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CN103081954A - Alcoholic solution preparation of wartwort secondary metabolism product and preparation method thereof - Google Patents

Alcoholic solution preparation of wartwort secondary metabolism product and preparation method thereof Download PDF

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CN103081954A
CN103081954A CN201310052036XA CN201310052036A CN103081954A CN 103081954 A CN103081954 A CN 103081954A CN 201310052036X A CN201310052036X A CN 201310052036XA CN 201310052036 A CN201310052036 A CN 201310052036A CN 103081954 A CN103081954 A CN 103081954A
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preparation
ethanol
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杜春华
马霖
许艳秋
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Qingdao Agricultural University
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Abstract

本发明公开一种泽漆次生代谢物质的乙醇溶液植物杀虫制剂及其制备方法。本发明将泽漆制成溶液制剂的方法为:将泽漆全草烘干,粉碎至30-100目;于搅拌容器中加入泽漆及4-6倍重量乙醇,在20-70℃下浸取6-72小时,间歇搅拌或全程持续搅拌,过滤得浸提液;向滤渣加入2-5倍原泽漆重量的乙醇,在20-70℃下浸取6-48小时,间歇搅拌或全程持续搅拌,过滤,该浸取和过滤过程重复1-3次;合并浸提液,浸提液减压蒸发得固形物5-20%的浓缩液并回收乙醇;分别加入0.002-0.15倍浓缩液重量的助溶剂、稳定剂、增效剂和乳化剂;搅拌0.2-3小时,过滤,得泽漆次生代谢物质的醇溶液制剂。The invention discloses an ethanol solution plant insecticide preparation of lacquer secondary metabolites and a preparation method thereof. The method of making the varnish into a solution preparation of the present invention is as follows: dry the whole varnish and crush it to 30-100 mesh; Take for 6-72 hours, stir intermittently or continuously throughout the whole process, and filter to obtain the extract; add 2-5 times the weight of ethanol to the filter residue, leaching at 20-70°C for 6-48 hours, stir intermittently or throughout the process Continue to stir, filter, repeat the leaching and filtering process 1-3 times; combine the extracts, evaporate the extracts under reduced pressure to obtain a concentrated solution with 5-20% solids and recover ethanol; add 0.002-0.15 times the concentrated solution respectively Cosolvent, stabilizer, synergist and emulsifier by weight; stirred for 0.2-3 hours, filtered, and alcohol solution preparation of secondary metabolites of Deze paint.

Description

泽漆次生代谢物质的醇溶液制剂及其制备方法Alcoholic solution preparation of secondary metabolites of varnish and its preparation method

技术领域 technical field

本发明涉及一种从大戟科(Euphorbiaceae)大戟属草本植物泽漆(Euphorbia helioscopia L.)提取次生代谢物质,并用提取物配制农业杀虫剂的方法。 The invention relates to a method for extracting secondary metabolites from Euphorbia helioscopia L., an herb of the genus Euphorbia ( Euphorbiaceae ), and preparing an agricultural insecticide with the extract.

背景技术 Background technique

随着人们对环境、食品安全的日益关注,以及农业病、虫、草抗药性的发展,人们更加重视从天然产物中寻找新农药的研究途径。从天然植物中寻找农药活性成分的研究方兴未艾。与有机合成农药相比,植物源农药具有低毒、易降解、害物不易产生抗性等特点。 As people pay more and more attention to the environment and food safety, as well as the development of pesticide resistance of agricultural diseases, insects, and weeds, people pay more attention to the research of finding new pesticides from natural products. The research on finding pesticide active ingredients from natural plants is in the ascendant. Compared with organic synthetic pesticides, botanical pesticides have the characteristics of low toxicity, easy degradation, and resistance to pests.

泽漆作为传统中药材在我国有悠久的应用历史。据《本草纲目》记载, 泽漆有利水消肿、消痰退热、散结杀虫等功效。在当代,临床可用于治疗水肿、腹水、痰多咳喘、恶性肿瘤等疾病。用泽漆杀灭人粪尿池中蛆虫以减少苍蝇孽生量在我国民间也有较长的应用史。多年来,植物化学研究者从泽漆中发现了包括萜类、黄酮类、有机酸、酚类、甾体类等不同结构类型具有生理活性的次生代谢产物,引起药物学、农药学,以及化学科技工作者的广泛关注。 As a traditional Chinese medicinal material, lacquer has a long history of application in my country. According to the records in "Compendium of Materia Medica", Zeqi has the effects of diuresis, swelling, phlegm, fever, stagnation and insecticide. In modern times, it can be used clinically to treat diseases such as edema, ascites, phlegm, cough and asthma, and malignant tumors. The use of varnish to kill maggots in human excrement and urine pools to reduce the number of flies has a long history of application among the people of our country. Over the years, phytochemical researchers have discovered physiologically active secondary metabolites of different structural types including terpenes, flavonoids, organic acids, phenols, steroids, etc. from varnish, causing pharmacology, pesticides, and Wide attention of chemical science and technology workers.

发明内容 Contents of the invention

本发明的目的是采用纯天然中草药泽漆为原料,提取次生代谢物质并配以表面活性剂、增效剂等各种助剂制成农业杀虫剂,害虫接触后产生触杀、胃毒、拒食等作用,从而达到无公害治理虫害的目的。 The purpose of the present invention is to use pure natural Chinese herbal medicine lacquer as raw material, extract secondary metabolites and prepare agricultural insecticides with various auxiliary agents such as surfactants and synergists, and produce contact killing, stomach poisoning, Anti-feeding and other functions, so as to achieve the purpose of pollution-free control of pests.

本发明对泽漆次生代谢物质进行提取并制备农业杀虫剂的方法为:将烘干的泽漆粉碎至30-100目;于搅拌容器中加入泽漆及4-6倍重量乙醇,在20-70℃下浸取6-72小时,间歇搅拌或全程持续搅拌,过滤得浸提液;向滤渣加入2-5倍原泽漆重量乙醇,在20-70℃下浸取6-48小时,间歇搅拌或全程持续搅拌,过滤,该浸取和过滤过程重复1-3次;合并浸提液,浸提液减压蒸发得固形物5-20%的浓缩液并回收乙醇;分别加入0.002-0.15倍浓缩液重量的助溶剂、稳定剂、增效剂和乳化剂,其中助溶剂、稳定剂、增效剂可同时使用或仅使用其中的一种或两种;搅拌0.2-3小时,过滤,得泽漆次生代谢物质的醇溶液制剂。 The method for extracting the secondary metabolites of the varnish and preparing the agricultural insecticide in the present invention is as follows: pulverize the dried varnish to 30-100 mesh; Leach at 20-70°C for 6-72 hours, stir intermittently or continuously throughout the process, and filter to obtain the extract; add 2-5 times the weight of the original varnish to the filter residue with ethanol, and leach at 20-70°C for 6-48 hours , stirring intermittently or continuously throughout the whole process, and filtering. The leaching and filtering process is repeated 1-3 times; the leaching solution is combined, and the leaching solution is evaporated under reduced pressure to obtain a concentrated solution of 5-20% solids and recover ethanol; add 0.002 - 0.15 times the weight of the concentrate, co-solvent, stabilizer, synergist and emulsifier, wherein co-solvent, stabilizer and synergist can be used simultaneously or only one or two of them can be used; stir for 0.2-3 hours, Filtration, alcohol solution preparation of secondary metabolites of Deze paint.

本发明所述助溶剂为苯甲酸钠或水杨酸钠;稳定剂为N,N-二甲基甲酰胺;增效剂为氮酮;乳化剂为Tween20、Tween40、Tween60、Tween80中的1种或数种与OP-10的混合物。 The co-solvent of the present invention is sodium benzoate or sodium salicylate; the stabilizer is N,N-dimethylformamide; the synergist is azone; the emulsifier is one or more of Tween20, Tween40, Tween60, Tween80 Several mixtures with OP-10.

本发明的优点:(1)泽漆次生代谢物质在自然条件下易于降解,对生态系统和食品生产安全;(2)泽漆植物杀虫剂是不同结构类型的多种成分的混合物,对害虫产生多位点、不同机制的作用,不易产生抗药性;(3)提取工艺稳定;(4)对菜青虫、苹梢鹰夜蛾、草履蚧等多种害虫有效,并可用于灌根防治韭蛆等地下害虫。 The advantages of the present invention: (1) the secondary metabolites of lacquer are easy to degrade under natural conditions, and are safe to the ecological system and food production; Pests produce multiple sites and different mechanisms, and are not easy to produce drug resistance; (3) The extraction process is stable; (4) Effective against various pests such as cabbage caterpillar, hawk moth, and paramecium, and can be used for root irrigation control Leek maggots and other underground pests.

具体实施方式 Detailed ways

下属实施例用于进一步说明本发明,但不限于本发明。 The following examples are used to further illustrate the present invention, but not limit the present invention.

提取及溶液制剂的制备例: Examples of extraction and preparation of solution preparations:

将烘干的泽漆粉碎至60目;于搅拌容器中加入300克泽漆和1500克乙醇,在25℃下浸取72小时,每6小时搅拌0.5小时,过滤得浸提液;向滤渣加入1000克乙醇,在25℃下浸取48小时,每3小时搅拌0.5小时,过滤,该浸取和过滤过程重复2次;合并浸提液,浸提液减压蒸发得固形物10%的浓缩液;加入浓缩液重量0.01倍的水杨酸钠,0.005倍N,N-二甲基甲酰胺,0.01倍的氮酮,0.03倍的Tween80、0.05倍的OP-10,搅拌1小时,过滤,得泽漆次生代谢物质的醇溶液制剂。 Grind the dried varnish to 60 mesh; add 300 grams of varnish and 1500 grams of ethanol to a stirring container, soak for 72 hours at 25 ° C, stir for 0.5 hours every 6 hours, and filter to obtain the extract; add to the filter residue 1000 grams of ethanol, leaching at 25°C for 48 hours, stirring every 3 hours for 0.5 hours, filtering, repeating the leaching and filtering process twice; combining the extracts, and evaporating the extracts under reduced pressure to obtain a concentration of 10% of the solids solution; add 0.01 times the weight of concentrated solution of sodium salicylate, 0.005 times of N,N-dimethylformamide, 0.01 times of azone, 0.03 times of Tween80, 0.05 times of OP-10, stir for 1 hour, filter, Alcoholic solution preparation of secondary metabolites of Deze paint.

杀虫活性典型测定: Typical determination of insecticidal activity:

将泽漆次生代谢物质的醇溶液制剂用水稀释300倍。在干净培养皿底部铺一张滤纸,吸取1ml的药液润湿滤纸,从采集到的韭蛆中挑选大小一致、健康无损伤的个体放到已润湿的滤纸上,每个培养皿放20只,放在适宜条件下培养,用黑布遮光,并适时补加水保持湿润,每隔一段时间观察一次韭蛆的活动情况,观察时用毛笔轻触韭蛆身体,不动者视为死亡。记录韭蛆的死亡情况,计算得韭蛆60小时的死亡率为85%。 The alcohol solution preparation of the secondary metabolites of the varnish is diluted 300 times with water. Lay a piece of filter paper on the bottom of a clean petri dish, absorb 1ml of liquid medicine to moisten the filter paper, select healthy and undamaged individuals of the same size from the collected leek maggots and put them on the wetted filter paper, put 20 in each petri dish. The maggots were cultured under suitable conditions, shaded with a black cloth, and kept moist by adding water at an appropriate time. The activities of the maggots were observed at regular intervals. During the observation, the maggots were lightly touched with a brush, and those who did not move were regarded as dead. Record the death situation of leek maggot, calculate the death rate of leek maggot 60 hours to be 85%.

Claims (4)

1.一种泽漆次生代谢物质乙醇溶液植物杀虫剂,其特征在于:以中草药为原料,用乙醇提取并配以助溶剂、稳定剂、增效剂和乳化剂而成,其制备方法为:将泽漆全草烘干,粉碎至30-100目;于搅拌容器中加入泽漆及4-6倍重量乙醇,在20-70℃下浸取6-72小时,间歇搅拌或全程持续搅拌,过滤得浸提液;向滤渣加入2-5倍原泽漆重量的乙醇,在20-70℃下浸取6-48小时,间歇搅拌或全程持续搅拌,过滤,该浸取和过滤过程重复2-3次;合并浸提液,浸提液减压蒸发得固形物5-20%的浓缩液并回收乙醇;分别加入0.002-0.15倍浓缩液重量的助溶剂、稳定剂、增效剂和乳化剂,其中助溶剂、稳定剂、增效剂可同时使用或仅使用其中的一种或两种;搅拌0.2-3小时,过滤,得泽漆次生代谢物质的醇溶液制剂。 1. a lacquer secondary metabolite ethanol solution plant insecticide is characterized in that: taking Chinese herbal medicine as raw material, extracting with ethanol and forming with cosolvent, stabilizer, synergist and emulsifier, its preparation method Method: dry the whole herb of varnish and crush it to 30-100 mesh; add varnish and 4-6 times the weight of ethanol in a stirring container, soak at 20-70°C for 6-72 hours, stir intermittently or continue the whole process Stir and filter to obtain the extract; add 2-5 times the weight of ethanol to the filter residue, and leaching at 20-70°C for 6-48 hours, stirring intermittently or continuously throughout the process, and filtering, the leaching and filtering process Repeat 2-3 times; combine the extracts, evaporate the extracts under reduced pressure to obtain a concentrated solution with 5-20% solids and recover ethanol; add 0.002-0.15 times the weight of the concentrated solution as a co-solvent, stabilizer, and synergist And emulsifier, in which cosolvent, stabilizer and synergist can be used at the same time or only one or two of them can be used; stir for 0.2-3 hours, filter, and obtain the alcohol solution preparation of the secondary metabolites of Deze paint. 2.如权利要求1所述的制剂及其制备方法,其特征在于所述的助溶剂为苯甲酸钠或水杨酸钠;所述稳定剂为N,N-二甲基甲酰胺;增效剂为氮酮;所述乳化剂为Tween20、Tween40、Tween60、Tween80中的1种或数种与OP-10的混合物。 2. preparation as claimed in claim 1 and preparation method thereof, it is characterized in that described solubilizer is sodium benzoate or sodium salicylate; Described stabilizer is N, N-dimethylformamide; Synergist It is azone; the emulsifier is a mixture of one or more of Tween20, Tween40, Tween60, Tween80 and OP-10. 3.如权利要求1所述的制剂及其制备方法,助溶剂、稳定剂、增效剂可同时使用或仅使用其中的一种或两种。 3. preparation as claimed in claim 1 and preparation method thereof, cosolvent, stabilizer, synergist can use simultaneously or only use wherein one or both. 4.如权利要求2所述苯甲酸钠、水杨酸钠、N,N-二甲基甲酰胺、氮酮、Tween20、Tween40、Tween60、Tween80、OP-10均具有助溶、稳定、助渗、增效、增溶、乳化等多种功能中的数种,权利要求2所述为其多种成分的组合物,而不限于所述功能。 4. as claimed in claim 2, sodium benzoate, sodium salicylate, N,N-dimethylformamide, azone, Tween20, Tween40, Tween60, Tween80, OP-10 all have dissolution aid, stability, penetration aid, Several of multiple functions such as synergism, solubilization, emulsification, etc., are described in claim 2 as a composition of multiple components, and are not limited to the functions.
CN201310052036XA 2013-02-18 2013-02-18 Alcoholic solution preparation of wartwort secondary metabolism product and preparation method thereof Pending CN103081954A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105669378A (en) * 2016-01-06 2016-06-15 安徽医科大学 Euphorbia helioscopia extract, preparation method and application thereof
CN111937906A (en) * 2020-08-31 2020-11-17 江西鑫邦科技有限责任公司 Plant growth regulating mixture and preparation method and application thereof
CN112006022A (en) * 2020-09-03 2020-12-01 山东农业大学 Reagent for overcoming self-incompatibility of brassica and radish and use method and application thereof

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CN102210334A (en) * 2011-04-21 2011-10-12 北京农学院 New application of euphorbia helioscopia in plant mite killing

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CN102210334A (en) * 2011-04-21 2011-10-12 北京农学院 New application of euphorbia helioscopia in plant mite killing

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105669378A (en) * 2016-01-06 2016-06-15 安徽医科大学 Euphorbia helioscopia extract, preparation method and application thereof
CN105669378B (en) * 2016-01-06 2018-12-28 安徽医科大学 Herba Euphorbiae Helioscopiae extract and preparation method and its usage
CN111937906A (en) * 2020-08-31 2020-11-17 江西鑫邦科技有限责任公司 Plant growth regulating mixture and preparation method and application thereof
CN112006022A (en) * 2020-09-03 2020-12-01 山东农业大学 Reagent for overcoming self-incompatibility of brassica and radish and use method and application thereof
CN112006022B (en) * 2020-09-03 2021-04-20 山东农业大学 Reagent for overcoming self-incompatibility of brassica and radish and use method and application thereof

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Application publication date: 20130508