CN102657243B - 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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- CN102657243B CN102657243B CN2012101366868A CN201210136686A CN102657243B CN 102657243 B CN102657243 B CN 102657243B CN 2012101366868 A CN2012101366868 A CN 2012101366868A CN 201210136686 A CN201210136686 A CN 201210136686A CN 102657243 B CN102657243 B CN 102657243B
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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 of domestic and international pesticide market, but the problems such as its " 3R " that causes, " three cause ", severe contamination environment and agricultural product, health to the mankind has 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, although China's Development and Production goes out some botanical pesticides preferably, limited due to technology, laboratory facilities, 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 to a certain extent the quick-acting of botanical pesticide.But still contain a certain amount of chemical pesticide in these Recompounded pesticides, it is as botanical pesticide nuisanceless, and the advantage of the aspect such as free from environmental pollution has not existed.Therefore, how reasonably choosing plant and carry out scientific and reasonable proportioning, obtain effect and fill a prescription significantly,, to improve the control efficiency of damage by disease and insect, is development plant resource Recompounded pesticide problem in the urgent need to address.
Summary of the invention
One of purpose of the present invention is to provide a kind of efficient, safety, the plant alkaloid complex microemulsion of low-residual take plant as raw material;
Two of purpose of the present invention is to provide a kind of preparation method of above-mentioned plant alkaloid complex microemulsion.
A kind of plant alkaloid complex microemulsion, its special feature be, by volume the percentage meter is composed as follows: alkaloid 8%-12%, and emulsifier 12%-18%, cosolvent 18%-22%, solvent 28%-32% surplus is water; Alkaloid 1.5-2.5 weight portion Cynanchum Komarovii and 0.5-1.5 weight portion Sophora alopecuroide in proportion obtain after ethanol, chloroform recovery the biology total alkali of serving as reasons wherein, emulsifier is Tween-80, and cosolvent is ethylene glycol, and solvent is the ethanol of volume fraction 75-95%.
Wherein alkaloidal extraction process is as follows: Cynanchum Komarovii and Sophora alopecuroide are dried in the shade, are ground into 20-40 purpose particle, be 1.5-2.5 by Cynanchum Komarovii and Sophora alopecuroide mass ratio: 0.5-1.5 mixes, the ethanol that adds again the volume fraction 95% that is equivalent to 8 times of quality of above-mentioned particle, soaked 24 hours under normal temperature, then ultrasonic extraction, the extraction temperature is 35-45 ℃, extraction time is 35-45 minute, filtering and collecting filter liquid, repeat aforesaid operations lixiviate 3 times at least, merging filtrate, reduced pressure concentration, solvent evaporated, obtain ethanol extract; The hydrochloric acid that adds wherein volume fraction 2% transfers to the pH value with extract and is 5-6, use ethyl acetate extraction, remove ethyl acetate layer, remainder is regulated pH to 9～10 with concentrated ammonia liquor, then extract with chloroform until with the alkaloid precipitating reagent, check inanimate object alkali, combining extraction liquid, reduced pressure concentration namely obtain alkaloid.
Wherein the alkaloid precipitating reagent is bismuth potassium iodide.
A kind of preparation method of plant alkaloid complex microemulsion, its special feature is, comprises the steps:
(1) Cynanchum Komarovii and Sophora alopecuroide are dried in the shade, are ground into 20-40 purpose particle, be 1.5-2.5 by Cynanchum Komarovii and Sophora alopecuroide mass ratio: 0.5-1.5 mixes, then adds the ethanol of the volume fraction 95% that is equivalent to 8 times of quality of above-mentioned particle, soaked 24 hours under normal temperature, then ultrasonic extraction, the extraction temperature is 35-45 ℃, extraction time is 35-45 minute, filtering and collecting filter liquid, repeat aforesaid operations lixiviate 3 times at least, merging filtrate, reduced pressure concentration, solvent evaporated, obtain ethanol extract; The hydrochloric acid that adds wherein volume fraction 2% transfers to the pH value with extract and is 5-6, use ethyl acetate extraction, remove ethyl acetate layer, remainder is regulated pH to 9～10 with concentrated ammonia liquor, then extract with chloroform until with the alkaloid precipitating reagent, check inanimate object alkali, it is stand-by that combining extraction liquid, reduced pressure concentration namely obtain 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 is because of its raw material sources in natural plants, and 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 a class low toxicity and low residue.And Cynanchum Komarovii, Sophora alopecuroide is distinguished at me and is distributed extensively, and effectively prevention and elimination of disease and pests, and having exploitation becomes the potentiality of botanical pesticide.A kind of plant alkaloid complex microemulsion disclosed by the invention is by to Cynanchum Komarovii, and Sophora alopecuroide carries out composite, relies on the synergistic effect between active ingredient, 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 use procedure.
Embodiment
Embodiment 1:
1, the alkaloidal extraction of active ingredient: take (the attached test plant brief introduction: Cynanchum Komarovii (Cynanchum komarovii) of the Cynanchum Komarovii of 600g and the Sophora alopecuroide dry powder of 300g, Asclepiadaceae (Asclepiadaceae) Cynanchum (Cynanchum) plant, gather the acrial part herb in the florescence before test, pick up from Yanchi county Ningxia domestic, the indoor rear pulverizing of drying in the shade, cross 40 mesh sieves, obtain plant drymeal; Sophora alopecuroide (Sophora alopecuroidesL.), pulse family (Leguminosae) sophora plant, gather the above and below ground herb in the fruit phase before test, pick up from Yanchi county Ningxia domestic, the indoor rear pulverizing of drying in the shade, cross 40 mesh sieves, obtains plant drymeal) add the ethanol of the volume fraction 95% of 720ml, soaked 24 hours under normal temperature, then ultrasonic extraction, the extraction temperature is 35-45 ℃, extraction time is 35-45 minute, filtering and collecting filter liquid, repeat aforesaid operations lixiviate 3 times, merge 3 times filtrate, reduced pressure concentration, solvent evaporated, obtain ethanol extract;
The hydrochloric acid that adds wherein volume fraction 2% transfers to the pH value with extract and is 5-6, use ethyl acetate extraction, remove ethyl acetate layer, remainder is regulated pH to 9～10 with the concentrated ammonia liquor that mass concentration is 30%, then extract with chloroform until with alkaloid precipitating reagent (bismuth potassium iodide), check inanimate object alkali, combining extraction liquid, reduced pressure concentration obtains alkaloid, and is standby;
2, the preparation of plant pesticide microemulsion: take alkaloid 10g, after adding the ethanol, 20mL cosolvent ethylene glycol of the volume fraction 95% of 30mL to dissolve, after adding again the 15mL Tween-80 to stir, add water and be settled to 100mL, obtain plant alkaloid complex microemulsion product 100mL.Get as required former medicine during test in right amount in miniaturised nebuliser, directly add clear water to stir, obtain required corresponding diluted concentration.
3, carry out field efficacy with above-mentioned embodiment gained plant alkaloid complex microemulsion, test as follows:
The computational methods of insect population decline rate and corrected mortality are:
(1) field experiment and the result of control Wolfberry Aphid:
Take 2.5% gamma cyhalothrin, 40% phoxim as the contrast medicament, the dilution respective concentration, separately establishing 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, Wolfberry Aphid insect population radix is higher, worm amount distribution uniform, in Wolfberry Aphid harm district, (10% with the alkaloid volume fraction in 10%, in following form, the 10% other mg/l of unit used of microemulsion is biological alkali mass concentration) built-up microemulsion dilution agent respective concentration is reagent,, take clear water as contrast (CK), use the small hand-held sprayer, the complete stool even spraying.10 branches are randomly drawed in each processing, fixing listing mark, and whole Aphed populations of investigation 20cm place, branch top every branches and leaves sheet positive and negative, investigate the insect population radix before dispenser, after medicine the 3rd, 5,7,10,15d investigates respectively remaining insect population quantity.Calculate insect population decline rate and control efficiency.
The field efficacy of table 1 microemulsion to Wolfberry Aphid
(2) field trial and the result of control diamond-back moth.
Be reagent with above-mentioned gained built-up microemulsion dilution agent respective concentration, take 2.5% gamma cyhalothrin, 40% phoxim as the contrast medicament, the dilution respective concentration, separately establishing the spray clear water is blank, other field trials with Wolfberry Aphid are identical.
The field efficacy of table 2 microemulsion to diamond-back moth
By table 1, table 2 as can be known, the 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, afterwards the drug effect continuous decrease; 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 Wolfberry 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 (1)
1. the preparation method of a plant alkaloid complex microemulsion, is characterized in that, comprises the steps:
(1) the alkaloidal extraction of active ingredient: the Sophora alopecuroide dry powder that takes the Cynanchum Komarovii of 600g and 300g adds the ethanol of the volume fraction 95% of 720mL, soaked 24 hours under normal temperature, then ultrasonic extraction, the extraction temperature is 35-45 ℃, extraction time is 35-45 minute, filtering and collecting filter liquid, repeat aforesaid operations lixiviate 3 times, merge 3 times filtrate, reduced pressure concentration, solvent evaporated, obtain ethanol extract;
The hydrochloric acid that adds wherein volume fraction 2% transfers to the pH value with extract and is 5-6, use ethyl acetate extraction, remove ethyl acetate layer, remainder is regulated pH to 9～10 with the concentrated ammonia liquor that mass concentration is 30%, then extract with chloroform until with alkaloid precipitating reagent bismuth potassium iodide, check inanimate object alkali, combining extraction liquid, reduced pressure concentration obtains alkaloid, and is standby;
(2) preparation of plant pesticide microemulsion: take alkaloid 10g, after adding the ethanol, 20mL cosolvent ethylene glycol of the volume fraction 95% of 30mL to dissolve, after adding again the 15mL Tween-80 to stir, add water and be settled to 100mL, obtain plant alkaloid complex microemulsion product 100mL.
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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 |
| 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 |
| 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 |
| 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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