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CN106135298A - Radix Carpesii extract and its preparation method and application - Google Patents

Radix Carpesii extract and its preparation method and application Download PDF

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CN106135298A
CN106135298A CN201610604491.XA CN201610604491A CN106135298A CN 106135298 A CN106135298 A CN 106135298A CN 201610604491 A CN201610604491 A CN 201610604491A CN 106135298 A CN106135298 A CN 106135298A
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extract
tianmingjing
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ethyl acetate
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胡林峰
朱红霞
杨晓迅
张百重
崔茂金
王昊鹏
朱英慧
李鹏
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Henan Institute of Science and Technology
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/12Asteraceae or Compositae [Aster or Sunflower family], e.g. daisy, pyrethrum, artichoke, lettuce, sunflower, wormwood or tarragon

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Biotechnology (AREA)
  • Botany (AREA)
  • Chemical & Material Sciences (AREA)
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  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

本发明公开了天名精提取物及其制备方法和应用。本发明的天名精杀菌剂对环境安全,天名精杀菌剂中的活性化合物是天然存在的物质,来源于自然,在长期的进化过程中已形成了其固有的参与能量与物质循环代谢途径,所以施用于环境中或植物上无残留,不会引起生物富集;对非靶标生物相对安全;对植物病原菌的作用机理不同于常规农药,使用后病原菌不易对其产生抗药性,对病原菌对常规杀菌剂的抗药性也有延缓作用。The invention discloses Tianmingjing extract, its preparation method and application. The Tianmingjing fungicide of the present invention is safe to the environment, and the active compound in the Tianmingjing fungicide is a naturally occurring substance, derived from nature, and has formed its inherent pathway of participating in energy and material cycle metabolism during the long-term evolution process , so there is no residue in the environment or on plants, and it will not cause bioaccumulation; it is relatively safe for non-target organisms; the mechanism of action on plant pathogens is different from conventional pesticides, and pathogens are not easy to develop resistance to them after use. Resistance to conventional fungicides also has a delaying effect.

Description

天名精提取物及其制备方法和应用Tianmingjing extract and its preparation method and application

技术领域technical field

本发明涉及植物提取物及其应用,具体涉及天名精提取物及其制备方法和应用。The invention relates to plant extracts and applications thereof, in particular to Tianmingjing extracts, preparation methods and applications thereof.

背景技术Background technique

自20世纪40年代以来,化学农药因其品种多、见效快、使用方便、价格低廉等特点而在农药市场中占据主导地位。然而,由于人们对化学农药的不合理使用和农药本身固有的缺点。致使化学农药在使用中产生了环境污染、人畜中毒、农药残留等问题。随着人们生活质量的提高和环保意识的增强.开发对人畜安全、无污染、低毒、低残留的生物农药已成为农药领域研究的新热点。植物源农药作为生物合理性农药的一部分,其开发研究一直是新农药研究的热点课题之一。植物源农药来源于自然,能在自然界降解.一般不会污染环境及农产品,在环境和人体中积累毒性的可能性不大,对人和牲畜相对安全,对害虫天敌伤害小,具有低毒、低残留的特点,能够保持农产品的高品质,因此植物源农药具有广阔的市场。Since the 1940s, chemical pesticides have dominated the pesticide market due to their variety, quick effect, convenient use, and low price. However, due to people's irrational use of chemical pesticides and the inherent shortcomings of pesticides. As a result, problems such as environmental pollution, human and animal poisoning, and pesticide residues have occurred in the use of chemical pesticides. With the improvement of people's quality of life and the enhancement of environmental awareness, the development of bio-pesticides that are safe for humans and animals, non-polluting, low-toxic, and low-residue has become a new hot spot in the field of pesticide research. As a part of biologically rational pesticides, the development and research of botanical pesticides has always been one of the hot topics in the research of new pesticides. Botanical pesticides are derived from nature and can be degraded in nature. Generally, they do not pollute the environment and agricultural products, and are less likely to accumulate toxicity in the environment and the human body. They are relatively safe for humans and livestock, have little damage to natural enemies of pests, and have low toxicity, The characteristics of low residue can maintain the high quality of agricultural products, so botanical pesticides have a broad market.

近几年来,国内外许多学者调查和研究了一些植物提取物的抗菌、杀菌活性。一些研究表明,植物源抑(杀)菌物质可作用于菌体细胞的多个结构,微生物产生抗性的风险较小。In recent years, many scholars at home and abroad have investigated and studied the antibacterial and bactericidal activities of some plant extracts. Some studies have shown that plant-derived antibacterial (killing) substances can act on multiple structures of bacterial cells, and the risk of microbial resistance is small.

植物源杀菌剂具有作用广谱、无明显的脊椎动物毒性或植物毒性、环境降解迅速且资源丰富、可再生等优点,因此对植物源杀菌剂的开发和应用具有非常广阔的前景。Botanical fungicides have the advantages of broad spectrum of action, no obvious vertebrate toxicity or phytotoxicity, rapid environmental degradation, abundant resources, and renewable, so the development and application of botanical fungicides have very broad prospects.

发明内容Contents of the invention

为了解决现有技术的不足,本发明提供了天名精提取物及其制备方法和应用。In order to solve the deficiencies of the prior art, the present invention provides Tianmingjing extract and its preparation method and application.

本发明的技术方案是:天名精提取物,由天名精的根、茎、叶和/或种子提取后制得。The technical solution of the present invention is: Tianmingjing extract, which is obtained after extracting the roots, stems, leaves and/or seeds of Tianmingjing.

天名精提取物的制备方法,包括以下步骤:步骤一,将干燥的天名精根、茎、叶和/或种子粉碎,加80%~95%的乙醇进行浸提,收集滤液,得天名精粗提物;步骤二,天名精粗提物经乙酸乙酯萃取,即得天名精抗菌提取物。The preparation method of Tianmingjing extract comprises the following steps: step 1, crushing dried Tianmingjing roots, stems, leaves and/or seeds, adding 80% to 95% ethanol for extraction, collecting the filtrate to obtain Tianmingjing The crude extract; step 2, the crude extract of Tianmingjing is extracted with ethyl acetate to obtain the antibacterial extract of Tianmingjing.

本发明的进一步改进包括:Further improvements of the present invention include:

所述的步骤一反复提取多次至浸提液颜色不再变化,合并滤液得提取液,将此提取液浓缩成稀浸膏,得天名精粗提物。The step 1 is repeated for several times until the color of the extract does not change, the filtrates are combined to obtain an extract, and the extract is concentrated into a dilute extract to obtain a crude extract.

所述步骤二中天名精粗提物经乙酸乙酯萃取后酯萃取物经大孔吸附树脂脱去色素,再经乙酸乙酯纯化处理。In the step 2, the crude extract of Tianmingjing is extracted with ethyl acetate, and the ester extract is depigmented with a macroporous adsorption resin, and then purified with ethyl acetate.

本发明进一步提供了天名精提取物在制备防治灰霉病菌、番茄叶霉病菌、番茄早疫病菌、黄瓜枯萎病菌、马铃薯早疫病菌和/或辣椒疫霉病菌药物中的应用。The present invention further provides the application of Tianmingjing extract in the preparation of medicines for preventing and treating Botrytis cinerea, tomato leaf mold, tomato early blight, cucumber wilt, potato early blight and/or capsicum phytophthora.

本发明还提供了含有天名精提取物的杀菌微乳剂的制备方法,在反应釜中,先将天名精提取物,农药助剂溶解于乙酸乙酯溶剂中,在40℃~50℃条件下,高速搅拌的情况下将所得溶剂加入蒸馏水中,恒搅拌1h,即得天名精杀菌微乳剂。The present invention also provides a preparation method of a bactericidal microemulsion containing Tianmingjing extract. In a reaction kettle, first dissolve Tianmingjing extract and pesticide adjuvant in ethyl acetate solvent, and heat Under the condition of high-speed stirring, add the obtained solvent into distilled water, and keep stirring for 1 hour to obtain Tianmingjing bactericidal microemulsion.

按照上述方法制得的含有天名精提取物的杀菌微乳剂。The bactericidal microemulsion containing Tianmingjing extract prepared according to the above method.

含有天名精提取物的杀菌微乳剂,按照分重量百分比包括:天名精提取物1~3份,溶剂1~2份,水3~5份,农药助剂1~2。The bactericidal microemulsion containing Tianmingjing extract comprises: 1-3 parts of Tianmingjing extract, 1-2 parts of solvent, 3-5 parts of water, and 1-2 parts of pesticide adjuvant according to weight percentage.

本发明和现有技术中常用的杀菌剂相比,有如下特点:Compared with the fungicides commonly used in the prior art, the present invention has the following characteristics:

1.对环境安全天名精杀菌剂中的活性化合物是天然存在的物质,来源于自然,在长期的进化过程中已形成了其固有的参与能量与物质循环代谢途径,所以施用与环境中或植物上,无残留,不会引起生物富集:1. Environmental safety The active compounds in Tianmingjing fungicides are naturally occurring substances, which are derived from nature. During the long-term evolution process, they have formed their inherent metabolic pathways to participate in energy and material circulation, so the application is compatible with the environment or On plants, no residues, will not cause bioconcentration:

2.对非靶标生物相对安全;2. Relatively safe to non-target organisms;

3.对植物病原菌的作用机理不同于常规农药,使用后病原菌不易对其产生抗药性,对病原菌对常规杀菌剂的抗药性也有延缓作用。3. The mechanism of action on plant pathogenic bacteria is different from that of conventional pesticides. After use, pathogenic bacteria are not easy to develop resistance to it, and it can also delay the resistance of pathogenic bacteria to conventional fungicides.

本发明的天名精杀菌剂对环境安全,天名精杀菌剂中的活性化合物是天然存在的物质,来源于自然,在长期的进化过程中已形成了其固有的参与能量与物质循环代谢途径,所以施用于环境中或植物上,无残留,不会引起生物富集;对非靶标生物相对安全;对植物病原菌的作用机理不同于常规农药,使用后病原菌不易对其产生抗药性,对病原菌对常规杀菌剂的抗药性也有延缓作用。The Tianmingjing fungicide of the present invention is safe to the environment, and the active compound in the Tianmingjing fungicide is a naturally occurring substance, derived from nature, and has formed its inherent pathway of participating in energy and material cycle metabolism during the long-term evolution process , so when applied in the environment or on plants, there is no residue and will not cause bioaccumulation; it is relatively safe to non-target organisms; the mechanism of action on plant pathogenic bacteria is different from conventional pesticides, and pathogenic bacteria are not easy to develop resistance to it after use. Resistance to conventional fungicides also has a delaying effect.

具体实施方式detailed description

下面结合实施例对本发明做详细说明。The present invention will be described in detail below in conjunction with the embodiments.

实施例1:天名精抗菌活性提取物的制备:Example 1: Preparation of Tianmingjing Antibacterial Active Extract:

取天名精干样100kg,加70%的乙醇回流提取2次,第一次加800kg 70%的乙醇,第二次加600kg 70%的乙醇,过滤,合并提取液,提取液回收乙醇并浓缩至相对密度1.05的稀浸膏,将此稀浸膏用乙酸乙酯萃取得乙酸乙酯相,乙酸乙酯相过D101大孔吸附树脂,先用30%的乙醇洗脱至无色,将此30%乙醇洗脱液弃去,再用85%的乙醇洗脱至无色,收集此85%乙醇洗脱液,回收乙醇并浓缩成相对密度1.25的稠膏,真空干燥,即得含天名精抗菌提取物(按内酯计,质量分数不低于60%)。Take 100kg of Tianming refined dry sample, add 70% ethanol for reflux extraction twice, add 800kg 70% ethanol for the first time, add 600kg 70% ethanol for the second time, filter, combine the extracts, reclaim the ethanol from the extracts and concentrate to Dilute extract with a relative density of 1.05, extract the thin extract with ethyl acetate to obtain an ethyl acetate phase, pass the ethyl acetate phase through D101 macroporous adsorption resin, and first elute with 30% ethanol until it is colorless. The % ethanol eluate was discarded, and then eluted with 85% ethanol until it was colorless, the 85% ethanol eluate was collected, the ethanol was recovered and concentrated into a thick paste with a relative density of 1.25, and dried in vacuum to obtain Tianmingjing Antibacterial extract (according to lactone, the mass fraction is not less than 60%).

实施例2:天名精杀菌微乳剂的制备:Embodiment 2: the preparation of Tianmingjing bactericidal microemulsion:

将天名精抗菌精制提取物2份加入到调整搅拌反应釜中,将农药助剂Termul 50301份用乙酸乙酯2份溶解,在40℃~50℃温度下高速搅拌,搅拌过程中加入去离子水3份,恒温搅拌1h,即得40%天名精杀菌微乳剂。Add 2 parts of Tianmingjing’s antibacterial and refined extract to the adjusted stirring reaction kettle, dissolve 1 part of the pesticide adjuvant Termul 5030 with 2 parts of ethyl acetate, stir at a high speed at a temperature of 40°C to 50°C, and add deionized 3 parts of water, stirred at constant temperature for 1 hour, and 40% Tianmingjing bactericidal microemulsion was obtained.

实施例3:天名精微乳剂抗菌活性测定Embodiment 3: Determination of Antibacterial Activity of Tianming Fine Microemulsion

将实施例2制得的天名精微乳剂0.02mL用熔化的PDA培养基定容至10mL,混匀后倒入培养皿中制备成带菌平板。供试病原菌预先用平板培养5-7天,用灭菌后的打孔器在培养好的菌落上打菌饼(直径为4mm),然后将菌饼倒扣在混药平板中央,毎处理重复3次。设置等量的灭菌水作为对照。接好的菌种平板放入恒温培养箱(25±1℃)培养,用十字交叉法分别测量72h的菌落直径,按以下公式计算抑制率,结果见表1。Dilute 0.02 mL of Tianming fine microemulsion prepared in Example 2 to 10 mL with melted PDA medium, mix well and pour it into a petri dish to prepare a plate with bacteria. Test the pathogenic bacteria with plate culture in advance for 5-7 days, use a sterilized hole puncher to make a bacterium cake (diameter is 4mm) on the bacterium colony that has been cultivated, then buckle the bacterium cake upside down in the center of the mixed medicine flat plate, and repeat each treatment 3 times. Set an equal amount of sterilized water as a control. The inoculated strain plate was placed in a constant temperature incubator (25±1°C) for cultivation, and the colony diameter was measured for 72 hours by the cross method, and the inhibition rate was calculated according to the following formula. The results are shown in Table 1.

菌落生长直径=菌落直径-4Colony growth diameter = colony diameter -4

表1天名精微乳剂抑菌活性Table 1 Antibacterial activity of Tianming microemulsion

注:表中数据为三次重复的平均值,同列数据后不同字母表示数据间差异显著(P<0.05,Duncan新复极差法);“-”表示未检测到抑菌活性。Note: the data in the table is the average value of three repetitions, and different letters after the data in the same column indicate significant differences between the data (P<0.05, Duncan's new multiple range method); "-" indicates that no antibacterial activity was detected.

以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。The basic principles and main features of the present invention and the advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the present invention is not limited by the above-mentioned embodiments, and what described in the above-mentioned embodiments and the description only illustrates the principles of the present invention, and the present invention will also have other functions without departing from the spirit and scope of the present invention. Variations and improvements are possible, which fall within the scope of the claimed invention. The protection scope of the present invention is defined by the appended claims and their equivalents.

Claims (8)

1.天名精提取物,其特征在于,由天名精的根、茎、叶和/或种子提取后制得。1. Tianmingjing extract, which is characterized in that it is prepared after extracting the roots, stems, leaves and/or seeds of Tianmingjing. 2.天名精提取物的制备方法,其特征在于,包括以下步骤:步骤一,将干燥的天名精根、茎、叶和/或种子粉碎,加80%~95%的乙醇进行浸提,收集滤液,得天名精粗提物;步骤二,天名精粗提物经乙酸乙酯萃取,即得天名精抗菌提取物。2. The preparation method of Tianmingjing extract is characterized in that it comprises the following steps: Step 1, the dried Tianmingjing roots, stems, leaves and/or seeds are pulverized, and 80% to 95% of ethanol is added to extract, The filtrate is collected to obtain the crude extract of Tianmingjing; step 2, the crude extract of Tianmingjing is extracted with ethyl acetate, and the antibacterial extract of Tianmingjing is obtained. 3.根据权利要求2所述的天名精提取物的制备方法,其特征在于,所述的步骤一反复提取多次至浸提液颜色不再变化,合并滤液得提取液,将此提取液浓缩成稀浸膏,得天名精粗提物。3. the preparation method of Tianmingjing extract according to claim 2, is characterized in that, described step 1 repeatedly extracts repeatedly to the extract solution color and no longer changes, merges filtrate to obtain extract, and this extract Concentrated into dilute extract, get the name of fine crude extract. 4.根据权利要求2所述的天名精提取物的制备方法,其特征在于,所述步骤二中天名精粗提物经乙酸乙酯萃取后酯萃取物经大孔吸附树脂脱去色素,再经乙酸乙酯纯化处理。4. the preparation method of Tianmingjing extract according to claim 2, is characterized in that, in described step 2, Tianmingjing crude extract extracts ester extract through macroporous adsorption resin to remove pigment after ethyl acetate extraction , and then purified by ethyl acetate. 5.天名精提取物在制备防治灰霉病菌、番茄叶霉病菌、番茄早疫病菌、黄瓜枯萎病菌、马铃薯早疫病菌和/或辣椒疫霉病菌药物中的应用。5. Application of Tianmingjing extract in the preparation of medicines for preventing and treating Botrytis cinerea, tomato leaf mold, tomato early blight, cucumber wilt, potato early blight and/or capsicum phytophthora. 6.含有天名精提取物的杀菌微乳剂的制备方法,其特征在于,在反应釜中,先将天名精提取物,农药助剂溶解于乙酸乙酯溶剂中,在40℃~50℃条件下,高速搅拌的情况下将所得溶剂加入蒸馏水中,恒搅拌1h,即得天名精杀菌微乳剂。6. The preparation method of the bactericidal microemulsion containing the Tianmingjing extract is characterized in that, in the reaction kettle, the Tianmingjing extract and the pesticide adjuvant are dissolved in ethyl acetate solvent and heated at 40°C to 50°C Under the condition of high-speed stirring, add the obtained solvent into distilled water, and keep stirring for 1 hour to obtain Tianmingjing bactericidal microemulsion. 7.含有天名精提取物的杀菌微乳剂,其特征在于,按照权利要求6所述的方法制得。7. The bactericidal microemulsion containing Tianmingjing extract is characterized in that it is prepared according to the method of claim 6. 8.含有天名精提取物的杀菌微乳剂,其特征在于,按照分重量百分比包括:天名精提取物1~3份,溶剂1~2份,水3~5份,农药助剂1~2份。8. The bactericidal microemulsion containing Tianmingjing extract is characterized in that, according to weight percentage, it includes: 1-3 parts of Tianmingjing extract, 1-2 parts of solvent, 3-5 parts of water, and 1-3 parts of pesticide adjuvant 2 servings.
CN201610604491.XA 2016-07-28 2016-07-28 Radix Carpesii extract and its preparation method and application Pending CN106135298A (en)

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CN108911845A (en) * 2018-07-26 2018-11-30 广西田阳县创新农业综合开发有限公司 A kind of mango Special slow release fertilizer and preparation method thereof

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