CN110447643B - Berberine smoke agent and application thereof - Google Patents
Berberine smoke agent and application thereof Download PDFInfo
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- CN110447643B CN110447643B CN201910831636.3A CN201910831636A CN110447643B CN 110447643 B CN110447643 B CN 110447643B CN 201910831636 A CN201910831636 A CN 201910831636A CN 110447643 B CN110447643 B CN 110447643B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, 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
- A01N25/18—Vapour or smoke emitting compositions with delayed or sustained release
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, 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
- A01N25/22—Biocides, 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 ingredients stabilising the active ingredients
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- General Health & Medical Sciences (AREA)
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- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
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- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
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Abstract
本发明公开了一种小檗碱烟剂及其应用。该小檗碱烟剂的制备方法包括以下步骤：(1)用水或乙醇从黄柏或黄连中提取小檗碱，过滤，浓缩，得到含小檗碱的植物提取液；(2)用含小檗碱的植物提取液浸泡烟丝2‑6小时，以烟丝吸附小檗碱，得烟丝小檗碱；(3)将烟丝小檗碱60‑70℃烘干或晾干，粉碎，过60目筛；(4)将过筛后的烟丝小檗碱与载体混合均匀，再向其中加入助燃剂、发烟剂、燃料混合，粉碎，过筛，得到小檗碱烟剂。该烟剂可用于大棚作物灰霉病、白粉病等病虫害防治，烟剂高效、省时、省工、施用方便，不使用机械等设备，无兑水等繁琐步骤，特别是对缺水的地区更具有特殊意义。The invention discloses a berberine nicotine and its application. The preparation method of the berberine nicotinant comprises the following steps: (1) extracting berberine from Cork or Coptis chinensis with water or ethanol, filtering and concentrating to obtain a berberine-containing plant extract; (2) using a berberine-containing plant extract Soak the cut tobacco in the alkali plant extract for 2-6 hours, absorb the berberine with the cut tobacco, and obtain the cut tobacco berberine; (3) dry or air-dry the cut tobacco berberine at 60-70°C, pulverize, and pass through a 60-mesh sieve; (4) Mixing the sieved cut tobacco berberine with the carrier uniformly, then adding a combustion accelerant, a smoke generating agent, and a fuel to it, mixing, pulverizing, and sieving to obtain a berberine nicotine. The smoke agent can be used for the prevention and control of botrytis, powdery mildew and other diseases and insect pests of greenhouse crops. The smoke agent is efficient, time-saving, labor-saving, convenient to apply, does not use machinery and other equipment, and has no cumbersome steps such as adding water, especially for areas lacking water. more special.
Description
Technical Field
The invention relates to a berberine smoke agent and application thereof, wherein the smoke agent can be used for preventing and treating diseases and insect pests such as gray mold, powdery mildew and the like of greenhouse crops.
Background
Berberine, also known as berberine, is a quaternary ammonium alkaloid C separated from Coptidis rhizoma, cortex Phellodendri, and radix Berberidis20H18NO4Is the main antibacterial active ingredient of the plants, is yellow needle-shaped crystal and is bitter in taste. The distribution is wide in the plant kingdom, and about 4 plants in 10 genera have the existence of the product. The berberine can effectively inhibit fungi such as gray mold, powdery mildew, leaf mold and the like, and bacteria such as pseudomonas syringae and xanthomonas. At present, the berberine registration mainly comprises wettable powder and soluble solutionAgents and aqueous agents. In the process of planting vegetables in the greenhouse, once gray mold, powdery mildew and the like occur, the damp environment is closed to promote the epidemic of the diseases in the greenhouse. At present, spray application is generally adopted for preventing and treating diseases such as gray mold of a greenhouse, the air humidity in the greenhouse can be directly increased by spraying the spray, the germination speed and the invasion chance of germ spores can be increased by spraying water on the surfaces of vegetables, and the disease occurrence is promoted. The application mode of the smoke can reduce the humidity in the greenhouse or on the surface of the plant, and the disease aggravation caused by the increase of the air humidity is avoided. Meanwhile, the smoke agent is efficient, time-saving, labor-saving and convenient to apply, does not use equipment such as machinery and the like, does not have complicated steps of adding water, and has special practical significance particularly for water-deficient areas.
Aerosol formulations, which are common on the market, use mainly chemical components, such as: chlorothalonil, dichlorvos, isoprocarb and the like. Preparing smoke agent by plant source pesticide such as: patent document 1(CN 106508978A, application No. 2016109265810) discloses a smoke agent for preventing gray mold prepared from cassia seed, xanthium sibiricum, verbena, cinnamon, eupatorium, bamboo charcoal powder, ammonium nitrate, ammonium chloride, talcum powder and surfactant; patent document 2(CN 106490025a, application No. 2016109265149) prepares smoke agent from radix Aconiti, herba Selaginellae Doederleinii, herba Schizophragmatis Integrifolii, herba Artemisiae Annuae, rhizoma et radix Veratri, bamboo charcoal powder, ammonium nitrate, ammonium chloride, pulvis Talci, and surfactant; patent document 3(CN1260120A, application No. CN99100078.1) directly crushes and screens tobacco leaves and castor oil residues, adds an oxidant, a combustion improver and the like to press the materials into blocks, twists with fire to induce fire and smoke, and is mainly used for preventing and treating vegetable aphids such as greenhouse cucumbers and also controlling red spiders and whiteflies; patent document 4(CN 106490036a, application No. 2016109265806) is prepared from giant knotweed rhizome, rhubarb, Chinese yam, humifuse euphorbia herb, kadsura longepedunculata, bamboo charcoal powder, ammonium nitrate, ammonium chloride, talcum powder and surfactant; patent document 5(CN108294021A, application number: 201810100735X) has sophora flavescens-nicotine emulsifiable concentrate as main agent, and sodium bicarbonate composition and modified sodium bicarbonate as auxiliary agent; wherein the sodium bicarbonate composition comprises soybean oil residue, soybean meal powder, and sodium bicarbonate; the modified sodium bicarbonate is amino-modified mesoporous silica-loaded sodium bicarbonate.
The berberine has melting point of 85-86 deg.C, boiling point of 354.2 deg.C (760mmHg), and flash point of 151.8 deg.C. The low melting point determines that the smoke agent prepared by the smoke agent is easy to be burnt and decomposed. The technology and method for preparing the berberine in the smoke agent are not found, and the literature that the berberine is infiltrated and absorbed by the tobacco shreds and is used as a combustion improver and a fire retardant is not found.
Based on the prior art, the invention is funded by a Beijing education committee scientific research-Beijing natural science fund combined plan project KZ201911417049, Beijing combined university personnel forcible school optimization plan and a Hebei province key research and development plan project.
Disclosure of Invention
The invention aims to provide a berberine smoke agent which can be used for preventing and treating diseases and insect pests such as gray mold, powdery mildew and the like of greenhouse crops.
The invention also aims to provide application of the berberine smoke agent.
In order to achieve the purpose, the invention adopts the following technical scheme:
a berberine smoke agent is prepared by the following steps:
(1) extracting berberine from cortex Phellodendri or Coptidis rhizoma with water or ethanol, filtering, and concentrating to obtain plant extractive solution containing berberine, wherein the berberine content is 20-70 wt%;
(2) soaking tobacco shreds in berberine-containing plant extractive solution at room temperature for 2-6 hr, and adsorbing berberine with tobacco shreds to obtain tobacco shreds berberine;
(3) drying or air drying berberine in tobacco at 60-70 deg.C, pulverizing, and sieving with 60 mesh sieve;
(4) mixing the sieved berberine in tobacco shred with carrier, adding combustion improver, smoke agent and fuel, mixing, pulverizing, and sieving with 60 mesh sieve to obtain berberine smoke agent.
The invention soaks the tobacco shred with the berberine-containing extract, and the tobacco shred absorbs a great amount of berberine, the tobacco shred absorbing berberine can be used as an adsorbent, a smoke agent and a flame retardant material, and the nicotine component in the tobacco shred can also be used for disinsection. The smoke agent fuel is mainly made of wood dust, coal powder, charcoal powder, starch, cane sugar and the like, and the invention adopts active carbon or sweet wormwood herb as fuel. The activated carbon is selected as the fuel, so that the combustion effect is achieved, dust particles can be adsorbed, and the emission of dust such as pm2.5 is reduced. The carrier is sodium lignosulphonate, diatomite or bentonite; the combustion improver is aluminum nitrate, potassium chlorate and potassium permanganate; the fuming agent is ammonium chloride or artemisia annua.
Preferably, in the step (2), the mass ratio of the berberine-containing plant extract to tobacco shreds is 1-10: 1.
In the step (4), the mixing ratio is as follows according to the weight percentage: 20-25% of cut tobacco berberine, 8-30% of carrier, 5-20% of fuel, 40-60% of combustion improver and 5-15% of smoke agent.
An application of berberine smoke agent in preventing and treating diseases and pests of greenhouse crops such as gray mold and powdery mildew is disclosed, wherein the smoke agent is ignited at evening, and the greenhouse is sealed for 8-12 hours.
The invention has the advantages that:
because of the low melting point of berberine, it is the focus of the present invention to prevent berberine from being carbonized (charred, burnt), which is avoided by the following 3 techniques. (1) Extracting berberine by a solvent to prepare an extracting solution, wherein multiple components in the extracting solution avoid direct exposure of the berberine; (2) the extracting solution is used for infiltrating the tobacco shreds, so that the berberine is adsorbed on the tobacco shreds, and the tobacco shreds not only adsorb, but also have combustion supporting and flame retarding effects; (3) mixing the cut tobacco berberine with the carrier, and further wrapping the berberine. The preparation method can effectively prevent the berberine from being carbonized when being prepared into the smoke agent.
The berberine smoke agent can be used for preventing and treating diseases and pests such as gray mold, powdery mildew and the like of greenhouse crops, is efficient, time-saving, labor-saving and convenient to apply, does not use equipment such as machinery and the like, does not have complicated steps such as water adding and the like, and particularly has special significance for water-deficient areas. The preparation method of the berberine smoke agent has simple and convenient process and is suitable for industrial production and application.
The berberine smoke agent of the invention meets the burning test standard: easy ignition, no open fire, dense smoke, impact force, no fuel injection, uninterrupted combustion and combustion time longer than 1 minute.
Detailed Description
The present invention is further illustrated by the following specific examples, but the present invention is not limited to the contents of the following examples.
Example 1
Weighing 200g of coptis chinensis, crushing, adding 800mL of water, extracting at 70 ℃ for 1.5 hours, filtering, adding 800mL of water into filter residues, continuing extracting for 1 hour, combining filtrates, filtering, concentrating under reduced pressure, and adding water to fix the volume of berberine to 56%. Mixing the above extractive solution with 25g tobacco shred, soaking for 4 hr, drying at 60 deg.C for 12 hr, pulverizing, and sieving with 60 mesh sieve to obtain tobacco shred berberine. Taking 20g of tobacco shred berberine, mixing with 10g of sodium lignosulphonate uniformly, adding 10g of ammonium chloride and 10g of sweet wormwood (crushed) in sequence, mixing, and adding 50g of aluminum nitrate. Pulverizing, and sieving with 60 mesh sieve to obtain berberine cigarette product.
Example 2
Weighing 200g of phellodendron, crushing, adding 800mL of 50% ethanol, extracting at 70 ℃ for 1.5 hours, filtering, adding 800mL of 50% ethanol into filter residues, continuing extracting for 1 hour, combining filtrates, filtering, concentrating under reduced pressure, and adding water to fix the berberine concentration to 32%. Mixing the above extractive solution with 25g tobacco shred, soaking for 5 hr, drying at 60 deg.C for 12 hr, pulverizing, and sieving with 60 mesh sieve to obtain tobacco shred berberine. Taking 20g of tobacco shred berberine, mixing with 15g of woody bentonite uniformly, adding 10g of ammonium chloride and 15g of activated carbon (crushed) in sequence, mixing, and adding 40g of potassium chlorate. Crushing, and sieving with a 60-mesh sieve to obtain the product.
Example 3
Weighing 200g of coptis chinensis, crushing, adding 800mL of 60% ethanol, extracting at 70 ℃ for 1.5 hours, filtering, adding 800mL of 60% ethanol into filter residues, continuing extracting for 1 hour, combining filtrates, filtering, concentrating under reduced pressure, and adding water to fix the berberine concentration to 45%. Mixing the above extractive solution with 30g tobacco shred, soaking for 4 hr, drying at 60 deg.C for 12 hr, pulverizing, and sieving with 60 mesh sieve to obtain tobacco shred berberine. Taking 20g of tobacco shred berberine, mixing with 30g of woody diatomite uniformly, then adding 15g of artemisia annua and 20g of activated carbon (crushing) in sequence, mixing, and adding 45g of potassium permanganate. Pulverizing, and sieving with 60 mesh sieve to obtain berberine cigarette product.
Example 4
Weighing 200g of coptis chinensis, crushing, adding 800mL of 35% ethanol, extracting at 70 ℃ for 1.5 hours, filtering, adding 800mL of 35% ethanol into filter residues, continuing extracting for 1 hour, combining filtrates, filtering, concentrating under reduced pressure, and adding water to fix the berberine concentration to 66%. Mixing the above extractive solution with 40g tobacco shred, soaking for 4 hr, drying at 60 deg.C for 12 hr, pulverizing, and sieving with 60 mesh sieve to obtain tobacco shred berberine. Taking 20g of tobacco shred berberine, mixing with 30g of woody bentonite uniformly, adding 12g of ammonium chloride and 15g of activated carbon (crushing) in sequence, mixing, and adding 50g of aluminum nitrate. Pulverizing, and sieving with 60 mesh sieve to obtain berberine cigarette product.
Example 5
Weighing 200g of coptis chinensis, crushing, adding 800mL of 75% ethanol, extracting at 70 ℃ for 1.5 hours, filtering, adding 800mL of 75% ethanol into filter residues, continuing extracting for 1 hour, combining filtrates, filtering, concentrating under reduced pressure, and adding water to fix the berberine concentration to 40%. Mixing the above extractive solution with 50g tobacco shred, soaking for 6 hr, drying at 60 deg.C for 12 hr, pulverizing, and sieving with 60 mesh sieve to obtain tobacco shred berberine. Taking 20g of tobacco shred berberine, mixing with 28g of lignin sodium sulfonate uniformly, then adding 13g of artemisia annua and 8g of active carbon (crushing) in sequence, mixing, and adding 50g of potassium permanganate. Pulverizing, and sieving with 60 mesh sieve to obtain berberine cigarette product.
Example 6
Weighing 200g of phellodendron, crushing, adding 800mL of 25% ethanol, extracting at 70 ℃ for 1.5 hours, filtering, adding 800mL of 25% ethanol into filter residues, continuing extracting for 1 hour, combining filtrates, filtering, concentrating under reduced pressure, and adding water to fix the berberine concentration to 35%. Mixing the above extractive solution with 30g tobacco shred, soaking for 6 hr, drying at 60 deg.C for 12 hr, pulverizing, and sieving with 60 mesh sieve to obtain tobacco shred berberine. Taking 20g of tobacco shred berberine, mixing with 28g of woody diatomite uniformly, then adding 15g of artemisia annua and 13g of activated carbon (crushing) in sequence, mixing, and adding 50g of potassium permanganate. Pulverizing, and sieving with 60 mesh sieve to obtain berberine cigarette product.
Example 7
The test was carried out in the tomato plantation base of Koelreuteria paniculata, Shijiazhuang, to test its efficacy against the gray mold of tomato. Totally 5 medicament treatments are set, namely 3 berberine smoke agents prepared in the embodiments 1, 3 and 5 of the invention respectively, 800 times of solution of 10 percent berberine wettable powder is used as a positive control, and water is used as a blank Control (CK). 1 greenhouse was used as 1 test cell, and 2 replicates were used. The cells adopt a completely random arrangement. Respectively carrying out medicament treatment on 6 days in 5 months and 20 days in 5 months in 2018, igniting or spraying the smoke agent for 2 times, wherein the smoke agent is sprayed on the ground at 7 days in the evening: 00 ignition, next day 8: 00 air is discharged. And 5, 25 days in 5 months, investigating 5 points of east, west, south, north and middle of each greenhouse with leaves, investigating 100 leaves for each point, grading diseases according to disease conditions, and recording the damage degree of diseases at each level. Level 0: no disease spots on the leaves; level 1: 1-2 scabs are formed on each leaf; and 3, level: 3-4 scabs are formed on each leaf; and 5, stage: each blade is provided with 5-6 scabs; and 7, stage: 7-10 scabs are arranged on each blade, or part of scabs are connected to occupy about 1/5 leaf area, 9 grades: more than 10 scabs exist on each leaf, or the area of the connected scabs occupying more than 1/4, and the drug effect calculation method is as follows.
Table 1 shows the results of berberine smoke-curing agent for tomato gray mold. The result shows that the berberine smoke agent has better prevention and treatment effect on tomato botrytis cinerea, has no phytotoxicity and has no adverse effect on beneficial organisms. The control effect of each embodiment of the smoke agent on the tomato gray mold is higher than that of the berberine wettable powder with the concentration of 10 percent.
TABLE 1 results of berberine smoke-control of tomato gray mold
| Treatment of | Dilution factor | Index of disease condition | Average control effect |
| CK | Water (W) | 37.64 | - |
| 10% berberine wettable powder | 800 | 12.67 | 67.32 |
| Example 1 | -- | 8.55 | 78.62 |
| Example 3 | -- | 10.33 | 72.35 |
| Example 5 | -- | 8.01 | 79.29 |
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