CN1049895C - Extraction of sophora alopecuroides extract and its composition - Google Patents
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- 238000000605 extraction Methods 0.000 title claims abstract description 10
- 239000000203 mixture Substances 0.000 title claims description 9
- 241001145009 Sophora alopecuroides Species 0.000 title 1
- 239000000575 pesticide Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract 2
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- 238000000034 method Methods 0.000 claims description 9
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 5
- DWFZBUWUXWZWKD-UHFFFAOYSA-N pyridaben Chemical compound C1=CC(C(C)(C)C)=CC=C1CSC1=C(Cl)C(=O)N(C(C)(C)C)N=C1 DWFZBUWUXWZWKD-UHFFFAOYSA-N 0.000 claims description 5
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- 238000010992 reflux Methods 0.000 claims description 4
- 239000005949 Malathion Substances 0.000 claims description 3
- 229960001701 chloroform Drugs 0.000 claims description 3
- JXSJBGJIGXNWCI-UHFFFAOYSA-N diethyl 2-[(dimethoxyphosphorothioyl)thio]succinate Chemical compound CCOC(=O)CC(SP(=S)(OC)OC)C(=O)OCC JXSJBGJIGXNWCI-UHFFFAOYSA-N 0.000 claims description 3
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- ZSBXGIUJOOQZMP-UHFFFAOYSA-N Isomatrine Natural products C1CCC2CN3C(=O)CCCC3C3C2N1CCC3 ZSBXGIUJOOQZMP-UHFFFAOYSA-N 0.000 claims 1
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 claims 1
- SKOLRLSBMUGVOY-GBJTYRQASA-N aloperine Chemical compound C1=C2CCCN[C@H]2[C@H]2CN3CCCC[C@@H]3[C@@H]1C2 SKOLRLSBMUGVOY-GBJTYRQASA-N 0.000 claims 1
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- ANJTVLIZGCUXLD-BDAKNGLRSA-N (-)-Cytisine Natural products C1NC[C@@H]2CN3C(=O)C=CC=C3[C@H]1C2 ANJTVLIZGCUXLD-BDAKNGLRSA-N 0.000 description 2
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- 229930017327 cytisine Natural products 0.000 description 2
- ANJTVLIZGCUXLD-UHFFFAOYSA-N ent-cytisine Natural products C1NCC2CN3C(=O)C=CC=C3C1C2 ANJTVLIZGCUXLD-UHFFFAOYSA-N 0.000 description 2
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- OWZREIFADZCYQD-NSHGMRRFSA-N deltamethrin Chemical compound CC1(C)[C@@H](C=C(Br)Br)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 OWZREIFADZCYQD-NSHGMRRFSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- NAGJZTKCGNOGPW-UHFFFAOYSA-K dioxido-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [O-]P([O-])([S-])=S NAGJZTKCGNOGPW-UHFFFAOYSA-K 0.000 description 1
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- XQUXKZZNEFRCAW-UHFFFAOYSA-N fenpropathrin Chemical compound CC1(C)C(C)(C)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 XQUXKZZNEFRCAW-UHFFFAOYSA-N 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明涉及苦豆子提取物的提取技术及采用该提取物与多种化学农药加工成乳油制剂的技术。本发明将两者按苦豆子提取物1-3；化学农药1的比例加工成乳油，使有效含量达到8-30%。由于两者对有害生物的作用机制不同，作用方式有异并且有明显的增效作用，使之成为目前防治有害生物的“无公害”或“少公害”的有效药剂，对人、畜安全，社会和经济效益显著。The invention relates to the extraction technology of Sophora sophorae extract and the technology of processing the extract into emulsifiable concentrate preparation with various chemical pesticides. In the present invention, the two are processed into emulsifiable concentrate according to the ratio of 1-3 of the Sophora japonica extract and 1 of the chemical pesticide, so that the effective content reaches 8-30%. Due to the different mechanism of action of the two on harmful organisms, the mode of action is different and there is obvious synergistic effect, making it an effective agent for "no pollution" or "less pollution" for the prevention and control of harmful organisms. It is safe for humans and animals. The social and economic benefits are remarkable.
Description
本发明涉及有苦豆子提取物的提取技术及用该技术产生的苦豆子提取物与化学农药的复配技术。The present invention relates to the extraction technology of Sophora sophora extract and the compounding technology of Sophora sophora extract and chemical pesticide produced by the technology.
苦豆子是一种豆科植物，其植物本身及其次生代谢物质有一定的驱虫杀菌功效。在环境中无残留隐患。Bitter bean is a kind of leguminous plant, the plant itself and its secondary metabolites have a certain effect of repelling insects and killing bacteria. No residual hazards in the environment.
拟除虫菊酯类杀虫刹(包括氰戊菊酯、溴氰菊酯、氯氰菊酯、氟氯氰菊酯、三氟氯氰菊酯及甲氰菊酯等)是一类对多种害虫高效且对高等动物毒性较低的杀虫剂，但由于多种害虫对其产生了高度抗性及农用成本高，已在很大程度上限制了此类杀虫剂的使用。Pyrethroid insecticides (including fenvalerate, deltamethrin, cypermethrin, cyfluthrin, cyhalothrin and fenpropathrin, etc.) are a class of insecticides that are highly effective against various pests and have low toxicity to higher animals. However, due to the high resistance of various pests to it and the high cost of agricultural use, the use of such insecticides has been limited to a large extent.
辛硫磷(O，O-二乙基-O-[对-苯基氰基甲醛]-硫代磷酸酯)是一种速效低毒的有机磷酸酯类杀虫剂，对多种害虫有较好的防治作用，但由于害虫对其产生了抗性及对螨类效果差，在生产中限制了其使用。Phoxim (O, O-diethyl-O-[p-phenylcyanoformaldehyde]-phosphorothioate) is a fast-acting and low-toxic organophosphate insecticide, which is effective against various pests. It has a good control effect, but due to the resistance of pests to it and the poor effect on mites, its use is limited in production.
马拉硫磷(O，O-二甲基-S-[1，2-二乙氧羰基]二硫代磷酸酯)是一种具内吸作用的低毒有机磷酸酯类杀虫杀螨剂，但由于害虫(螨)对其产生了高度抗药性，极大地限制了其在生产上的使用。Malathion (O, O-dimethyl-S-[1,2-diethoxycarbonyl] phosphorodithioate) is a low-toxic organophosphate insecticide and acaricide with systemic action , but due to the high resistance of pests (mite) to it, its use in production is greatly limited.
丙溴磷(O-[4-溴-2-氯苯基]-S-正丙基硫代磷酸酯)是一种新型三元不对称有机磷酸酯类杀虫剂，对多种害虫有较好的防治作用，但由于其对害虫速效性差、对害螨效果不理想及农用成本高的缺点，在生产上限制了其使用。Profenofos (O-[4-bromo-2-chlorophenyl]-S-n-propyl phosphorothioate) is a new type of ternary asymmetric organophosphate insecticide, which is effective against various pests. Good control effect, but due to its poor quick-acting effect on pests, unsatisfactory effect on harmful mites and high agricultural cost, its use is limited in production.
哒螨酮(2-特丁基-5-[4-特丁基苄硫基]4-氯哒嗪-3[2H]-酮)是一种高效杀螨剂，由于其成本高，在应用中亦受到了限制。Pyridaben (2-tert-butyl-5-[4-tert-butylbenzylthio]4-chloropyridazin-3[2H]-one) is a highly effective acaricide. Due to its high cost, it is widely used in is also restricted.
本发明已发现：The inventors have found that:
一、使用有机溶剂如甲醇、乙醇和三氯甲烷等从苦豆子(包括茎、叶、花、果实和种子)中提取苦豆子提取物的技术。One, use organic solvents such as methanol, ethanol and chloroform etc. to extract the technology of Sophora Sophora extract from Sophora Sophora (comprising stem, leaf, flower, fruit and seed).
所涉及的提取技术为：The extraction techniques involved are:
“回流提取法”工艺：取经干燥并粉碎后的苦豆子全株或种子，装入提取器(涉及单效萃取和多效萃取)，加入原料1-10倍的有机溶剂，浸泡后回流提取，收集滤液，待取样用改良碘化铋钾试剂分析确定有效成分提取完毕后，合并滤液并取样分析，按0.1％金雀花碱(cytisine)含量定容。然后将废渣加热回收溶剂。废渣可作饲料或肥料。"Refluxing extraction method" process: Take the dried and crushed whole plant or seeds of Sophora aphorae, put it into the extractor (involving single-effect extraction and multi-effect extraction), add 1-10 times the organic solvent of the raw material, reflux extraction after soaking, Collect the filtrate, and use the modified bismuth iodide potassium reagent to analyze and confirm that the active ingredients have been extracted, then combine the filtrate and take a sample for analysis, and make the volume according to the content of 0.1% cytisine. The waste residue is then heated to recover the solvent. The waste residue can be used as feed or fertilizer.
“冷浸法”提取工艺：取干燥并粉碎之苦豆子全株或种子，加入原料重量1-10倍的上述溶剂，经充分搅拌后浸泡1-72小时，进行压滤或离心，收集滤液。然后再多次往原料中加入适量溶剂，浸泡数小时经搅拌后进行压滤或离心。将多次滤液合并，经沉淀后收集上清液按0.1％金雀花碱含量定容。然后将废渣加热回收溶剂，废渣可作饲料或肥料。"Cold soaking method" extraction process: Take the dried and crushed whole plant or seeds of Sophora japonica, add 1-10 times the weight of the raw material in the above-mentioned solvent, stir thoroughly and soak for 1-72 hours, press filter or centrifuge, and collect the filtrate. Then add an appropriate amount of solvent to the raw material several times, soak for several hours, and then press filter or centrifuge after stirring. The multiple filtrates were combined, and the supernatant was collected after precipitation to make up the volume according to the content of 0.1% cytisine. Then the waste residue is heated to recover the solvent, and the waste residue can be used as feed or fertilizer.
本发明所涉及的溶剂有：甲醇、乙醇和三氯甲烷等。The solvents involved in the present invention are: methanol, ethanol and chloroform etc.
二、苦豆子提取物与化学农药的增效复配技术。2. Synergistic compounding technology of Sophora sophora extract and chemical pesticides.
本发明涉及的原料有苦豆子提取物及杀虫、杀螨剂如氰戊菊酯、辛硫磷、马拉硫磷及哒螨酮等。The raw materials involved in the present invention include Sophora sophora extract and insecticides and acaricides such as fenvalerate, phoxim, malathion and pyridaben.
本类组合物可依据传统方法按比例加工成有效成分含量为8％-30％的乳油。This type of composition can be processed into emulsifiable concentrate with an active ingredient content of 8%-30% in proportion according to the traditional method.
本发明加工成乳油的工艺流程如下，但不限于此。
本发明所涉及的乳化剂有QR-01、QR-03、QR-11、QNR-10、农乳0201及2201等。The emulsifiers involved in the present invention include QR-01, QR-03, QR-11, QNR-10, Nongru 0201 and 2201, etc.
本发明加工成乳油可通过以下“实例”进一步加以说明。以下所有份数均指有效成分重量比。The processing of the present invention into emulsifiable concentrate can be further illustrated by the following "instances". All the following parts refer to the weight ratio of active ingredients.
实例1 苦豆子提取物 10份Example 1 Bitter bean extract 10 parts
辛硫磷 20份phoxim 20 servings
溶剂1 40份Solvent 1 40 parts
溶剂2 20份Solvent 2 20 parts
乳化剂 8份Emulsifier 8 parts
稳定剂 2份Stabilizer 2 parts
将其按上述流程加工成乳油。It is processed into emulsifiable concentrate according to the above process.
实例2 苦豆子提取物 10份Example 2 Bitter bean extract 10 parts
哒螨酮 6份Pyridaben 6 parts
溶剂1 40份Solvent 1 40 parts
溶剂2 34份Solvent 2 34 parts
乳化剂 8份Emulsifier 8 parts
稳定剂 2份Stabilizer 2 parts
将其按上述流程加工成乳油。It is processed into emulsifiable concentrate according to the above process.
使用上述实例1所涉及的农药组合物，防治抗药性菜蚜、苹果黄蚜及棉蚜的方法为：在上述害虫大发生时，将本农药组合物用水稀释成1500-2000倍液对作物进行均匀喷雾，对上述害虫第二天的防治效果为93.66-99.81％；用上述农药组合物用水稀释成1500倍液对蔬菜进行均匀喷雾，对菜青虫和小菜蛾第二天的防治效果为96.58-98.36％。Using the pesticide composition involved in the above example 1, the method for preventing and treating drug-resistant cabbage aphid, apple yellow aphid and cotton aphid is: when the above-mentioned pests occur in large numbers, the pesticide composition is diluted with water to 1500-2000 times of liquid to carry out the treatment on the crops. Uniform spraying, the control effect on the above-mentioned pests on the second day is 93.66-99.81%; the above-mentioned pesticide composition is diluted with water to 1500 times to spray vegetables evenly, and the control effect on the next day on cabbage caterpillar and diamondback moth is 96.58-99.81%. 98.36%.
使用上述实例2所涉及的农药组合物，采用水稀释3000倍的浓度，对苹果红蜘蛛第10天的防治效果为93.87％。Using the pesticide composition involved in the above example 2 and diluting it with water to a concentration of 3000 times, the control effect on apple spider mite on the 10th day was 93.87%.
实例1及2所涉及农药组合物因其对昆虫的不同作用机制及作用方式，表现了显著的增效作用，该组合物均为低毒且可大大降低农用成本及害虫抗药性的产生。The pesticide compositions involved in Examples 1 and 2 show significant synergistic effects due to their different action mechanisms and modes of action on insects. The compositions are all low-toxic and can greatly reduce agricultural costs and the generation of pest resistance.
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| CN97105689A CN1049895C (en) | 1997-02-18 | 1997-02-18 | Extraction of sophora alopecuroides extract and its composition |
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| CN97105689A CN1049895C (en) | 1997-02-18 | 1997-02-18 | Extraction of sophora alopecuroides extract and its composition |
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| CN1049895C true CN1049895C (en) | 2000-03-01 |
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| CN1110339C (en) * | 2000-06-19 | 2003-06-04 | 宁夏药物研究所 | Process for preparing total allooerine liquid |
| CN101139234B (en) * | 2007-08-13 | 2011-03-30 | 淮安市农业科学研究院 | Nuisance-free medical fertilizers for prevention and curing of nematode and underground pest and production process thereof |
| CN101624393B (en) * | 2009-08-04 | 2011-08-24 | 王答祺 | Method for extracting cytosine and thermopsine from thermopsis lanceolata seeds |
| CN103371169B (en) * | 2012-04-16 | 2014-10-22 | 上海韬鸿化工科技有限公司 | Sophoramine insect-preventing missible oil, sophoramine insect-preventing fabric and preparation method of fabric |
| CN103651427B (en) * | 2012-09-21 | 2015-02-11 | 上海韬鸿化工科技有限公司 | Mosquito repellent cream, mosquito repellent mat and preparation method thereof |
| CN103585262A (en) * | 2013-08-31 | 2014-02-19 | 内蒙古农牧业科学院 | Sophora alopecuroides L alkaloid preparation for preventing and curing livestock ectoparasite disease |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134282A (en) * | 1995-04-27 | 1996-10-30 | 贾毅 | Tea for sobering up |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1134282A (en) * | 1995-04-27 | 1996-10-30 | 贾毅 | Tea for sobering up |
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