CN102657243A - Plant alkaloid compound microemulsion and preparation method of plant alkaloid compound microemulsion - Google Patents
Plant alkaloid compound microemulsion and preparation method of plant alkaloid compound microemulsion Download PDFInfo
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- CN102657243A CN102657243A CN2012101366868A CN201210136686A CN102657243A CN 102657243 A CN102657243 A CN 102657243A CN 2012101366868 A CN2012101366868 A CN 2012101366868A CN 201210136686 A CN201210136686 A CN 201210136686A CN 102657243 A CN102657243 A CN 102657243A
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Abstract
The invention relates to plant alkaloid compound microemulsion and a preparation method of the plant alkaloid compound microemulsion. The plant alkaloid compound microemulsion is characterized by consisting of the following ingredients in percentage by volume: 8 percent to 12 percent of alkaloid, 12 percent to 18 percent of emulsifying agents, 18 percent to 22 percent of cosolvents and the balance solvents, wherein the alkaloid is total alkaloid prepared from 1.5 to 2.5 weight parts of brunnera and 0.5 to 1.5 weight parts of sophora alopecuroide through ethanol and chloroform extraction, the emulsifying agents are tween-80, the cosolvents are glycol, and the solvents are ethanol with the volume percentage being 75 to 95 percent. The plant alkaloid compound microemulsion disclosed by the invention is compounded by the brunnera and the sophora alopecuroide, the synergia effect among active ingredients is utilized, the medicine effect and the integral prevention and treatment effect of products are improved, the duration is long, low toxicity and environment protection are realized, and the resistance cannot be easily generated in the use process.
Description
Technical field
The present invention relates to a kind of plant alkaloid complex microemulsion and preparation method thereof.
Background technology
Chemical pesticide is so that its quick-acting is fast, effectively kill pests is still the present main force in domestic and international agricultural chemicals market; But problems such as its " 3R " that causes, " three cause "; Severe contamination environment and agricultural product; Human beings'health is caused great harm, be unfavorable for the sustainable development of green agriculture, more be unfavorable for the outlet of agricultural product.Therefore, use the pollution-free plant source pesticide instead of chemical agricultural chemicals of high-efficiency low-toxicity must become the emphasis that novel agrochemical develops.
In recent years, though China's Development and Production goes out some botanical pesticides preferably, because technology, laboratory facilities are limited, make progress slower.These action of agricultural chemicals are slow in the effect of diseases and pests of agronomic crop, and quick-acting is not strong, limited it and promoted the use of.Some take botanical pesticide and the composite method of chemical pesticide are improved the control efficiency of botanical pesticide, have obtained certain effect, have improved the quick-acting of botanical pesticide to a certain extent.But still contain a certain amount of chemical pesticide in these Recompounded pesticides, nuisanceless, the advantage of aspect such as free from environmental pollution has not existed as botanical pesticide for it.Therefore, how reasonably choosing plant and carry out scientific and reasonable proportioning, obtain the obvious results prescription, to improve the control efficiency of damage by disease and insect, is the problem that development plant resource Recompounded pesticide presses for solution.
Summary of the invention
It is efficient, the safety of raw material, the plant alkaloid complex microemulsion of low-residual with the plant that one of the object of the invention provides a kind of;
Two of the object of the invention provides a kind of preparation method of above-mentioned plant alkaloid complex microemulsion.
A kind of plant alkaloid complex microemulsion, its special feature are that by volume the percentage meter is formed as follows: alkaloid 8%-12%, and emulsifier 12%-18%, cosolvent 18%-22%, solvent 28%-32% surplus is a water; The alkaloid biology total alkali that 1.5-2.5 weight portion OX-heart Piao Zi and 0.5-1.5 weight portion Sophora alopecuroide in proportion obtain after through ethanol, chloroform extraction of serving as reasons wherein, emulsifier is a Tween-80, and cosolvent is an ethylene glycol, and solvent is the ethanol of volume fraction 75-95%.
Wherein alkaloid extraction technology is following: OX-heart Piao Zi and Sophora alopecuroide are dried in the shade, are ground into 20-40 purpose particle, and be 1.5-2.5 by OX-heart Piao Zi and Sophora alopecuroide mass ratio: 0.5-1.5 mixes, and adds the ethanol of the volume fraction 95% that is equivalent to 8 times of quality of above-mentioned particle again; Normal temperature soaked 24 hours down, ultrasonic Extraction then, and extracting temperature is 35-45 ℃; Extraction time is 35-45 minute, and filtering and collecting filter liquid repeats aforesaid operations lixiviate 3 times at least; Merging filtrate; Concentrating under reduced pressure, solvent evaporated gets ethanol extract; To the hydrochloric acid that wherein adds volume fraction 2% extract is transferred to the pH value and be 5-6; Use ethyl acetate extraction; Remove ethyl acetate layer, remainder is regulated pH to 9～10 with concentrated ammonia liquor, extracts till checking inanimate object alkali with the alkaloid precipitating reagent with chloroform then; Combining extraction liquid, concentrating under reduced pressure promptly get alkaloid.
Wherein the alkaloid precipitating reagent is a bismuth potassium iodide.
A kind of preparation method of plant alkaloid complex microemulsion, its special feature is, comprises the steps:
(1) OX-heart Piao Zi and Sophora alopecuroide are dried in the shade, are ground into 20-40 purpose particle, be 1.5-2.5 by OX-heart Piao Zi and Sophora alopecuroide mass ratio: 0.5-1.5 mixes, and adds the ethanol of the volume fraction 95% that is equivalent to 8 times of quality of above-mentioned particle again, and normal temperature soaked 24 hours down; Ultrasonic Extraction then, extracting temperature is 35-45 ℃, extraction time is 35-45 minute; Filtering and collecting filter liquid repeats aforesaid operations lixiviate 3 times at least, merging filtrate; Concentrating under reduced pressure, solvent evaporated gets ethanol extract; To the hydrochloric acid that wherein adds volume fraction 2% extract is transferred to the pH value and be 5-6; Use ethyl acetate extraction; Remove ethyl acetate layer, remainder is regulated pH to 9～10 with concentrated ammonia liquor, extracts till checking inanimate object alkali with the alkaloid precipitating reagent with chloroform then; It is for use that combining extraction liquid, concentrating under reduced pressure promptly get alkaloid;
(2) according to the proportioning of claim 1, alkaloid and solvent, cosolvent, emulsifier and water that step 1 is obtained are mixed with solution in proportion, are the plant alkaloid complex microemulsion.
Botanical pesticide because of its raw material sources in natural plants, to the person poultry safety, sick worm is difficult for developing immunity to drugs and is paid much attention to, and is the safety-type agricultural chemicals of one type of low toxicity and low residue.And OX-heart Piao Zi, Sophora alopecuroide is distinguished at me and is distributed extensively, and effectively prevention and elimination of disease and pests, has the potentiality that exploitation becomes botanical pesticide.A kind of plant alkaloid complex microemulsion disclosed by the invention is through to OX-heart Piao Zi, and Sophora alopecuroide carries out composite, relies on the synergistic effect between the active ingredient; The drug effect and the integrated control effect of product have been improved; Lasting period is long, and low toxicity, environmental protection are difficult for producing resistance in the use.
Embodiment
Embodiment 1:
1, active ingredient alkaloid extraction: take by weighing the OX-heart Piao Zi of 600g and the Sophora alopecuroide dry powder of 300g and (attach test plant brief introduction: OX-heart Piao Zi (Cynanchum komarovii); Asclepiadaceae (Asclepiadaceae) Cynanchum (Cynanchum) plant; Gather the acrial part herb in the florescence before the test, it is domestic to pick up from the Ningxia Yanchi County, and pulverize the indoor back of drying in the shade; Cross 40 mesh sieves, get plant drymeal; Sophora alopecuroide (Sophora alopecuroidesL.), pulse family (Leguminosae) sophora plant is gathered the above and below ground herb in the fruit phase before the test, and it is domestic to pick up from the Ningxia Yanchi County; Pulverize the indoor back of drying in the shade, and crosses 40 mesh sieves, plant drymeal) add the ethanol of the volume fraction 95% of 720ml, normal temperature soaked 24 hours down; Ultrasonic Extraction then, extracting temperature is 35-45 ℃, extraction time is 35-45 minute; Filtering and collecting filter liquid repeats aforesaid operations lixiviate 3 times, merges filtrating 3 times; Concentrating under reduced pressure, solvent evaporated gets ethanol extract;
To the hydrochloric acid that wherein adds volume fraction 2% extract is transferred to the pH value and be 5-6; Use ethyl acetate extraction, remove ethyl acetate layer, remainder use mass concentration is 30% concentrated ammonia liquor adjusting pH to 9～10; Extract till checking inanimate object alkali with chloroform then with alkaloid precipitating reagent (bismuth potassium iodide); Combining extraction liquid, concentrating under reduced pressure gets alkaloid, and is subsequent use;
2, the preparation of plant pesticide microemulsion: take by weighing alkaloid 10g; After the ethanol of the volume fraction 95% of adding 30mL, the dissolving of 20mL cosolvent ethylene glycol; Add again after the 15mL Tween-80 stirs, add water and be settled to 100mL, obtain plant alkaloid complex microemulsion product 100mL.Get former medicine during test as required in right amount in miniaturised nebuliser, directly add clear water and stir, promptly get required corresponding diluted concentration.
3, carry out field efficacy with above-mentioned embodiment gained plant alkaloid complex microemulsion, test as follows:
The go down computational methods of rate and corrected mortality of insect population are:
(1) field experiment and the result of control matrimony vine aphid:
With 2.5% gamma cyhalothrin, 40% phoxim is the contrast medicament, the dilution respective concentration, and other establishes the spray clear water is blank.Selected experiment field, the matrimony vine tree grows fine.Matrimony vine spacing in the rows 2m, line-spacing 2m, the age of tree 5 years; Tree vigo(u)r is medium, and matrimony vine aphid insect population radix is higher, worm amount distribution uniform; In matrimony vine aphid damage district, be reagent in 10% (10% with the alkaloid volume fraction, and the other used mg/l of unit of 10% microemulsion is biological alkali mass concentration in the following table) complex microemulsion dilution respective concentration; With the clear water is contrast (CK), uses the small hand-held sprayer, the complete stool even spraying.10 branches are randomly drawed in each processing, the mark of fixedly listing, and whole aphid quantity of investigation 20cm place, branch top every branches and leaves sheet positive and negative, investigation insect population radix before the dispenser is behind the medicine the 3rd, 5,7,10,15d investigates remaining insect population quantity respectively.Calculate insect population go down rate and control efficiency.
Table 1 microemulsion is to the field efficacy of matrimony vine aphid
(2) field trial and the result of control diamond-back moth.
With above-mentioned gained complex microemulsion dilution respective concentration is reagent, serves as the contrast medicament with 2.5% gamma cyhalothrin, 40% phoxim, the dilution respective concentration, and other establishes the spray clear water is blank, other field trials with the matrimony vine aphid are identical.
Table 2 microemulsion is to the field efficacy of diamond-back moth
Can know that by table 1, table 2 quick-acting of chemical pesticide is strong, but lasting effect is far away from the Recompounded pesticide microemulsion.Chemical pesticide the 3rd day preventive effect after dispenser reaches the highest, and drug effect continues to descend afterwards; Complex microemulsion of the present invention is best in the performance of 7d drug effect, and is long than traditional chemical agricultural chemicals lasting effect, and diamond-back moth and matrimony vine aphid are all had desirable control efficiency; Be difficult for developing immunity to drugs; Reduce spraying times, reduced residually, embodied the advantage of complex microemulsion.
Claims (4)
1. a plant alkaloid complex microemulsion is characterized in that, by volume the percentage meter is formed as follows: alkaloid 8%-12%, and emulsifier 12%-18%, cosolvent 18%-22%, solvent 28%-32% surplus is a water; The alkaloid biology total alkali that 1.5-2.5 weight portion OX-heart Piao Zi and 0.5-1.5 weight portion Sophora alopecuroide in proportion obtain after through ethanol, chloroform extraction of serving as reasons wherein, emulsifier is a Tween-80, and cosolvent is an ethylene glycol, and solvent is the ethanol of volume fraction 75-95%.
2. a kind of plant alkaloid complex microemulsion as claimed in claim 1, it is characterized in that: wherein alkaloid extraction technology is following: OX-heart Piao Zi and Sophora alopecuroide are dried in the shade, are ground into 20-40 purpose particle, and be 1.5-2.5 by OX-heart Piao Zi and Sophora alopecuroide mass ratio: 0.5-1.5 mixes; The ethanol that adds the volume fraction 95% that is equivalent to 8 times of quality of above-mentioned particle again, normal temperature soaked 24 hours down, then ultrasonic Extraction; Extracting temperature is 35-45 ℃, and extraction time is 35-45 minute, filtering and collecting filter liquid; Repeat aforesaid operations lixiviate 3 times at least, merging filtrate, concentrating under reduced pressure; Solvent evaporated gets ethanol extract; To the hydrochloric acid that wherein adds volume fraction 2% extract is transferred to the pH value and be 5-6; Use ethyl acetate extraction; Remove ethyl acetate layer, remainder is regulated pH to 9～10 with concentrated ammonia liquor, extracts till checking inanimate object alkali with the alkaloid precipitating reagent with chloroform then; Combining extraction liquid, concentrating under reduced pressure promptly get alkaloid.
3. a kind of plant alkaloid complex microemulsion as claimed in claim 1 is characterized in that: wherein the alkaloid precipitating reagent is a bismuth potassium iodide.
4. the preparation method of a plant alkaloid complex microemulsion is characterized in that, comprises the steps:
(1) OX-heart Piao Zi and Sophora alopecuroide are dried in the shade, are ground into 20-40 purpose particle, be 1.5-2.5 by OX-heart Piao Zi and Sophora alopecuroide mass ratio: 0.5-1.5 mixes, and adds the ethanol of the volume fraction 95% that is equivalent to 8 times of quality of above-mentioned particle again, and normal temperature soaked 24 hours down; Ultrasonic Extraction then, extracting temperature is 35-45 ℃, extraction time is 35-45 minute; Filtering and collecting filter liquid repeats aforesaid operations lixiviate 3 times at least, merging filtrate; Concentrating under reduced pressure, solvent evaporated gets ethanol extract; To the hydrochloric acid that wherein adds volume fraction 2% extract is transferred to the pH value and be 5-6; Use ethyl acetate extraction; Remove ethyl acetate layer, remainder is regulated pH to 9～10 with concentrated ammonia liquor, extracts till checking inanimate object alkali with the alkaloid precipitating reagent with chloroform then; It is for use that combining extraction liquid, concentrating under reduced pressure promptly get alkaloid;
(2) according to the proportioning of claim 1, alkaloid and solvent, cosolvent, emulsifier and water that step 1 is obtained are mixed with solution in proportion, are the plant alkaloid complex microemulsion.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104068076A (en) * | 2014-06-27 | 2014-10-01 | 何芳 | Preparation method for particle pesticide |
| CN105284914A (en) * | 2015-12-04 | 2016-02-03 | 成都新朝阳作物科学有限公司 | Pesticide composition containing cynanchum komarovii and sophora alopecuroide extract as well as preparation method and application thereof |
| CN107114416A (en) * | 2017-06-07 | 2017-09-01 | 江苏徐淮地区淮阴农业科学研究所 | Prevent and treat the botanical fungicide of rice blast |
| CN107173398A (en) * | 2017-06-07 | 2017-09-19 | 江苏徐淮地区淮阴农业科学研究所 | Prevent and treat the botanical fungicide of wheat scab |
| CN108651448A (en) * | 2018-05-11 | 2018-10-16 | 广西师范大学 | A kind of formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104068076A (en) * | 2014-06-27 | 2014-10-01 | 何芳 | Preparation method for particle pesticide |
| CN105284914A (en) * | 2015-12-04 | 2016-02-03 | 成都新朝阳作物科学有限公司 | Pesticide composition containing cynanchum komarovii and sophora alopecuroide extract as well as preparation method and application thereof |
| CN107114416A (en) * | 2017-06-07 | 2017-09-01 | 江苏徐淮地区淮阴农业科学研究所 | Prevent and treat the botanical fungicide of rice blast |
| CN107173398A (en) * | 2017-06-07 | 2017-09-19 | 江苏徐淮地区淮阴农业科学研究所 | Prevent and treat the botanical fungicide of wheat scab |
| CN108651448A (en) * | 2018-05-11 | 2018-10-16 | 广西师范大学 | A kind of formula and preparation method thereof of Schima superba bark saponin pest killing micro emulsion |
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