CN115226728B - Preparation method and application of radix seu herba Gei aleppici alkaloid extract - Google Patents
Preparation method and application of radix seu herba Gei aleppici alkaloid extract Download PDFInfo
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- CN115226728B CN115226728B CN202210467456.3A CN202210467456A CN115226728B CN 115226728 B CN115226728 B CN 115226728B CN 202210467456 A CN202210467456 A CN 202210467456A CN 115226728 B CN115226728 B CN 115226728B
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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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G5/00—Alkaloids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention relates to the field of alkaloid extraction, in particular to a preparation method and application of active substances for inhibiting plant pathogenic bacteria by extracting root tuber of radix polygoni multiflori. The preparation method comprises the following steps of S1: weighing the large flower land and the small root tuber, drying and crushing to obtain small dried large flower land and small root tuber particles; s2: taking the small particles of the root tuber of the radix sophorae falvescentis as raw materials, adding an acidic solution for leaching, filtering, and collecting filter residues and filtrate A; s3: and (3) regulating the pH value of the filtrate A to about 9 by using an alkaline solution, then adding an extractant for extraction to obtain a water phase and an extract B, and washing and concentrating the extract to obtain the radix seu herba Gei aleppici alkaloid extract. The radix sophorae flavescentis alkaloid extract prepared by the method has good effect on preventing and treating citrus canker.
Description
Technical Field
The invention relates to the field of alkaloid extraction, in particular to a preparation method and application of active substances for inhibiting plant pathogenic bacteria by extracting root tuber of radix polygoni multiflori.
Background
At present, chemical pesticides are mainly adopted for citrus canker, and due to long-term use of the chemical pesticides, germs generate drug resistance, and the use of the chemical pesticides can remain in soil and even enter water body seeds, so that environmental pollution is caused. Research in recent decades has shown that secondary metabolites in plants have very good biological activity and even become efficient, natural, easily degradable, residue-free biopesticides.
Deng Yecheng it has been found that Guangxi di extract has a strong inhibitory effect on brown spot germ, black spot germ, citrus scab germ and citrus canker germ (Deng Yecheng Li Jierong Gao Chengwei Yang Linlin. Guangxi di extract and its compound antibacterial activity [ J ]. Plant protection, 2006, 32 (4): 43-46.), but the plant material for this study is Guangxi di-intolerant, and methanol extract is used, which contains many inactive ingredients and impurities, resulting in a small proportion of effective active ingredients, leading to poor effect of the extract. According to previous studies, the active ingredients of stephania sinica Diels for inhibiting pathogenic bacteria are mainly secondary metabolites-alkaloids contained in the plants. The extract obtained by the exclusive method suitable for extracting and refining the alkaloids has better pathogenic bacteria inhibiting effect.
The large flower field can not be distributed in Yunnan, sichuan and other places in China, is a stephania plant, is a new species discovered by scientific research workers Luo Xianrui in 1988 in China, and is characterized in that the flower is very large, so the large flower field can not be used. According to the research, the root tuber of the large-flowered rehmannia has high alkaloid content, and the alkaloid extract of the root tuber has strong capability of inhibiting citrus canker. Therefore, the invention provides the preparation method of the radix aconiti kusnezoffii root alkaloid extract capable of effectively inhibiting the citrus canker, the method is simple to operate and low in cost, and the obtained alkaloid extract is strong in activity and has development prospect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an extraction method of the radix rehmanniae praeparata alkaloid, so as to at least achieve the advantages of simple operation and low cost.
The aim of the invention is realized by the following technical scheme:
the preparation method of the root tuber alkaloid extract of the radix stephaniae tetrandrae is characterized by comprising the following steps of:
s1: weighing the large flower land and the small root tuber, drying and crushing to obtain small dried large flower land and small root tuber particles;
s2: taking the small particles of the root tuber of the radix sophorae falvescentis as raw materials, adding an acidic solution for leaching, filtering, and collecting filter residues and filtrate;
s3: and (3) regulating the pH value of the filtrate to 8.5-9.5 by using an alkaline solution, then adding an extractant for extraction to obtain a water phase and an extract, and washing and concentrating the extract to obtain the radix seu herba Desmodii Styracifolii alkaloid extract.
Further, the dosage ratio of the small particle of the large flower soil free root tuber, the oxalic acid solution and the extractant is 1kg:7-16L:10-30L.
Further, in step S1, the temperature of the drying is 50-60 ℃; the crushed grain size is less than 2.5mm.
Further, in step S2, the acidic solution includes 2-10% oxalic acid solution or hydrochloric acid solution.
Further, in step S2, the number of times of leaching is two or more.
Further, in step S3, the alkaline solution includes lime milk or ammonia water.
Further, in step S3, the extractant includes diethyl ether, chloroform and dichloromethane or methyl tert-butyl ether.
Further, in step S3, the number of times of the extraction is two or more.
Another object of the invention is the use of said root tuber alkaloid extract of the large-flowered ground in the inhibition of plant pathogenic bacteria.
Further, the plant pathogenic bacteria are citrus canker bacteria.
Further, the specific application method of the root tuber alkaloid extract of the radix stephaniae tetrandrae comprises the following steps: mixing the alkaloid extract of radix Stephaniae Dillenii with emulsifying agent Tween 80 and water to obtain 150-450ppm medicinal liquid.
The beneficial effects of the invention are as follows:
1. the plant raw material used in the invention, namely the large flower field, can not be interplanted under citrus forests, and the resources are rich; the extraction method of the active component alkaloid is simple to operate, the yield of the total alkaloid extract is between 3% and 5%, and the simple production and the large-scale industrial production of the orchard are easy.
2. The acid and the alkali used in the invention are relatively weak acid and alkali, have good tolerance to the extraction container and are environment-friendly.
3. The medicine formula prepared from the alkaloid extract has good effect on preventing and treating citrus canker, and the medicine is natural in source, easy to degrade, free of residues and environment-friendly.
Description of the embodiments
The technical scheme of the present invention is described in further detail below, but the scope of the present invention is not limited to the following.
Examples
Weighing 2 kg of large-flower-land-free tuberous roots, drying at 50-60 ℃, crushing, sieving with a 10-mesh sieve to obtain small particles of the large-flower-land-free tuberous roots, pouring into a container, adding 8L of 0.1 mol/L oxalic acid solution, stirring at regular time, soaking for 12 hours, filtering, and collecting filter residues and filtrate 1; mixing the obtained filter residue with 0.1 mol/L oxalic acid solution for 6L again, regularly stirring, soaking for 6 hours, and filtering to obtain filtrate 2; mixing filtrate 1 and filtrate 2, regulating pH of the filtrate to about 9 with lime cream, extracting alkali water solution with 10L methyl tert-butyl ether, separating, and collecting methyl tert-butyl ether extract; then extracting the alkali water solution with 10L of methyl tertiary butyl ether again, separating the solution, collecting methyl tertiary butyl ether extract, combining the two methyl tertiary butyl ether extracts, then washing the methyl tertiary butyl ether extract with 10L of distilled water for 2 times, and concentrating the methyl tertiary butyl ether extract to obtain 64 g of radix seu herba Geranii total alkaloids extract with an extraction rate of 3.2%. Then weighing 1.5 g of the root tuber alkaloid extract of the radix sophorae falvescentis, preparing into powder, dispersing in 8.5 liters of water, adding 1.5 liters of tween 80, and stirring to prepare an emulsion, namely the liquid medicine of 150ppm of the root tuber alkaloid extract of the radix sophorae falvescentis.
Comparative example 1
Weighing 2 kg of Guangxi di-containing tuberous roots, drying at 50-60 ℃, crushing, sieving with a 10-mesh sieve to obtain dried Guangxi di-containing tuberous root small particles, pouring into a container, adding 8L of 0.1 mol/L oxalic acid solution, stirring at regular time, soaking for 12 hours, filtering, and collecting filter residues and filtrate 1; mixing the obtained filter residue with 0.1 mol/L oxalic acid solution for 6L again, regularly stirring, soaking for 6 hours, and filtering to obtain filtrate 2; mixing filtrate 1 and filtrate 2, regulating pH of the filtrate to about 9 with lime cream, extracting alkali water solution with 10L methyl tert-butyl ether, separating, and collecting methyl tert-butyl ether extract; then extracting the alkali water solution with 10L of methyl tertiary butyl ether again, separating the solution, collecting methyl tertiary butyl ether extract, combining the two methyl tertiary butyl ether extracts, then washing the methyl tertiary butyl ether extract with 10L of distilled water for 2 times, and concentrating the methyl tertiary butyl ether extract to obtain 61 g of radix codonopsis Guangxi total alkaloids extract with the extraction rate of 3.05 percent. Then 1.5 g of the root tuber alkaloid extract of the radix sophorae tonkinensis is prepared into powder, dispersed in 8.5 liters of water, then 1.5 liters of tween 80 is added, and stirred to prepare an emulsion, namely the liquid medicine of 150ppm of the root tuber alkaloid extract of the radix sophorae tonkinensis.
Examples
100 square meters of citrus forest 2 blocks infected with citrus canker are selected, and 10 kg of each of the root tuber alkaloid extract 150pp of the large-flower land of example 1 and the liquid medicine 150ppm of comparative example 1 is used as a control medicament, and are fully sprayed on citrus leaves and branches respectively in the afternoon period of a cloudy day. And checking the control effect after 10 days.
After 10 days, checking the control effect of the liquid medicine with 150ppm of the root tuber alkaloid extract of the large-flowered land: 89.2% of the citrus canker leaves are prevented and treated.
After 10 days, checking the control effect of the liquid medicine of 150ppm of the Guangxi di-sodium root tuber alkaloid extract: 72.6% of the citrus canker leaves are prevented and treated.
Examples
The preparation method comprises the steps of selecting 5 citrus forests with 20 square meters infected with citrus canker, taking 2 kg of each of the root tuber alkaloid extracts of 150ppm, 250ppm, 350ppm, 450ppm and 550ppm of the large-flowered soil of example 1 as a control medicament, fully spraying the medicinal liquid on citrus leaves and tips respectively in the afternoon period of a cloudy day, and checking the control effect after 10 days.
After 10 days, checking the control effect of the liquid medicine with 150ppm of the root tuber alkaloid extract of the large-flowered land: 81% of the leaves infected with citrus canker are prevented and treated.
After 10 days, checking the control effect of the liquid medicine of 150ppm of the Guangxi di-sodium root tuber alkaloid extract: 64% of the leaves infected with citrus canker are prevented and treated. After 10 days, checking the control effect of the medicinal liquid with 250ppm of the root tuber alkaloid extract of Guangxi di: 72% of the citrus canker leaves are prevented and treated.
After 10 days, checking the control effect of the liquid medicine with 350ppm of the root tuber alkaloid extract of Guangxi di: 80% of the citrus canker leaves are prevented and treated.
After 10 days, checking the control effect of the liquid medicine with 450ppm of the Guangxi di-sodium root tuber alkaloid extract: 86% of the citrus canker leaves are prevented and treated.
After 10 days, checking the control effect of the medicinal liquid with 550ppm of the root tuber alkaloid extract of Guangxi di: 91% of the citrus canker leaves infected are prevented and treated.
The foregoing is merely a preferred embodiment of the invention, and it is to be understood that the invention is not limited to the form disclosed herein but is not to be construed as excluding other embodiments, but is capable of numerous other combinations, modifications and environments and is capable of modifications within the scope of the inventive concept, either as taught or as a matter of routine skill or knowledge in the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.
Claims (5)
1. The application of the root tuber alkaloid extract of the large-flower land for inhibiting citrus canker is characterized in that the preparation method of the root tuber alkaloid extract of the large-flower land comprises the following steps:
s1: weighing the large flower land and the small root tuber, drying and crushing to obtain small dried large flower land and small root tuber particles;
s2: taking the small particles of the root tuber of the radix sophorae falvescentis as raw materials, adding an acidic solution for leaching, filtering, and collecting filter residues and filtrate A;
s3: regulating the pH value of the filtrate to 8.5-9.5 by using an alkaline solution, then adding an extractant for extraction to obtain a water phase and an extract B, and washing and concentrating the extract to obtain the radix seu herba Desmodii Styracifolii alkaloid extract;
the dosage ratio of the large-flower-land-free tuberous root small particles, the acid solution and the extractant is 1kg:7-36L:10-30L;
in the step S2, the acid solution is 2-10% oxalic acid solution or hydrochloric acid solution;
in the step S3, the extractant is diethyl ether, chloroform and methylene dichloride or methyl tertiary butyl ether.
2. The use according to claim 1, characterized in that: in the step S1, the temperature of the drying is 50-60 ℃; the crushed grain size is less than 2.5mm.
3. The use according to claim 1, characterized in that: in step S2, the number of times of leaching is two or more.
4. The use according to claim 1, characterized in that: in step S3, the alkaline solution includes lime milk or ammonia water.
5. The use according to claim 1, characterized in that: in step S3, the number of times of extraction is two or more.
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| CN202210467456.3A CN115226728B (en) | 2022-04-29 | 2022-04-29 | Preparation method and application of radix seu herba Gei aleppici alkaloid extract |
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| CN115226728B true CN115226728B (en) | 2023-07-25 |
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| CN1613851A (en) * | 2004-09-08 | 2005-05-11 | 华南农业大学 | Extracting method for natural alkali of isoquinoline |
| CN102670720A (en) * | 2011-03-16 | 2012-09-19 | 朱毅 | Stephania hainanensis total alkaloid extract and preparation method thereof |
| CN102250001A (en) * | 2011-05-18 | 2011-11-23 | 成都大学 | Method for rapidly preparing denudatine from long-handle aconitum szechenyianum gay plant |
| CN102631414B (en) * | 2012-04-25 | 2013-09-25 | 成都煜泉绿健科技有限公司 | SepHaniadelavayi Diels total alkaloid extraction and purification technology |
| CN106176873B (en) * | 2016-08-10 | 2020-04-21 | 南阳师范学院 | Capsella bursa-pastoris total alkaloid extract and preparation method and application thereof |
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