarp of citrus fruit as vegetable material, and this citrus fruit is tangerine, mandarin orange, orange, golden mandarin orange, the general name of shaddock, trifoliate orange etc.
In the pericarp of citrus fruit, contain a variety of bioactive ingredients, wherein mainly contain: flavonoids, polyphenol, adjacent pyrrole are fed ketone, monoterpene, triterpene, coumarin, carotenoid, class propyl alcohol, acridone, glycerose lipid, P-zeaxanthin and nobiletin etc., in these materials, much there is bactericidal activity, picture flavonoids, coumarin, terpene etc., also there are some to there is antivirus action, as P-zeaxanthin, nobiletin, limonin etc.
The extraction process of plant resource sterilizing synergistic agent of the present invention, comprises the following steps:
1. by the pericarp cleaning, drying of citrus fruit, pulverize as 50-100 object particle;
2. the pericarp particle crushing is dropped in reactor, add the mixed extract that consists of second alcohol and water, wherein the percentage by weight of ethanol is 70%-90%, stirring and refluxing 3-4h at 50-80 ℃, add in thermal reflow process and apply ultrasonic, once ultrasonic at interval of 30-40min, each ultrasonic concussion 10-15min, reflux and finish to filter, retain filtrate;
3. residue is added to mixed extract again, 2. repeating step extracts once again, filters, and retains filtrate;
4. step, the mixed extract in is 2. changed to water step residue is 3. extracted again, filters, and retains filtrate;
5. merge all filtrate, concentrate, obtain sterilizing synergistic agent of the present invention, can make grain products, medicinal extract product or fluid product;
6. ethanol is reclaimed.
In technique, the drying mode of described pericarp is natural seasoning; The ethanol of described step in is 6. recycled in step mixed extract 2.; Described ethanol is more than 95% general industry ethanol, and water is ordinary tap water.
Extracts from Plant Recourses of the present invention, can be as sterilizing synergistic agent application in agricultural bacteriocide, and as the synergist of traditional chemical bactericide, the addition of this synergist is the 5-50% of gross weight by weight.
As formulation, can be applied to according to the actual needs microemulsion, suspending agent, wetting powder or dosage form of water dispersible granule.
Preparation method for liquid preparation is: using former liquid medicine or add the former medicine of solid after dissolution with solvents and emulsifier, cosolvent, antifreeze, stabilizing agent etc. mix as oil phase under 1000r/min stirs according to the required and of the present invention extract of formula, thickener, PH conditioning agent are added to the water and are mixed as water, under 1000 ~ 2000r/min stirs, water is slowly added in oil phase, continue to stir 30min, make product.
Preparation method for solid pharmaceutical preparation is: extract decompression rotary evaporation of the present invention is concentrated, at vacuum-0.06 ~ 50 ~ 60 ℃ of-0.08MPa temperature, drying under reduced pressure is to powdery solid, with the former medicine of solid, wetting agent, dispersant, carrier etc. according to formula required mixing, reach fineness, wetting dispersion etc. through air-flow crushing and require, also can be through fluidized granulating as water dispersible granules.
Described emulsifier, wetting agent, dispersant, cosolvent, antifreeze, stabilizing agent, thickener, PH conditioning agent etc. are all selected from the conventional kind in agricultural bacteriocide preparation technique field.
Beneficial effect of the present invention is: plant resource sterilizing synergistic agent of the present invention, from the pericarp of natural plants-citrus fruit, is a kind of constituted mode itself existing in the Nature, therefore environmentally friendly, to non-target organism safety.Extraction process of the present invention is simplified also easily operation, extract and 1 st pure water extraction through twice ethanol water, most of Fungicidal active substance can be extracted completely, and adopt ultrasonic assisted extraction, guarantee the complete and efficiency of extracting, greatly shortened extraction time, utilized ultrasonic cavitation effect to destroy cell wall, recovery rate is high, and utilization rate of raw materials is large.Holistic cost is cheap, and extract is cheap and easy to get, uses safety, and recoverable, environmentally safe.This extract has bactericidal activity, use as sterilizing synergistic agent, it is applied in agricultural, especially be applied to sterilization pesticide field, the well pesticide resistance problem of opposing germ, can strengthen drug effect, with the compatibility of environment, to person poultry harmless, alleviate the pollution to environment, little to natural biotic influence, environmental protection, can extensive use in agricultural bacteriocide, in liquid preparation and solid pharmaceutical preparation, all can add, having good promotion and application prospect, be suitable for long-term use, is also the main flow in the future developing.
Embodiment
In order to understand better the present invention, describe technical scheme of the present invention in detail with instantiation below, but the present invention is not limited thereto.
Extraction process specific embodiment of the present invention is as follows:
1. by the pericarp cleaning, drying of citrus fruit, pulverizing is 50 object particles;
2. the pericarp particle 100g crushing is dropped in reactor, add the 200ml mixed extract that consists of second alcohol and water, wherein the percentage by weight of ethanol is 80%, stirring and refluxing 3h at 50-80 ℃, add in thermal reflow process and apply ultrasonic, once ultrasonic at interval of 30min, each ultrasonic concussion 10min, reflux and finish to filter, retain filtrate;
3. step residue is 2. added to 100ml mixed extract again, 2. repeating step extracts once again, filters, and retains filtrate;
4. step, the mixed extract in is 2. changed to 50ml water step residue is 3. extracted again, filters, and retains filtrate;
5. combining step 2., 3., 4. in all filtrate, heating distillation and concentration, obtain sterilizing synergistic agent concentrate of the present invention.
Step is the middle alcohol determining moisture that reclaims 5., and calculating can be used as extract recycling after adding new ethanol.
For the extraction process of solid particle, its difference is, extraction process step 5. in, merge the rotary evaporation that reduces pressure after all filtrate, then at vacuum-0.06 ~ 50 ~ 60 ℃ of-0.08MPa temperature, drying under reduced pressure further removes mixed extract, can obtain the solid particle of sterilizing synergistic agent of the present invention.
Embodiment 1
Extract of the present invention is the application in 5% micro-emulsion of phenyl ether methyl cyclic-azole as synergist, each component proportion by weight:
Difenoconazole 5%
Phenethyl phenol polyethenoxy polyethenoxy ether 4%
Alkylphenol polyoxyethylene 4%
Alkyl benzene calcium sulfonate 2%
Cyclohexanone 10%
Concentrate 5% of the present invention
Citric acid 0.2%
Water surplus
Its preparation process is as follows: Difenoconazole is dissolved with cyclohexanone, add phenethyl phenol polyethenoxy polyethenoxy ether, alkylphenol polyoxyethylene, alkyl benzene calcium sulfonate, concentrate of the present invention to stir as oil phase, citric acid is added to the water and is stirred as water, under 1000 ~ 2000r/min stirs, water is slowly added to oil phase, continue to stir 30min.
Embodiment 2
Extract of the present invention is the application in 10% Difenoconazole wetting powder as synergist, each component proportion by weight:
Difenoconazole 10%
Solid particle 50% of the present invention
Sodium alkyl sulfate 2%
Calcium lignosulfonate 4%
Pull open powder 4%
White carbon surplus
Its preparation process is as follows: by extract solid particle of the present invention, with Difenoconazole, sodium alkyl sulfate, calcium lignosulfonate, pull open powder, white carbon mixes, after air-flow crushing, mix.
Embodiment 3
Extract of the present invention is the application in 10% difenoconazole water dispersible granule as synergist, each component proportion by weight:
Difenoconazole 10%
Solid particle 15% of the present invention
WDG wetting agent 4%
WDG dispersant 4%
White carbon 5%
Kaolin surplus
Its preparation process is as follows: by extract solid particle of the present invention, mix with Difenoconazole, WDG wetting agent, WDG dispersant, white carbon, kaolin, after air-flow crushing, mix, after detection fineness wetability is qualified, then add polymerization glue to carry out fluidized granulating.
Embodiment 4
Extract of the present invention is the application in 10% dimethomorph suspending agent as synergist, each component proportion by weight:
Dimethomorph 10%
Solid particle 30% of the present invention
SC wetting agent 4%
SC dispersant 4%
White carbon 1%
Xanthans 2%
Water surplus
Its preparation process is as follows: by extract solid particle of the present invention, add part water high speed dispersion 30min under 4000r/min stirs with dimethomorph, SC wetting agent, SC dispersant, white carbon, then proceed to sand mill and add zirconium oxide bead sand milling 2h, the qualified rear filtration zirconium pearl of fineness, retains filtrate.Add dispersed with stirring in remaining water evenly as water, water under agitation slowly to be added in the filtrate after sand milling xanthans, continue to stir 30min, mix.
Claims (10)
1. a plant resource sterilizing synergistic agent, is characterized in that, the pericarp extract that described plant resource sterilizing synergistic agent is citrus fruit.
2. the extraction process of plant resource sterilizing synergistic agent as claimed in claim 1, comprises the following steps:
By the pericarp cleaning, drying of citrus fruit, pulverize as 50-100 object particle;
The pericarp particle crushing is dropped in reactor, add the mixed extract that consists of second alcohol and water, wherein the percentage by weight of ethanol is 70%-90%, stirring and refluxing 3-4h at 50-80 ℃, add in thermal reflow process and apply ultrasonic, once ultrasonic at interval of 30-40min, each ultrasonic concussion 10-15min, reflux and finish to filter, retain filtrate;
Residue is added to mixed extract again, and 2. repeating step extracts once again, filters, and retains filtrate;
Mixed extract step in is 2. changed to water step residue is 3. extracted again, filters, and retains filtrate;
Merge all filtrate, concentrate, obtain sterilizing synergistic agent of the present invention;
Ethanol is reclaimed.
3. the extraction process of plant resource sterilizing synergistic agent according to claim 2, is characterized in that, the drying mode of described pericarp is natural seasoning.
4. the extraction process of plant resource sterilizing synergistic agent according to claim 2, is characterized in that, the ethanol of described step in is 6. recycled in step mixed extract 2..
5. the extraction process of plant resource sterilizing synergistic agent according to claim 2, is characterized in that, described ethanol is more than 95% general industry ethanol, and water is ordinary tap water.
6. the application of plant resource sterilizing synergistic agent according to claim 1 in agricultural bacteriocide.
7. plant resource sterilizing synergistic agent according to claim 6 is as the synergist application of traditional chemical bactericide.
8. according to the plant resource sterilizing synergistic agent described in claim 6 or 7, it is characterized in that, the addition of this synergist is 5-50% by weight.
9. according to the plant resource sterilizing synergistic agent described in claim 6 or 7, it is characterized in that, described sterilizing synergistic agent is applied to microemulsion, suspending agent, wetting powder or dosage form of water dispersible granule.
10. plant resource sterilizing synergistic agent according to claim 8, is characterized in that, described sterilizing synergistic agent is applied to microemulsion, suspending agent, wetting powder or dosage form of water dispersible granule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210514141.6A CN103843838A (en) | 2012-12-05 | 2012-12-05 | Plant source bactericidal synergist, extraction process and application thereof to agricultural bactericide |
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| CN201210514141.6A CN103843838A (en) | 2012-12-05 | 2012-12-05 | Plant source bactericidal synergist, extraction process and application thereof to agricultural bactericide |
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| CN103843838A true CN103843838A (en) | 2014-06-11 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484366A (en) * | 2020-03-31 | 2020-08-04 | 华南农业大学 | Disease-resistant insect-resistant liquid pesticide fertilizer and preparation method thereof |
| TWI753619B (en) * | 2020-10-21 | 2022-01-21 | 亞東學校財團法人亞東科技大學 | A natural disinfectant formulated with edible fungi and plant extracts |
-
2012
- 2012-12-05 CN CN201210514141.6A patent/CN103843838A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484366A (en) * | 2020-03-31 | 2020-08-04 | 华南农业大学 | Disease-resistant insect-resistant liquid pesticide fertilizer and preparation method thereof |
| TWI753619B (en) * | 2020-10-21 | 2022-01-21 | 亞東學校財團法人亞東科技大學 | A natural disinfectant formulated with edible fungi and plant extracts |
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Application publication date: 20140611 |