CN103222469B - Method for producing sophocarpidine water aqua by using enzymolysis method - Google Patents
Method for producing sophocarpidine water aqua by using enzymolysis method Download PDFInfo
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- CN103222469B CN103222469B CN201310181936.4A CN201310181936A CN103222469B CN 103222469 B CN103222469 B CN 103222469B CN 201310181936 A CN201310181936 A CN 201310181936A CN 103222469 B CN103222469 B CN 103222469B
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Abstract
The invention discloses a method for producing sophocarpidine water aqua by using an enzymolysis method. The method comprises the following steps of: carrying out enzymolysis on crushed sophocarpidine raw materials by using a composite bio-enzyme; then extracting, filtering and concentrating an enzymatic feed liquid subjected to the enzymolysis to obtain a sophocarpidine concentrated solution; and then compounding the obtained sophocarpidine concentrated solution and other phytoextraction intermediates, stabilizing agents and surfactants to obtain the sophocarpidine water aqua. By using the method, active ingredients in the raw materials can be high extracted with a high rate; the sophocarpidine water aqua prepared by using the method disclosed by the invention has high insecticidal performance and high storage stability, is convenient to store and use; and a botanical pesticide of the sophocarpidine water aqua has the characteristics of low toxicity to a human body, no pesticide residue, no influence on environments, no direct killing effect on natural enemies of pests and is capable of satisfying the requirements on environmental protection, ecological balance keeping and uncontaminated production.
Description
Technical field
The present invention relates to a kind of production method of agriculture medicament, be specifically related to a kind of method that uses enzymatic isolation method to produce aqueous matrine solution.
Background technology
At present, the insecticide overwhelming majority of the existing pesticide species of China is organic phosphor, carbamate, pyrethroid pesticide, although drug effect is higher than the drug effect of botanical pesticide, along with the raising of people's living standard, the characteristic of its high toxicity, high residue cannot adapt to the requirement to food.Extracting botanical biological pesticide has become at present feasible mode, its hypotoxicity, noresidue, to environment without influence characteristic, be just applicable to the needs of current social development.
Since China's exploitation thing agricultural chemicals, the control efficiency of botanical pesticide is not high, and lethality is that 85% left and right, storage at normal temperature stability are bad, and above 2 become the bottleneck that affects botanical pesticide development, hindered greatly the application and development of botanical pesticide.
There is abundant plant resources in China, has the multiple plant variety that can be used for making botanical pesticide, the rhizome of these plants flower, fruit, seed etc. is refined to processing and can be made into vegetable insecticide.There are nicotine, matrine, nimbin, toosendanin, Tong punt-pole element, different goat's horn to turn round glucoside, Tea Saponin, rotenone, pyrethrins, plants essential oil and genetically modified plants (seed) etc. for the composition of making botanical pesticide.Active insecticidal components contained in these plant corpuss is different, widely different between different plants.
The preparation method of botanical pesticide mainly contains: directly extract (1): the plant large for plant harvest yield, active constituent content is high, its active ingredient is active strong and be difficult to artificial syntheticly, can directly plant itself or its extract be processed into agricultural chemicals commodity.(2) total man's work biomimetic synthesis: for plant corpus intensive amount is very micro-but the compound that biologically active is higher and structure comparatively simply can be manually synthetic adopts the synthetic mode of full artificial bionic to develop.(3) modify synthetic method: for the active component that content high activity is low or toxicity is high in plant, after simple modification, can significantly improve activity or fall hypotoxic, and be manually difficult to synthetic or the too high compound of synthetic cost, adopt the synthetic method of modification to carry out product development.(4) directed synthetic method: for containing high activity material but compound is difficult to again artificial synthetic, and plant corpus itself is difficult to be obtained or is difficult to the floristics of planting or biological harvest yield is little, can utilize biotechnology (cell culture technology, Organ culture techniques etc.) to carry out the directed active substance of producing of biosynthesis and after extracting, be processed into preparation use.(5) template synthetic method: study its structure-activity relationship after separating identified activity composition, obtain ideal structure as the higher compound of template synthesizing activity, develop novel agrochemical.(6) composite: Chinese medicine compound prescription is the main clinical situation that the traditional Chinese medical science is cured the disease, after drug matching, can make medicament produce obvious synergistic effect or produce new active ingredient, equally, botanical pesticide is carried out to composite its control efficiency to nuisance that also can improve.
Because matrine has larger raw material sources and good insecticidal effect, and have on human body hypotoxicity, noresidue, on environment without features such as impacts, comparatively extensive for research and the application of matrine at present, but the insecticide of the production technology gained of existing matrine vegetable insecticide, its insecticidal activity is lower, the storage at normal temperature stability of medicament is bad, and not high for the extraction efficiency of matrine active ingredient in raw material in existing technique, directly limit extensive use and the High-efficient Production of matrine vegetable insecticide.So, need at present a kind of can high efficiency extraction matrine active ingredient, matrine medicament has higher insecticidal properties and the matrine water agent and process for producing same of bin stability preferably.
Summary of the invention
The technical issues that need to address of the present invention are just to overcome the defect of prior art, a kind of method that uses enzymatic isolation method to produce aqueous matrine solution is provided, its utilization has bioactive enzyme and carrys out enzymolysis matrine raw material, active ingredient in matrine can be dissolved in extraction solvent completely, reach good extraction effect; And the aqueous matrine solution that the method makes has higher insecticidal properties and good bin stability, on human body hypotoxicity, noresidue, on environment without impact, can meet market and social demand.
For addressing the above problem, the present invention adopts technical scheme to be: a kind of method that uses enzymatic isolation method to produce aqueous matrine solution, the method is first used compound biological enzyme to carry out enzymolysis the matrine raw material after pulverizing, then after the enzymolysis feed liquid obtaining after enzymolysis being extracted, filter, being concentrated, obtain matrine concentrate, then will after gained matrine concentrate and other plant extract intermediate, stabilizing agent and surfactant compound, obtain described aqueous matrine solution.
In order to realize the production for described aqueous matrine solution, the procedure of processing of this method is:
1. pulverize: for the ease of by the extracts active ingredients in kuh-seng raw material out, will after the section of herbal raw material kuh-seng, pulverize as graininess kuh-seng powder;
2. enzymolysis: for kuh-seng powder can further be decomposed, matrine active ingredient is wherein easy to be dissolved in solvent and carries out high efficiency extraction, kuh-seng powder, water and compound biological enzyme are added in insulation rotating cylinder and mixed, raw material is carried out to enzymolysis and obtain enzymolysis feed liquid;
3. extract: for by the extracts active ingredients in enzymolysis feed liquid out, upper step gained enzymolysis feed liquid and water are added to extractor and extract and obtain extract;
4. filter: for the solid particle in filtering extract, improve the quality of liquid, upper step gained extract is filtered, obtain filtered fluid after removing filter residue;
5. concentrated: in order to improve the content of matrine active ingredient in filtered fluid, upper step gained filtered fluid to be added to concentration tank, use the concentrated matrine concentrate that makes of Steam Heating;
6. composite: in order to improve drug effect and the insecticidal effect of aqueous matrine solution, upper step gained matrine concentrate is added to composite tank, under heating condition, in composite tank, add other plant extract intermediate, add again water, plant extract stabilizing agent and plant extract surfactant to mix and obtain mixed liquor, then obtain aqueous matrine solution after adding settling tank to remove precipitation mixed liquor;
7. filling: upper step gained aqueous matrine solution is added and carries out after measuring tank obtaining aqueous matrine solution finished product after filling, vanning, packing.
The present invention is in order to improve the decomposition of compound biological enzyme for matrine powder vegetable fiber, improve the recovery rate of active ingredient, preferably technical scheme also has, the mass ratio of the powder of kuh-seng described in enzymolysis step, water and compound biological enzyme is 1:(1～2): (0.1～0.3), enzymatic hydrolysis condition is 40～50 ℃ of insulations 5～7 hours.
The present invention is in order efficiently to decompose the vegetable fiber in matrine powder, and preferably technical scheme also has, and compound biological enzyme described in enzymolysis step is cellulase, amylase and pectase, and three's mass ratio is 3:(0～5): (0～2).
The present invention is in order to improve the recovery rate for active ingredient matrine, and preferably technical scheme also has, and the volume ratio of the feed liquid of enzymolysis described in extraction step and water is 1:(0.5～4), extraction conditions is to extract 2～6 hours at 50～90 ℃ of temperature
The present invention is in order to make final products aqueous matrine solution have preferably insecticidal effect, and preferably technical scheme also has, and in concentration step, in gained matrine concentrate, the mass content of matrine is greater than 1%.
The present invention is in order further to improve the insecticidal effect of aqueous matrine solution, make aqueous matrine solution have human body hypotoxicity, noresidue, feature on environment without impact simultaneously, preferably technical scheme also has, and other plant extract intermediate described in composite step is the extraction concentrate of one or more plant materials in capsicum, the root of langdu, tobacco leaf, the Chinese prickly ash dregs of rice, tea seed.
The present invention is in order to improve the drug effect of aqueous matrine solution, improve the bin stability of product, preferably technical scheme also has, in the composite operation of composite step, the each amount of substance adding take volume ratio is matrine concentrate 6 volumes, concentrated chilli liquid 2 volumes, root of langdu concentrate 4 volumes, tobacco concentrated liquid 2 volumes, Chinese prickly ash dregs of rice concentrate 3 volumes, tea seed concentrate 2 volumes.
The present invention is in order to improve the effective drug effect of aqueous matrine solution, improves the stability of liquid, and in described aqueous matrine solution, matrine mass fraction is more than or equal to 0.3%, and in aqueous matrine solution, to be less than or equal to 0.5%, pH value be 3.0～7.0 to the mass fraction of insoluble matter.
The present invention is in order to reach for the better extraction effect of matrine active ingredient, and preferably technical scheme also has, and the granularity of the kuh-seng of graininess described in first step powder is 40～60 orders.
Advantage of the present invention and beneficial effect are:
1, utilization of the present invention has bioactive enzyme and carrys out the vegetable fiber in enzymolysis matrine raw material, active ingredient in matrine can be dissolved in completely and extract in solvent, reaches very high recovery rate for active ingredient;
2, the aqueous matrine solution that the inventive method makes has higher insecticidal properties and higher bin stability, be convenient to store and use, compare the conventional medicament making that extracts, the medicament insecticidal activity that the present invention manufactures improves more than 10%, bin stability has improved more than 20%, can meet the requirement of all kinds of agricultural production medications.
3, the botanical pesticide that the inventive method is produced have on human body hypotoxicity, non agricultural chemical residuum, on environment without impact, feature to pest natural enemy without direct killing effect, can meet environmental protection, keep ecological balance and non-harmful production requirement.
4, the aqueous matrine solution that the inventive method is produced has wider insecticidal spectrum, can be used in insects such as killing cabbage caterpillar, aphid, cotton bollworm, two spotted spider mite.
The drug effect lasting period of the aqueous matrine solution that 5, the inventive method is produced is long, and the lasting period reaches about 10-15 days, and uses safety, all can use at florescence, young fruit period, can not produce poisoning to crop, can not produce fruit russeting to young fruit.
Embodiment
The following example will further illustrate content of the present invention.
Embodiment 1
It is a kind of method that uses enzymatic isolation method to produce aqueous matrine solution that the present invention adopts technical scheme, and the concrete implementation step of the method is:
1. pulverize: be 50 object graininess kuh-seng powders by pulverizing after the section of herbal raw material kuh-seng;
2. enzymolysis: kuh-seng powder, water and compound biological enzyme are added take mass ratio as 1:1.5:0.2 in insulation rotating cylinder and mix, raw material is carried out to enzymolysis, obtain enzymolysis feed liquid in 45 ℃ of insulations after 6 hours; Compound biological enzyme is cellulase, amylase and pectase, and three's mass ratio is 3:5:2.
3. extract: by gained enzymolysis feed liquid and water, the ratio take volume ratio as 1:2 is added to extractor and extracts, and extracts and within 4 hours, obtain extract at 65 ℃ of temperature;
4. filter: it is to filter in 200 object liquid medicine filters that gained extract is added to filter screen order number, obtain filtered fluid after removing the filter residue in extract;
5. concentrated: gained filtered fluid is added to concentration tank, use Steam Heating to concentrate and make matrine concentrate, in this matrine concentrate, the mass content of matrine is 1.2%
6. composite: gained matrine concentrate is added to composite tank, under heating condition, in composite tank, add other plant extract intermediate, add again water, plant extract surfactant, plant extract stabilizing agent to mix and obtain mixed liquor, then obtain aqueous matrine solution after adding settling tank to remove precipitation mixed liquor; Other plant extract intermediate is the extraction concentrate of capsaicine, the root of langdu, nicotine, Chinese prickly ash and tea seed five Plants raw materials; The each amount of substance adding take volume ratio is matrine concentrate 6 volumes, concentrated chilli liquid 2 volumes, root of langdu concentrate 4 volumes, tobacco concentrated liquid 2 volumes, Chinese prickly ash dregs of rice concentrate 3 volumes, tea seed concentrate 2 volumes.
7. filling: gained aqueous matrine solution is added and carries out after measuring tank obtaining aqueous matrine solution finished product after filling, vanning, packing.In gained aqueous matrine solution, the mass fraction of matrine is 0.35%, and in aqueous matrine solution, the mass fraction of insoluble matter is that 0.2%, pH value is 5.0.
The experiment that the aqueous matrine solution making with embodiment 1 carries out, shows that the aqueous matrine solution of this method manufacture has good insecticidal effect, safety and bin stability.Concrete experiment is as follows:
Experiment 1:2010 uses the test result of embodiment 1 gained aqueous matrine solution to cotton cotton bollworm
Experiment 2:2011 uses the test result of embodiment 1 gained aqueous matrine solution to cotton cotton bollworm
The data of Comprehensive Experiment 1 and experiment 2 show, the initial stage that enzymolysis aqueous matrine solution occurs cotton cotton bollworm is used this preparation 90-120 gram/acre spray application, and control efficiency can reach 78%～92%, and from the service condition of 2 years various places, control efficiency is comparatively desirable.
Experiment 3:2010 uses the test result of embodiment 1 gained aqueous matrine solution to tea tree two spotted spider mite
Experiment 4:2011 uses the test result of embodiment 1 gained aqueous matrine solution to tea tree two spotted spider mite
The data of Comprehensive Experiment 3 and experiment 4 show, the aqueous matrine solution of embodiment 1 gained uses this preparation 90-120 gram/acre spray application at tea tree two spotted spider mite initial stage of origination, control efficiency reaches 75%～90%, and from the service condition of 2 years various places, control efficiency is comparatively desirable.
Experiment 5: the aqueous matrine solution that embodiment 1 gained kuh-seng aqua product and conventional method make is for the contrast experiment's of cabbage caterpillar control efficiency result:
The data of Comprehensive Experiment 5 show, embodiment 1 gained aqueous matrine solution uses this preparation spray application at cabbage caterpillar initial stage of origination, and the control efficiency of the aqueous matrine solution that control efficiency makes compared with conventional method is high more than 10%.
Comprehensive Experiment 1 shows to experiment 5 data, and the control efficiency of the aqueous matrine solution that the aqueous matrine solution that the inventive method embodiment 1 makes makes compared with conventional method is better.
Embodiment 2
Technical scheme of the present invention is a kind of method that uses enzymatic isolation method to produce aqueous matrine solution, and preferably embodiment also has, and concrete implementation step is:
1. pulverize: be 40 object graininess kuh-seng powders by pulverizing after the section of herbal raw material kuh-seng;
2. enzymolysis: kuh-seng powder, water and compound biological enzyme are added take mass ratio as 1:2:0.3 in insulation rotating cylinder and mix, raw material is carried out to enzymolysis, obtain enzymolysis feed liquid in 40 ℃ of insulations after 7 hours; Compound biological enzyme is cellulase.
3. extract: by gained enzymolysis feed liquid and water, the ratio take volume ratio as 1:2 is added to extractor and extracts, and extracts and within 3 hours, obtain extract at 75 ℃ of temperature;
4. filter: it is to filter in 230 object liquid medicine filters that gained extract is added to filter screen order number, obtain filtered fluid after removing the filter residue in extract;
5. concentrated: gained filtered fluid is added to concentration tank, use Steam Heating to concentrate and make matrine concentrate, in this matrine concentrate, the mass content of matrine is 1.1%
6. composite: gained matrine concentrate is added to composite tank, under heating condition, in composite tank, add other plant extract intermediate, add again water, plant extract surfactant, plant extract stabilizing agent to mix and obtain mixed liquor, then obtain aqueous matrine solution after adding settling tank to remove precipitation mixed liquor; Other plant extract intermediate is the extraction concentrate of capsaicine, the root of langdu, nicotine, Chinese prickly ash and tea seed five Plants raw materials; The each amount of substance adding take volume ratio is matrine concentrate 6 volumes, concentrated chilli liquid 2 volumes, root of langdu concentrate 4 volumes, tobacco concentrated liquid 2 volumes, Chinese prickly ash dregs of rice concentrate 3 volumes, tea seed concentrate 2 volumes.
7. filling: gained aqueous matrine solution is added and carries out after measuring tank obtaining aqueous matrine solution finished product after filling, vanning, packing.In gained aqueous matrine solution, the mass fraction of matrine is 0.35%, and in aqueous matrine solution, insoluble matter quality mark is that 0.3%, pH value is 6.0.
Embodiment 3
Technical scheme of the present invention is a kind of method that uses enzymatic isolation method to produce aqueous matrine solution, and preferably embodiment also has, and concrete implementation step is:
1. pulverize: be 45 object graininess kuh-seng powders by pulverizing after the section of herbal raw material kuh-seng;
2. enzymolysis: kuh-seng powder, water and compound biological enzyme are added take mass ratio as 1:2:0.2 in insulation rotating cylinder and mix, raw material is carried out to enzymolysis, obtain enzymolysis feed liquid in 45 ℃ of insulations after 5 hours; Compound biological enzyme is cellulase, amylase and pectase, and three's mass ratio is 3:3:1
3. extract: by gained enzymolysis feed liquid and water, the ratio take volume ratio as 1:4 is added to extractor and extracts, and extracts and within 6 hours, obtain extract at 55 ℃ of temperature;
4. filter: it is to filter in 250 object liquid medicine filters that gained extract is added to filter screen order number, obtain filtered fluid after removing the filter residue in extract;
5. concentrated: gained filtered fluid is added to concentration tank, use Steam Heating to concentrate and make matrine concentrate, in this matrine concentrate, the mass content of matrine is 1.2%
6. composite: gained matrine concentrate is added to composite tank, under heating condition, in composite tank, add other plant extract intermediate, add again water, plant extract surfactant, plant extract stabilizing agent to mix and obtain mixed liquor, then obtain aqueous matrine solution after adding settling tank to remove precipitation mixed liquor; Other plant extract intermediate is the extraction concentrate of capsaicine, the root of langdu, nicotine, Chinese prickly ash and tea seed five Plants raw materials; The each amount of substance adding take volume ratio is matrine concentrate 6 volumes, concentrated chilli liquid 2 volumes, root of langdu concentrate 4 volumes, tobacco concentrated liquid 2 volumes, Chinese prickly ash dregs of rice concentrate 3 volumes, tea seed concentrate 2 volumes.
7. filling: gained aqueous matrine solution is added and carries out after measuring tank obtaining aqueous matrine solution finished product after filling, vanning, packing.In gained aqueous matrine solution, the mass fraction of matrine is 0.38%, and in aqueous matrine solution, the mass fraction of insoluble matter is that 0.4%, pH value is 5.0.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.And the apparent variation of being amplified out thus or variation are still among protection scope of the present invention.
Claims (1)
1. a method that uses enzymatic isolation method to produce aqueous matrine solution, it is characterized in that, the method is first used compound biological enzyme to carry out enzymolysis the matrine raw material after pulverizing, then after the enzymolysis feed liquid obtaining after enzymolysis being extracted, filter, being concentrated, obtain matrine concentrate, to after gained matrine concentrate and other plant extract intermediate, stabilizing agent and surfactant compound, obtain described aqueous matrine solution again, the method procedure of processing is:
1. pulverize: will after the section of herbal raw material kuh-seng, pulverize as graininess kuh-seng powder, the granularity of described graininess kuh-seng powder is 40～60 orders;
2. enzymolysis: kuh-seng powder, water and compound biological enzyme are added in insulation rotating cylinder and mixed, raw material is carried out to enzymolysis and obtain enzymolysis feed liquid;
3. extract: enzymolysis step gained enzymolysis feed liquid and water are added to extractor and extract and obtain extract;
4. filter: extraction step gained extract is filtered, obtain filtered fluid after removing filter residue;
5. concentrated: filtration step gained filtered fluid to be added to concentration tank, use the concentrated matrine concentrate that makes of Steam Heating;
6. composite: concentration step gained matrine concentrate is added to composite tank, under heating condition, in composite tank, add other plant extract intermediate, add again water, plant extract surfactant, plant extract stabilizing agent to mix and obtain mixed liquor, then obtain aqueous matrine solution after adding settling tank to remove precipitation mixed liquor;
7. filling: composite step gained aqueous matrine solution is added and carries out after measuring tank obtaining aqueous matrine solution finished product after filling, vanning, packing,
Wherein, the mass ratio of the powder of kuh-seng described in enzymolysis step, water and compound biological enzyme is 1:(1～2): (0.1～0.3), enzymatic hydrolysis condition is 40～50 ℃ of insulations 5～7 hours, and
Wherein other plant extract intermediate described in composite step is the extraction concentrate of the various plants raw material in capsicum, the root of langdu, tobacco leaf, the Chinese prickly ash dregs of rice, tea seed, in the composite operation of composite step, the each amount of substance adding take volume ratio is matrine concentrate 6 volumes, concentrated chilli liquid 2 volumes, root of langdu concentrate 4 volumes, tobacco concentrated liquid 2 volumes, Chinese prickly ash dregs of rice concentrate 3 volumes, tea seed concentrate 2 volumes.
2.use enzymatic isolation method as claimed in claim 1 is produced the method for aqueous matrine solution, it is characterized in that, compound biological enzyme described in enzymolysis step is cellulase, amylase and pectase, and three's mass ratio is 3:(0～5): (0～2).
3.use enzymatic isolation method as claimed in claim 2 is produced the method for aqueous matrine solution, it is characterized in that, the volume ratio of the feed liquid of enzymolysis described in extraction step and water is 1:(0.5～4), extraction conditions is to extract 2～6 hours at 50～90 ℃ of temperature.
4.use enzymatic isolation method as claimed in claim 3 is produced the method for aqueous matrine solution, it is characterized in that, in concentration step, in gained matrine concentrate, the mass content of matrine is greater than 1%.
5.use enzymatic isolation method as claimed in claim 4 is produced the method for aqueous matrine solution, it is characterized in that, in described aqueous matrine solution, matrine mass fraction is more than or equal to 0.3%, and in aqueous matrine solution, to be less than or equal to 0.5%, pH value be 3.0～7.0 to the mass fraction of insoluble matter.
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| CN103563623A (en) * | 2013-10-14 | 2014-02-12 | 合肥绿叶园林工程有限责任公司 | Ginkgo seedling planting cultivation method |
| CN111567576A (en) * | 2020-05-07 | 2020-08-25 | 重庆杏磊湾环境治理有限公司 | Production process of biological enzyme fly-killing adjuvant |
| CN113768843B (en) * | 2021-10-18 | 2023-03-28 | 山东花物堂生物科技有限公司 | A radix Sophorae Flavescentis extract for cosmetic and its preparation method |
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| CN101233865A (en) * | 2008-02-26 | 2008-08-06 | 天津市恒源伟业生物科技发展有限公司 | Matrine agent plant pesticide special for killing aphids and preparation thereof |
| CN101233866A (en) * | 2008-02-26 | 2008-08-06 | 天津市恒源伟业生物科技发展有限公司 | Matrine agent plant pesticide special for killing cabbage worm and preparation thereof |
| CN101233867A (en) * | 2008-02-26 | 2008-08-06 | 天津市恒源伟业生物科技发展有限公司 | Matrine agent plant pesticide and preparation thereof |
| CN101926372A (en) * | 2010-07-12 | 2010-12-29 | 重庆东方农药有限公司 | Nicotinamide-matrine aqua vegetable insecticide and preparation method thereof |
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| US7384657B2 (en) * | 2004-10-14 | 2008-06-10 | Jeffrey Young | Composition of natural herb extract for treating cardiovascular disease and its method of preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101233865A (en) * | 2008-02-26 | 2008-08-06 | 天津市恒源伟业生物科技发展有限公司 | Matrine agent plant pesticide special for killing aphids and preparation thereof |
| CN101233866A (en) * | 2008-02-26 | 2008-08-06 | 天津市恒源伟业生物科技发展有限公司 | Matrine agent plant pesticide special for killing cabbage worm and preparation thereof |
| CN101233867A (en) * | 2008-02-26 | 2008-08-06 | 天津市恒源伟业生物科技发展有限公司 | Matrine agent plant pesticide and preparation thereof |
| CN101926372A (en) * | 2010-07-12 | 2010-12-29 | 重庆东方农药有限公司 | Nicotinamide-matrine aqua vegetable insecticide and preparation method thereof |
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