CN1386423A - Aqueous solution of insecticide of black nightshade root and its preparing process - Google Patents
Aqueous solution of insecticide of black nightshade root and its preparing process Download PDFInfo
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- CN1386423A CN1386423A CN 02111915 CN02111915A CN1386423A CN 1386423 A CN1386423 A CN 1386423A CN 02111915 CN02111915 CN 02111915 CN 02111915 A CN02111915 A CN 02111915A CN 1386423 A CN1386423 A CN 1386423A
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Abstract
An aqueous solution of insecticide is prepared from black nightshade root, water and adsorbent through washing black nightshade roots, drying in air at 20-30 deg.C, pulverizing by 20-40 meshes, extracting in the solvent prepared from ethanol (or methanol) and water 4 times (24 hr for each once), vacuum concentrating, dissolving in water, extracting in ethylacetate 6 times, vacuum concentrating, dissolving in water, chromatography in silicon gel column sequentially using ethanol, methanol and water as eluent, vacuum concentrating, and dissolving in water. Its advantages are high effect and no environmental pollution.
Description
Technical field: what the present invention relates to is a kind of aqueous solution of insecticide and preparation method thereof, and particularly a kind of aqueous solution of insecticide of black nightshade root and preparation method thereof belongs to pesticide field.
Background technology: black nightshade (Solanum nigrum L.), plant of Solanaceae is distributed in the most of provinces and regions of China, and resource is very abundant, is a kind of weeds, and large stretch of single giving birth to or mixed giving birth to often arranged, and is born in the hillside border, and irritate in the thick grass and between the garden, village at the small stream side; Also can utilize the wild country, deserted mountain to carry out artificial planting.Be used for prevention and elimination of disease and pests about black nightshade on agricultural, on the books in " Chinese agriculture encyclopedia " (agricultural chemicals volume) book: the black nightshade herb can be prevented and treated rice borer and two spotted spider mite, does not do further investigation but have the people afterwards.Through prior art retrieval is found: Chinese patent application number is: 99100079.X, name is called: " a kind of vegetalitas colorado potato beetle special-purpose insecticide ", this patent application technology is the mixing of several plant extract, and black nightshade is only as wherein a plant species, utilization be the black nightshade herb; And it is only effective to colorado potato beetle, is not further finding with the bibliographical information of black nightshade root as control vegetable-crop pest-insect and garden pest insects in the retrieval.
Summary of the invention: the objective of the invention is to overcome deficiency of the prior art, a kind of aqueous solution of insecticide of black nightshade root and preparation method thereof is provided, the present invention is to various vegetables insect such as diamond-back moth, cabbage caterpillar, the negative locust of short volume, phyllotreta striolata and daicon leaf beetle etc., and garden pest insects such as evonymus looper, the wild snout moth's larva of little sawfly of rose and Chinese littleleaf box thin,tough silk etc. all shows high antifeedant activity, especially the antagonism diamond-back moth has good control efficiency, and the present invention is directly used in the nuisanceless of control vegetable-crop pest-insect and garden pest insects, pollution-free, liquid insecticide as agricultural chemical prepared from natural plant of no residual hazard and preparation method thereof.The present invention is achieved by the following technical solutions:
Each weight percentages of components of the present invention is: black nightshade root extract 7-10%, water 89.84-92.96%, adsorbent 0.04-0.16%.Black nightshade extract is to be raw material with the black nightshade root, adopts technology such as solvent extraction method, solvent extraction, normal phase column chromatography and is prepared from conjunction with concentrate drying, drying at room temperature method, and water is distilled water or deionized water.Adsorbent is in order to increase the adsorptivity of medicament.
Preparation method of the present invention is specific as follows:
(1), gather black nightshade root, clean and dry the back and become 20-40 order particle in 20-30 ℃ of following crushed after being dried;
(2), with 10 times of mixed solvents to black nightshade root crushed material weight, the ethanol in the mixed solvent: water be 4: 1 or with the mixed solvent of methyl alcohol and water or directly water as solvent;
(3), at ambient temperature flood and extract 4 times, 1 time 24 hours, the method with vacuum concentration was condensed into paste with the mixed solvent extract, got the black nightshade root extract;
(4), utilize ultrasonic, behind low amounts of water dissolving paste, with equal-volume ethyl acetate extraction 6 times;
(5), with water layer extract vacuum concentration after do, with the low amounts of water dissolving, be leacheate with ethanol, first alcohol and water successively, silica G (100-200 order) is carried out column chromatography and is obtained active principle;
(6), the component vacuum concentration is become paste, with the 2-3 water-soluble aqueous solution of insecticide of black nightshade root that solves doubly.
The present invention has substantive distinguishing features and marked improvement, following advantage is compared with prior art arranged: environmentally safe; To people, animal and Environmental security, be the agent of a kind of nuisance-free plant insects; This aqueous solution of insecticide is that wide to distribute, resourceful wild plant black nightshade root is a raw material, and is easy to artificial cultivation; Help the better utilization resource, acrial part is as Chinese herbal medicine, and under ground portion is as agricultural chemicals; Extraction process is simple, need not special instrument, and the solvent after the recovery also can reuse; Have certain action spectrum, vegetable-crop pest-insect (as diamond-back moth, cabbage caterpillar, daikon leaf beetle, the negative locust of short volume and phyllotreta striolata) and garden pest insects (as evonymus looper, the little sawfly of rose and Chinese littleleaf box thin,tough silk open country snout moth's larva etc.) are all had good control efficiency.
Embodiment: below provide specific embodiment to describe in detail:
Embodiment 1: take by weighing black nightshade root powder (20 order particle) 240g, use ethanol: the mixed solvent 2400ml room temperature dipping of water=4: 1 extracts 4 times, 1 time 24 hours, vacuum concentration reclaims solvent and gets paste 44.9g, separate with 200ml is water-soluble, equal-volume ethyl acetate extraction 6 times, the water extract concentrates the back and separates with 140ml is water-soluble, get the 15ml aqueous solution, successively with ethanol, methyl alcohol, water is leacheate, and silica G (100 order) is carried out column chromatography and got active principle, is concentrated into dried component 5.47g, again with water 44.22mL, it is 10% aqua that adsorbent 0.08ml is mixed with concentration, and its bioassay results sees Table:
Table, the 10% black nightshade root extraction active principle aqueous solution is to the food refusal effect of 7 kinds of insects.
For examination insect bioassay results
Food refusal rate preventive effect
Evonymus looper 84.2% 62.5%
The little sawfly of rose 98.3% 97.2%
Diamond-back moth 74.6% 72.0%
Cabbage caterpillar 88.9%-
Phyllotreta striolata 98.5%-
The negative locust 77.0% of short volume-
Daicon leaf beetle 65.3%-
In addition, evonymus looper has been carried out field experiment, the result proves that the food refusal rate is 71.24%, and preventive effect is 63.16%, and this result is similar with the indoor bioassay result, has also proved the food refusal effect of this aqueous solution of insecticide simultaneously.
Embodiment 2: take by weighing black nightshade root powder (30 order particle) 240g, use ethanol: the mixed solvent 2400ml room temperature dipping of water=4: 1 extracts 4 times, 1 time 24 hours, vacuum concentration reclaims solvent and gets paste 44.9g, separate with 200ml is water-soluble, equal-volume ethyl acetate extraction 6 times, the water extract concentrates the back and separates with 140ml is water-soluble, get the 15ml aqueous solution, successively with ethanol, methyl alcohol, water is leacheate, silica G (150 order) is carried out column chromatography and is got active principle, be concentrated into dried component 5.47g, again with water 53.82mL, it is 8.5% aqua that adsorbent 0.59ml is mixed with concentration, and this aqua has good food refusal effect to above 7 kinds of insects, for example, the food refusal rate to representative insect diamond-back moth second instar larvae is also quite obvious.
Embodiment 3: take by weighing black nightshade root powder (40 order particle) 240g, use ethanol: the mixed solvent 2400ml room temperature dipping of water=4: 1 extracts 4 times, 1 time 24 hours, vacuum concentration reclaims solvent and gets paste 44.9g, separate with 200ml is water-soluble, equal-volume ethyl acetate extraction 6 times, the water extract concentrates the back and separates with 140ml is water-soluble, get the 15ml aqueous solution, successively with ethanol, methyl alcohol, water is leacheate, silica G (200 order) is carried out column chromatography and is got active principle, be concentrated into dried component 5.47g, again with water 67.55mL, it is 7% aqua that adsorbent 0.03ml is mixed with concentration, and this aqua is to the little sawfly of rose, cabbage caterpillar and phyllotreta striolata still have good food refusal effect and control efficiency.
Claims (3)
1, a kind of aqueous solution of insecticide of black nightshade root is characterized in that each weight percentages of components is: black nightshade root extract 7-10%, water 89.84-92.96%, adsorbent 0.04-0.16%.
2, this aqueous solution of insecticide of black nightshade root according to claim 1 is characterized in that black nightshade extract is is raw material with the black nightshade root, adopts technology such as solvent extraction method, solvent extraction, normal phase column chromatography and is prepared from conjunction with concentrate drying, drying at room temperature method.
3, a kind of preparation method of aqueous solution of insecticide of black nightshade root is characterized in that the preparation method is specific as follows:
(1), gather black nightshade root, clean and dry back crushed after being dried under 20-30C and become 20-40 order particle;
(2), with 10 times of mixed solvents to black nightshade root crushed material weight, the ethanol in the mixed solvent: water be 4: 1 or with the mixed solvent of methyl alcohol and water or directly water as solvent;
(3), at ambient temperature flood and extract 4 times, 1 time 24 hours, the method with vacuum concentration was condensed into paste with the mixed solvent extract, got the black nightshade root extract;
(4), utilize ultrasonic, behind low amounts of water dissolving paste, with equal-volume ethyl acetate extraction 6 times;
(5), with water layer extract vacuum concentration after do, with the low amounts of water dissolving, be leacheate with ethanol, first alcohol and water successively, 100-200 order silica G is carried out column chromatography and is obtained active principle;
(6), the component vacuum concentration is become paste, with the 2-3 water-soluble aqueous solution of insecticide of black nightshade root that solves doubly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 02111915 CN1386423A (en) | 2002-06-03 | 2002-06-03 | Aqueous solution of insecticide of black nightshade root and its preparing process |
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| CN 02111915 CN1386423A (en) | 2002-06-03 | 2002-06-03 | Aqueous solution of insecticide of black nightshade root and its preparing process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102511513A (en) * | 2011-11-25 | 2012-06-27 | 上海交通大学 | Compound plant bactericide, preparation thereof and application |
| CN105284931A (en) * | 2015-10-19 | 2016-02-03 | 湖南中烟工业有限责任公司 | Plant source composition for prevention and treatment of prodenia litura and plant source pesticide and application thereof |
| CN106577844A (en) * | 2016-11-15 | 2017-04-26 | 中国农业科学院麻类研究所 | Preparation for prevention and cure of pepper phytophthora blight, and production and application thereof |
-
2002
- 2002-06-03 CN CN 02111915 patent/CN1386423A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102511513A (en) * | 2011-11-25 | 2012-06-27 | 上海交通大学 | Compound plant bactericide, preparation thereof and application |
| CN102511513B (en) * | 2011-11-25 | 2014-08-06 | 上海交通大学 | Compound plant bactericide, preparation thereof and application |
| CN105284931A (en) * | 2015-10-19 | 2016-02-03 | 湖南中烟工业有限责任公司 | Plant source composition for prevention and treatment of prodenia litura and plant source pesticide and application thereof |
| CN105284931B (en) * | 2015-10-19 | 2018-01-26 | 湖南中烟工业有限责任公司 | A kind of botanical composition for preventing and treating prodenia litura and its botanical pesticide and application |
| CN106577844A (en) * | 2016-11-15 | 2017-04-26 | 中国农业科学院麻类研究所 | Preparation for prevention and cure of pepper phytophthora blight, and production and application thereof |
| CN106577844B (en) * | 2016-11-15 | 2019-08-30 | 中国农业科学院麻类研究所 | Prevent and treat capsicum epidemic disease preparation, its preparation and application |
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