CN103222469A - 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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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 of using 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, though drug effect is than the drug effect height of botanical pesticide, along with the raising of people's living standard, the characteristic of its high toxicity, high residue can't adapt to the requirement to food.Extracting botanical biological pesticide has become feasible mode at present, its hypotoxicity, noresidue, environment is not had influence characteristic, just has been fit to the needs of current social development.
Since China exploitation thing agricultural chemicals, the control efficiency of botanical pesticide is not high, and lethality is about 85%, storage at normal temperature stability is bad, more than 2 become and influence the bottleneck that botanical pesticide develops, hindered the application and the development of botanical pesticide greatly.
There is abundant plant resources in China, and the multiple plant variety that can be used for making botanical pesticide is arranged, and the rhizome of these plants flower, fruit, seed etc. is refined processing can be made into vegetable insecticide.The composition that is used to make botanical pesticide has 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.Contained active insecticidal components has nothing in common with each other in these plant corpuss, widely different between the different plants.
The preparation method of botanical pesticide mainly contains: directly extract (1): the plant big for plant harvest yield, that active constituent content is high, its active ingredient is active strong and be difficult to synthetic, then can directly plant itself or its extract be processed into the agricultural chemicals commodity.(2) total man worker's biomimetic synthesis: in that the plant corpus intensive amount is very little but the compound that biologically active is higher and structure comparatively simply can synthetic then adopts the bionical synthetic mode of total man worker to develop.(3) modify synthetic method: for the active component that the content high activity is low or toxicity is high in plant, after simple the modification, can significantly improve activity or reduce toxicity, and manually be difficult to synthetic or the too high compound of synthetic cost, then adopt the synthetic method of modification to carry out product development.(4) directed synthetic method: for containing the high activity material but compound is difficult to synthetic again, and plant corpus itself be difficult for to obtain or is difficult to plant or biological harvest yield floristics seldom, can utilize biotechnology (cell culture technology, organ culture technology etc.) to carry out the directed active substance of producing of biosynthesis and be processed into preparation use after extracting.(5) template synthetic method: its structure-activity relationship of research behind the isolation identification active component, 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, and can make medicament generation obvious synergistic effect after the drug matching or produce new active ingredient, and is same, and botanical pesticide is carried out composite its control efficiency to nuisance that also can improve.
Because matrine has bigger raw material sources and insecticidal effect preferably, and have and do not have characteristics such as influence to human body hypotoxicity, noresidue, to environment, research and application for matrine is comparatively extensive 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 the extraction efficiency for matrine active ingredient in the raw material is not high in the existing technology, has directly limited the 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, the matrine medicament has the 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 just are to overcome the defective of prior art, a kind of method of using enzymatic isolation method to produce aqueous matrine solution is provided, it utilizes the enzyme of biologically active to come enzymolysis matrine raw material, make the active ingredient in the matrine can be dissolved in fully in the extraction solvent, reach extraction effect preferably; And the aqueous matrine solution that this method makes has higher insecticidal properties and bin stability preferably, to human body hypotoxicity, noresidue, environment is not had influence, can satisfy the demand of market and society.
For addressing the above problem, the present invention adopts technical scheme to be: a kind of method of using enzymatic isolation method to produce aqueous matrine solution, matrine raw material after this method will be pulverized earlier uses compound biological enzyme to carry out enzymolysis, obtain the matrine concentrate after then the enzymolysis feed liquid that obtains behind the enzymolysis being extracted, filter, being concentrated, will obtain described aqueous matrine solution behind gained matrine concentrate and other plant extract intermediate, stabilizing agent and the surfactant compound again.
In order to realize the production for described aqueous matrine solution, the procedure of processing of this method is:
1. pulverize: be graininess kuh-seng powder for the ease of the extracts active ingredients in the kuh-seng raw material being come out, herbal raw material kuh-seng section back being pulverized;
2. enzymolysis: for the kuh-seng powder can further be decomposed, make wherein matrine active ingredient be easy to be dissolved in the solvent and carry out high efficiency extraction, with mixing in kuh-seng powder, water and the compound biological enzyme adding insulation rotating cylinder, raw material is carried out enzymolysis obtain the enzymolysis feed liquid;
3. extract: for the extracts active ingredients in the enzymolysis feed liquid is come out, will go up step gained enzymolysis feed liquid and water and be added to extractor and extract and obtain extract;
4. filter: for the solid particle in the filtering extract, improve the quality of soup, will go up step gained extract and filter, obtain filtered fluid after removing filter residue;
5. concentrate: in order to improve matrine content of effective in the filtered fluid, will go up step gained filtered fluid and add concentration tank, and use Steam Heating to concentrate and make the matrine concentrate;
6. composite: for drug effect and the insecticidal effect that improves aqueous matrine solution, to go up step gained matrine concentrate and add composite jar, under heating condition, in composite jar, add other plant extract intermediate, add entry, plant extract stabilizing agent and plant extract surfactant again and mix and obtain mixed liquor, again mixed liquor is added settling tank and remove post precipitation and obtain aqueous matrine solution;
7. can: will go up step gained aqueous matrine solution and carry out obtaining the aqueous matrine solution finished product after can, vanning, the packing after adding measuring tank.
The present invention is in order to improve the decomposition of compound biological enzyme for matrine powder vegetable fiber, improve extraction ratio of effective constituents, preferable technical scheme also has, the mass ratio of the powder of kuh-seng described in the enzymolysis step, water and compound biological enzyme is 1:(1～2): (0.1～0.3), enzymatic hydrolysis condition are 40～50 ℃ of insulations 5～7 hours.
The present invention is in order efficiently to decompose the vegetable fiber in the matrine powder, and preferable technical scheme also has, and compound biological enzyme described in the 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 the active ingredient matrine, and preferable technical scheme also has, and the volume ratio of feed liquid of enzymolysis described in the extraction step and water is 1:(0.5～4), extraction conditions is to extract 2～6 hours under 50～90 ℃ of temperature
The present invention is in order to make the final products aqueous matrine solution have preferable insecticidal effect, and preferable technical scheme also has, in the concentration step in the gained matrine concentrate mass content of matrine greater than 1%.
The present invention is in order further to improve the insecticidal effect of aqueous matrine solution, make aqueous matrine solution has does not have influence to human body hypotoxicity, noresidue, to environment characteristics simultaneously, preferable technical scheme also has, and other plant extract intermediate described in the 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, the tea seed.
The present invention is in order to improve the drug effect of aqueous matrine solution, improve the bin stability of product, preferable technical scheme also has, in the composite operation of composite step, each amount of substance that adds with 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 improves the stability of soup in order to improve the effective drug effect of aqueous matrine solution, and the matrine mass fraction is more than or equal to 0.3% in the described aqueous matrine solution, and the mass fraction of insoluble matter is smaller or equal to 0.5% in the aqueous matrine solution, and the pH value is 3.0～7.0.
The present invention is in order to reach for the better extraction effect of matrine active ingredient, and preferable 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, the present invention utilizes the enzyme of biologically active to come vegetable fiber in the enzymolysis matrine raw material, makes active ingredient in the matrine to be dissolved in fully and extracts in the solvent, reaches very high recovery rate for active ingredient;
2, the aqueous matrine solution that makes of the inventive method has higher insecticidal properties and higher bin stability, be convenient to store and use, compare the conventional medicament that makes that extracts, the medicament insecticidal activity that the present invention makes improves more than 10%, bin stability has improved more than 20%, can satisfy the requirement of all kinds of agricultural production medications.
3, the botanical pesticide produced of the inventive method has human body hypotoxicity, non agricultural chemical residuum, environment is not had influence, pest natural enemy is not had the characteristics of direct killing effect, can satisfy environmental protection, keep ecological balance and non-harmful production requirement.
4, the aqueous matrine solution of the inventive method production has wider insecticidal spectrum, can be used in insects such as killing cabbage caterpillar, aphid, cotton bollworm, two spotted spider mite.
5, the drug effect lasting period of the aqueous matrine solution produced of the inventive method long, the lasting period reached about 10-15 days, and safe in utilization, 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 specify content of the present invention.
Embodiment 1
It is a kind of method of using enzymatic isolation method to produce aqueous matrine solution that the present invention adopts technical scheme, and the concrete implementation step of this method is:
1. pulverize: it is 50 purpose graininess kuh-seng powders that herbal raw material kuh-seng section back is pulverized;
2. enzymolysis: with kuh-seng powder, water and compound biological enzyme is that 1:1.5:0.2 adds in the insulation rotating cylinder and mixes with the mass ratio, and raw material is carried out enzymolysis, obtains the 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: with gained enzymolysis feed liquid and water is that the ratio of 1:2 is added to extractor and extracts with the volume ratio, and extraction obtained extract in 4 hours under 65 ℃ of temperature;
4. filter: it is to filter in the 200 purpose liquid medicine filters that the gained extract is added filter screen order number, obtains filtered fluid after removing the filter residue in the extract;
5. concentrate: the gained filtered fluid is added concentration tank, use Steam Heating to concentrate and make the matrine concentrate, the mass content of matrine is 1.2% in this matrine concentrate
6. composite: that gained matrine concentrate is added composite jar, under heating condition, in composite jar, add other plant extract intermediate, add entry, plant extract surfactant, plant extract stabilizing agent again and mix and obtain mixed liquor, again mixed liquor is added settling tank and remove post precipitation and obtain aqueous matrine solution; Other plant extract intermediate is the extraction concentrate of capsaicine, the root of langdu, nicotine, Chinese prickly ash and tea seed five plant species raw materials; Each amount of substance that adds with 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. can: will carry out obtaining the aqueous matrine solution finished product after can, vanning, the packing behind the gained aqueous matrine solution adding measuring tank.The mass fraction of matrine is 0.35% in the gained aqueous matrine solution, and the mass fraction of insoluble matter is 0.2% in the aqueous matrine solution, and the pH value is 5.0.
The experiment that the aqueous matrine solution that makes with embodiment 1 carries out shows that the aqueous matrine solution of this method manufacturing has insecticidal effect, safety and bin stability preferably.Concrete experiment is as follows:
Experiment 1:2010 uses the test result of embodiment 1 gained aqueous matrine solution to the cotton cotton bollworm
Experiment 2:2011 uses the test result of embodiment 1 gained aqueous matrine solution to the cotton cotton bollworm
The data of Comprehensive Experiment 1 and experiment 2 show that the enzymolysis aqueous matrine solution uses this preparation 90-120 gram/mu spray application at the initial stage that the cotton cotton bollworm is taken place, and control efficiency can reach 78%～92%, and from the operating position 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 the tea tree two spotted spider mite
Experiment 4:2011 uses the test result of embodiment 1 gained aqueous matrine solution to the 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/mu spray application at tea tree two spotted spider mite initial stage of origination, control efficiency reaches 75%～90%, and from the operating position 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 that embodiment 1 gained aqueous matrine solution uses this preparation spray application at the cabbage caterpillar initial stage of origination, and control efficiency is high more than 10% than the control efficiency of the aqueous matrine solution that conventional method makes.
Comprehensive Experiment 1 to the data of experiment 5 show that the aqueous matrine solution that the inventive method embodiment 1 makes is better than the control efficiency of the aqueous matrine solution that conventional method makes.
Embodiment 2
Technical scheme of the present invention is a kind of method of using enzymatic isolation method to produce aqueous matrine solution, and preferred implementation also has, and concrete implementation step is:
1. pulverize: it is 40 purpose graininess kuh-seng powders that herbal raw material kuh-seng section back is pulverized;
2. enzymolysis: with kuh-seng powder, water and compound biological enzyme is that 1:2:0.3 adds in the insulation rotating cylinder and mixes with the mass ratio, and raw material is carried out enzymolysis, obtains the enzymolysis feed liquid in 40 ℃ of insulations after 7 hours; Compound biological enzyme is a cellulase.
3. extract: with gained enzymolysis feed liquid and water is that the ratio of 1:2 is added to extractor and extracts with the volume ratio, and extraction obtained extract in 3 hours under 75 ℃ of temperature;
4. filter: it is to filter in the 230 purpose liquid medicine filters that the gained extract is added filter screen order number, obtains filtered fluid after removing the filter residue in the extract;
5. concentrate: the gained filtered fluid is added concentration tank, use Steam Heating to concentrate and make the matrine concentrate, the mass content of matrine is 1.1% in this matrine concentrate
6. composite: that gained matrine concentrate is added composite jar, under heating condition, in composite jar, add other plant extract intermediate, add entry, plant extract surfactant, plant extract stabilizing agent again and mix and obtain mixed liquor, again mixed liquor is added settling tank and remove post precipitation and obtain aqueous matrine solution; Other plant extract intermediate is the extraction concentrate of capsaicine, the root of langdu, nicotine, Chinese prickly ash and tea seed five plant species raw materials; Each amount of substance that adds with 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. can: will carry out obtaining the aqueous matrine solution finished product after can, vanning, the packing behind the gained aqueous matrine solution adding measuring tank.The mass fraction of matrine is 0.35% in the gained aqueous matrine solution, and insoluble matter quality mark is 0.3% in the aqueous matrine solution, and the pH value is 6.0.
Embodiment 3
Technical scheme of the present invention is a kind of method of using enzymatic isolation method to produce aqueous matrine solution, and preferred implementation also has, and concrete implementation step is:
1. pulverize: it is 45 purpose graininess kuh-seng powders that herbal raw material kuh-seng section back is pulverized;
2. enzymolysis: with kuh-seng powder, water and compound biological enzyme is that 1:2:0.2 adds in the insulation rotating cylinder and mixes with the mass ratio, and raw material is carried out enzymolysis, obtains the 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: with gained enzymolysis feed liquid and water is that the ratio of 1:4 is added to extractor and extracts with the volume ratio, and extraction obtained extract in 6 hours under 55 ℃ of temperature;
4. filter: it is to filter in the 250 purpose liquid medicine filters that the gained extract is added filter screen order number, obtains filtered fluid after removing the filter residue in the extract;
5. concentrate: the gained filtered fluid is added concentration tank, use Steam Heating to concentrate and make the matrine concentrate, the mass content of matrine is 1.2% in this matrine concentrate
6. composite: that gained matrine concentrate is added composite jar, under heating condition, in composite jar, add other plant extract intermediate, add entry, plant extract surfactant, plant extract stabilizing agent again and mix and obtain mixed liquor, again mixed liquor is added settling tank and remove post precipitation and obtain aqueous matrine solution; Other plant extract intermediate is the extraction concentrate of capsaicine, the root of langdu, nicotine, Chinese prickly ash and tea seed five plant species raw materials; Each amount of substance that adds with 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. can: will carry out obtaining the aqueous matrine solution finished product after can, vanning, the packing behind the gained aqueous matrine solution adding measuring tank.The mass fraction of matrine is 0.38% in the gained aqueous matrine solution, and the mass fraction of insoluble matter is 0.4% in the aqueous matrine solution, and the pH value is 5.0.
It should be noted that at last: obviously, the foregoing description only is for example of the present invention clearly is described, and is not the qualification 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 need not also can't give exhaustive to all embodiments.And conspicuous variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (10)
1. method of using enzymatic isolation method to produce aqueous matrine solution, it is characterized in that, matrine raw material after this method will be pulverized earlier uses compound biological enzyme to carry out enzymolysis, obtain the matrine concentrate after then the enzymolysis feed liquid that obtains behind the enzymolysis being extracted, filter, being concentrated, will obtain described aqueous matrine solution behind gained matrine concentrate and other plant extract intermediate, stabilizing agent and the surfactant compound again.
2. use enzymatic isolation method as claimed in claim 1 is produced the method for aqueous matrine solution, it is characterized in that this method procedure of processing is:
1. pulverize: it is graininess kuh-seng powder that herbal raw material kuh-seng section back is pulverized;
2. enzymolysis: kuh-seng powder, water and compound biological enzyme added in the insulation rotating cylinder mix, raw material is carried out enzymolysis obtain the enzymolysis feed liquid;
3. extract: enzymolysis step gained enzymolysis feed liquid and water are added to extractor extract and obtain extract;
4. filter: extraction step gained extract is filtered, obtain filtered fluid after removing filter residue;
5. concentrate: filtration step gained filtered fluid is added concentration tank, use Steam Heating to concentrate and make the matrine concentrate;
6. composite: that concentration step gained matrine concentrate is added composite jar, under heating condition, in composite jar, add other plant extract intermediate, add entry, plant extract surfactant, plant extract stabilizing agent again and mix and obtain mixed liquor, again mixed liquor is added settling tank and remove post precipitation and obtain aqueous matrine solution;
7. can: will carry out obtaining the aqueous matrine solution finished product after can, vanning, the packing behind the composite step gained aqueous matrine solution adding measuring tank.
3. use enzymatic isolation method as claimed in claim 2 is produced the method for aqueous matrine solution, it is characterized in that, the mass ratio of the powder of kuh-seng described in the enzymolysis step, water and compound biological enzyme is 1:(1～2): (0.1～0.3), enzymatic hydrolysis condition are 40～50 ℃ of insulations 5～7 hours.
4. use enzymatic isolation method as claimed in claim 3 is produced the method for aqueous matrine solution, it is characterized in that compound biological enzyme described in the enzymolysis step is cellulase, amylase and pectase, and three's mass ratio is 3:(0～5): (0～2).
5. use enzymatic isolation method as claimed in claim 4 is produced the method for aqueous matrine solution, it is characterized in that the volume ratio of feed liquid of enzymolysis described in the extraction step and water is 1:(0.5～4), extraction conditions is to extract 2～6 hours under 50～90 ℃ of temperature.
6. use enzymatic isolation method as claimed in claim 5 is produced the method for aqueous matrine solution, it is characterized in that, in the concentration step in the gained matrine concentrate mass content of matrine greater than 1%.
7. use enzymatic isolation method as claimed in claim 6 is produced the method for aqueous matrine solution, it is characterized in that other plant extract intermediate described in the 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, the tea seed.
8. use enzymatic isolation method as claimed in claim 7 is produced the method for aqueous matrine solution, it is characterized in that, in the composite operation of composite step, each amount of substance that adds with 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.
9. use enzymatic isolation method as claimed in claim 8 is produced the method for aqueous matrine solution, it is characterized in that the granularity of the kuh-seng of graininess described in first step powder is 40～60 orders.
10. use enzymatic isolation method as claimed in claim 9 is produced the method for aqueous matrine solution, it is characterized in that, the matrine mass fraction is more than or equal to 0.3% in the described aqueous matrine solution, and the mass fraction of insoluble matter is smaller or equal to 0.5% in the aqueous matrine solution, and the pH value is 3.0～7.0.
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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 |
| CN113768843A (en) * | 2021-10-18 | 2021-12-10 | 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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| CN103222469B (en) | 2014-07-02 |
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