CN114938808A - Magnolia officinalis alkali and nuciferine medicinal composition and preparation method thereof - Google Patents
Magnolia officinalis alkali and nuciferine medicinal composition and preparation method thereof Download PDFInfo
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
- A01N43/42—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
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- A—HUMAN NECESSITIES
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
The invention discloses a officinal magnolia alkali and nuciferine pharmaceutical composition and a preparation method thereof, wherein the composition comprises the officinal magnolia alkali and nuciferine, and the proportion of the officinal magnolia alkali to the nuciferine is as follows: 1: 9-9: 1, the composition comprises missible oil, wettable powder, a suspending agent and water dispersible granules, and can be used for preventing and treating the plum brown rot. The active ingredients contained in the invention are the magnoline and the nuciferine which are both extracted from plants, can be decomposed in natural environment, have no chemical residue, are green and healthy to people and livestock, and greatly improve the quality safety of agricultural products. After the composition is compounded, the composition has obvious synergistic effect, and compared with a single active ingredient, the control effect of the composition is obviously improved; the active ingredients in the composition can delay the generation of drug resistance of pathogenic bacteria while effectively preventing and treating crop diseases, is beneficial to delaying the service life of pesticide active ingredients, reduces the production cost and the use cost, is beneficial to the comprehensive prevention and treatment of resistant diseases, and has simple preparation process.
Description
Technical Field
The invention relates to a pharmaceutical composition, in particular to a magnoline and nuciferine pharmaceutical composition and a preparation method thereof, and belongs to the technical field of pesticide compounding.
Background
Plum brown rot is caused by fungi of the genera sclerotinia (Monilinia) and Monilia (Monilia), wherein the main pathogenic bacterium is sclerotinia sclerotiorum (m.fructicola). The infection sites of the disease are distributed on the surface and pedicles of the fruit, the fruit is invaded to generate yellow brown disease spots, the disease spots are gradually enlarged and accompanied with grey velvet-shaped particle protrusions, the surface of the fruit becomes dark brown to black after the disease is aggravated, grey mildew layers gradually grow around the disease spots, and finally the diseased fruit is rotten, loses water and withers to cause fruit drop and dead fruit. The disease overwinter with mycelium in the tree and within the runt fruits or ulcerated parts of the branch tips. In the next spring, a large number of conidia are generated, primary infection is carried out through insect injury, mechanical injury or natural orifice invasion by virtue of wind and rain or insect propagation, and a large number of spores are generated on the surface of a diseased part for secondary infection in rainy and foggy weather; the flowering phase is low in temperature, moist and rainy, and is easy to cause flower rot; the fruits are warm and rainy and foggy in the mature period and are easy to rot. At present, the prevention and control of the plum brown rot still mainly adopt chemical agents, but the drug resistance of pathogenic bacteria is easily improved, and frequent application of the drugs also easily causes environmental pollution and pesticide residue, so that research and development of plant active substances for preventing and controlling the plum brown rot have important significance for the development of the plum industry.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the magnoline and nuciferine are added with different components to form different formulations, so that the composition has the characteristics of synergistic action, low use cost, good effect, greenness and no pollution, can be used for preventing and treating plum brown rot, and effectively solves the existing problems.
The technical scheme of the invention is as follows: a officinal magnolia alkali and nuciferine pharmaceutical composition comprises officinal magnolia alkali and nuciferine, wherein the mass ratio of the officinal magnolia alkali to the nuciferine is as follows: 1: 9-9: 1.
The magnoline is a benzyl isoquinoline alkaloid separated and extracted from the dry bark, root bark or branch bark of magnolia officinalis or magnolia biloba belonging to the deciduous tree family, has the activities of sterilization, disinsection and weeding, shows stronger sensitivity and better drug-resistant reduction action on a plurality of pathogenic fungi, is easy to degrade in the environment, is safe to the environment, is harmless to human and livestock, and has huge fungicide development potential. The molecular formula of the magnoline is C19H24NO3+, and the structural formula is as follows:
nuciferine is an aporphine alkaloid derived from dried lotus leaves of Nymphaeaceae, and is also a quality control component of lotus leaves loaded in Chinese pharmacopoeia. Has good insecticidal, antibacterial and antiviral effects. Nuciferine can achieve bactericidal effect by destroying cell structures of bacteria and fungi, inhibiting mitosis, and influencing energy metabolism. Nuciferine has a molecular formula of C19H21NO2, and a structural formula of:
the formulation of the composition comprises missible oil, wettable powder, a suspending agent and water dispersible granules, and the composition can be used for preventing and treating the plum brown rot.
The composition comprises the following emulsion agent types in percentage by mass: 1-20% of magnoline, 1-20% of nuciferine, 5-20% of emulsifier, 5-30% of solvent, 0.5-10% of thickening agent, 0.5-10% of preservative and the balance of distilled water.
The emulsifier can be any one of castor oil polyoxyethylene ether, calcium dodecyl benzene sulfonate, fatty acid polyoxyethylene ether, styryl phenol polyoxyethylene ether, nonylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester, the solvent is any one of dimethyl sulfoxide, xylene, toluene, methanol, ethanol, acetone, isopropanol, methyl esterified vegetable oil and dimethylformamide, the thickener is any one of methyl cellulose, xanthan gum, polyvinyl alcohol, magnesium aluminum silicate, carboxymethyl cellulose and carboxyethyl cellulose, and the preservative is any one of nisin or 2-bromo-2-nitro-1, 3-propanediol.
A preparation method of a officinal magnolia base and nuciferine pharmaceutical composition comprises the following steps: uniformly mixing the magnoline and the nuciferine in proportion, completely dissolving the mixture by using a solvent, sequentially adding an emulsifier, a thickening agent and a preservative, and uniformly stirring to obtain the officinal magnolia and nuciferine missible oil.
The wettable powder of the composition comprises the following components in percentage by mass: 1-20% of magnoline, 1-20% of nuciferine, 1-5% of a wetting agent, 1-10% of a dispersing agent, 0.5-10% of a penetrating agent and the balance of a filler.
The wetting agent is any one of sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, naphthalene sulfonate, alkyl sulfonate and alkylbenzene sulfonate polyoxyethylene triphenyl-ethylene phenyl phosphate; the dispersing agent is any one of lignosulfonate, polycarboxylate, alkyl naphthalene formaldehyde condensate sulfonate, fatty acid polyoxyethylene ester, fatty amine polyoxyethylene ether and glycerol fatty acid ester polyoxyethylene ether, and the penetrating agent is fatty alcohol polyoxyethylene ether; the filler can be any one of kaolin, diatomite, bentonite, white carbon black, sepiolite, talcum powder and pottery clay.
A preparation method of a officinal magnolia base and nuciferine pharmaceutical composition comprises the following steps: mixing the magnoline, the nuciferine, the wetting agent, the dispersing agent, the penetrating agent and the filler, crushing the mixture by using an airflow crusher, and then uniformly mixing the crushed mixture to obtain the magnoline and nuciferine wettable powder.
The suspending agent of the composition comprises the following components in percentage by mass: 1-20% of magnoline, 1-20% of nuciferine, 1-10% of dispersing agent, 1-10% of emulsifier, 0.1-5% of wetting agent, 0.5-5% of thickening agent, 0.1-2% of defoaming agent, 0.1-5% of antifreezing agent and the balance of distilled water.
The dispersing agent is any one of lignosulfonate, polycarboxylate, alkyl naphthalene formaldehyde condensate sulfonate, fatty acid polyoxyethylene ester, fatty amine polyoxyethylene ether and glycerin fatty acid ester polyoxyethylene ether, and the emulsifying agent is any one of castor oil polyoxyethylene ether, calcium dodecyl benzene sulfonate, fatty acid polyoxyethylene ether, styrylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester; the wetting agent is any one of sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, naphthalene sulfonate and alkyl sulfonate; the thickener is any one of methylcellulose, xanthan gum, polyvinyl alcohol, magnesium aluminum silicate, carboxymethyl cellulose and carboxyethyl cellulose; the defoaming agent is any one of silicone oil, silicone compounds, C10-20 saturated fatty acid compounds, C8-10 fatty alcohols, hexanol, butanol and octanol; the antifreeze is any one of glycerol, polyethylene glycol, sorbitol, urea, glycerol, ethylene glycol and propylene glycol.
A preparation method of a officinal magnolia base and nuciferine pharmaceutical composition comprises the following steps: uniformly mixing the dispersing agent, the emulsifying agent, the wetting agent, the thickening agent, the defoaming agent and the antifreezing agent, adding the magnoline and the nuciferine, and uniformly stirring until the magnoline and the nuciferine are completely dissolved to obtain the magnoline and nuciferine suspending agent.
The composition comprises the following water dispersible granules in percentage by mass: 1-20% of magnoline, 1-20% of nuciferine, 40-80% of carrier, 1-10% of dispersing agent, 1-10% of wetting agent, 0.5-10% of disintegrating agent and the balance of filler.
The carrier can be kaolin or black carbon soil; the dispersing agent is any one of lignosulfonate, polycarboxylate, alkyl naphthalene formaldehyde condensate sulfonate, fatty acid polyoxyethylene ester, fatty amine polyoxyethylene ether and glycerol fatty acid ester polyoxyethylene ether; the wetting agent is any one of sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, naphthalene sulfonate and alkyl sulfonate; the disintegrating agent is any one of sucrose, bentonite, urea, glucose, ammonium sulfate, aluminum chloride, citric acid, and succinic acid.
A preparation method of a officinal magnolia alkali and nuciferine medicinal composition comprises the following steps: uniformly mixing the magnoline, the nuciferine, the carrier, the dispersing agent and the disintegrating agent, then crushing the mixture, mixing the crushed mixture with the wetting agent dissolved by adding water to obtain a suspension, drying the suspension, and then mixing the dried suspension with the diatomite at a high speed for granulation to obtain the magnoline and nuciferine water dispersible granules.
The invention has the beneficial effects that: compared with the prior art, the technical scheme of the invention has the characteristics of low research and development cost, convenient use and easy popularization, and indoor screening and field tests show that the combination of the magnoline and the nuciferine can improve the toxicity of the drug on the plum brown rot and the field control effect, and has good use effect.
The active ingredients contained in the invention are the magnoline and the nuciferine which are both extracted from plants, can be decomposed in natural environment, have no chemical residue, are green and healthy to people and livestock, and greatly improve the quality safety of agricultural products.
After the composition is compounded, the composition has obvious synergistic interaction in a certain range, and compared with a single active ingredient, the control effect of the composition is obviously improved;
the active ingredients in the composition can delay the generation of drug resistance of pathogenic bacteria while effectively preventing and treating crop diseases, is favorable for delaying the service life of the pesticide active ingredients, further reduces the production cost and the use cost, and is favorable for comprehensive prevention and treatment of resistant diseases;
the composition disclosed by the invention is simple in preparation process and suitable for large-scale popularization and application in actual production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below.
Example 1: a pharmaceutical composition containing magnoline and nuciferine comprises the effective component ratio of the magnoline to the nuciferine of 1: 9-9: 1.
The formulation of the composition comprises missible oil, wettable powder, suspending agent and water dispersible granules.
The specific implementation method comprises the following steps:
1 materials and methods
1.1 test materials
Magnoliae officinalis base (Changsha Shanhe biological science, purity is greater than or equal to 98%), nuciferine (Chengdu Rui biological science, purity is greater than or equal to 98%). Sclerotinia sclerotiorum (monilinia. fructicola), provided by the university of guizhou, deposited at the institute of crop protection.
1.2 test methods
1.2.1 indoor virulence assay: adopting a hypha growth rate inhibition method, mixing the magnoline and the nuciferine according to the proportion of 1:1, 1:3, 1:5, 1:7, 1:9, 9:1, 7:1, 5:1 and 3:1, respectively using a single agent as a control, diluting to each concentration required by a test, adding a test medicament with a certain prepared concentration into a sterilized PDA culture medium (cooled to about 50 ℃), fully shaking and mixing uniformly to prepare medicament-containing flat plates with different concentration gradients, and using the PDA flat plate added with the same mass of sterile water as a Control (CK). And (3) punching a bacterial cake at the edge of the activated pathogenic bacteria colony for 7 days by using a puncher with the diameter of 5mm, inoculating the bacterial cake to the center of a PDA (personal digital assistant) plate containing medicines with different concentration gradients, placing the plate in a constant-temperature incubator at 25 ℃ for dark culture, repeating each treatment for 3 times, measuring the diameter of each treated bacterial colony by adopting a cross method when the bacterial colony of a blank control group occupies about 2/3 of a culture dish, and calculating the inhibition rate of each medicament treatment on the growth of the pathogenic bacteria according to the following formula.
Inhibition (%) - (control colony diameter-treated colony diameter)/control colony diameter ] × 100
By using the indoor biological determination data processing system software of the pesticide, the toxicity regression curve equation of each medicament to different pathogenic bacteria is calculated, and the correlation coefficient r, the effective inhibition intermediate concentration EC50, the standard error and the confidence interval are calculated.
Calculating the virulence index, theoretical virulence index, actual virulence index and the cotoxicity coefficient (CTC) value of the mixture by a Sun Yunpei method, and performing comprehensive evaluation according to the virulence index, the theoretical virulence index, the actual virulence index and the cotoxicity coefficient (CTC) value, wherein CTC >120 represents synergism, CTC <80 represents addition, and CTC <80 represents antagonism. The formula for calculating the co-toxicity coefficient CTC value is as follows:
measured agent virulence index (ATI) ═ EC50 for standard agent/EC 50 for test agent x 100
Theoretical virulence index (TTI) of the combination (virulence index of agent a × Ax) + (virulence index of agent B × Bx)
Co-toxicity coefficient (CTC) ═ ATI/TTI × 100
Ax is the percentage content of the medicament A in the mixture;
bx is the percentage content of the medicament B in the mixture.
1.2.2 field control effect test: the most obvious compound proportion of the synergistic effect is selected for field efficacy test, two single agents are used as control, and equal amount of clear water is sprayed as blank Control (CK). The total number of the treatments is 4, each treatment is repeated for 3 times, the total number of the treatments is 12 cells, random arrangement is adopted, the row spacing of the plum tree is 3m multiplied by 4m, and protection rows are arranged among the cells. Respectively spraying the liquid medicine once by adopting a conventional spraying method in the fruit setting period and the near-mature period, and uniformly spraying the liquid medicine on the surfaces of fruits and leaves.
And investigating the control effect 10 days before harvesting. Each cell was investigated for 5 plants, each plant was sampled at 5 points east, west, south, north and middle, and each point was investigated for 30 fruits fixedly. Recording the total number of fruits and the number of diseased fruits, and calculating the prevention and treatment effect.
Disease fruit rate (%) (number of diseased fruits/total number of investigated fruits) × 100
2 results of the test
2.1 the inhibitory effect data of the combination of Houttubine and nuciferine on the growth of M.fructicola hyphae is shown in Table 1 and Table 2.
TABLE 1 toxicity test results of M.fructicola by Magnoliae officinalis alkali, nuciferine and their mixture
As can be seen from Table 1, the co-toxicity coefficient of the compound of the magnoline and the nuciferine on M.fructicola is 116.82-550.07, the EC50 value is 1.2849-9.7781 mg.L < -1 >, and all the proportions show good antibacterial effect on the M.fructicola. Magnoline: the effective component ratio of nuciferine is 1:1, 1:3, 1:5, 1:7, 9:1, 7:1, 5:1 and 3:1, the CTC of the composition is more than 120, the synergistic effect is shown as synergistic effect, and when the effective component ratio is 1:1, the maximum CTC value is 550.07; the minimum EC50 value was 1.2849 mg. L-1.
TABLE 2 field control of brown rot in plums by different treatments
As can be seen from the table 2, the combination of the magnoline and the nuciferine can reduce the incidence rate of the plum brown rot and improve the field control effect. The prevention and treatment effect of the compound preparation of the magnoline and the nuciferine on the brown rot of the plum is obviously better than the prevention and treatment effect of the preparation of a single active ingredient, and in the application range, the composition preparation is not found to cause phytotoxicity to crops, so that the composition provided by the invention is good in safety and worthy of popularization and application in production.
The invention determines the indoor bacteriostatic effect of the officinal magnolia alkali and nuciferine medicinal composition on the pathogenic bacteria of the American-type and Australian stone fruits and the field control effect on the plum brown rot. The two alkaloids have low cost, are non-toxic and harmless, can be used as a potential biopesticide, and have wide development and application prospects.
The present invention is not described in detail, but is known to those skilled in the art. Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. A officinal magnolia alkali and nuciferine pharmaceutical composition is characterized in that: the composition comprises the magnoline and the nuciferine, wherein the mass ratio of the magnoline to the nuciferine is as follows: 1: 9-9: 1.
2. The magnolia officinalis base and nuciferine pharmaceutical composition as claimed in claim 1, wherein: the formulation of the composition comprises missible oil, wettable powder, a suspending agent and water dispersible granules, and the composition can be used for preventing and treating the plum brown rot.
3. The magnolia officinalis base and nuciferine pharmaceutical composition as claimed in claim 2, wherein: the composition comprises the following emulsion agent types in percentage by mass: 1-20% of magnoline, 1-20% of nuciferine, 5-20% of emulsifier, 5-30% of solvent, 0.5-10% of thickening agent, 0.5-10% of preservative and the balance of distilled water.
4. The method of preparing a magnolia officinalis base and nuciferine pharmaceutical composition as claimed in claim 3, wherein: the method comprises the following steps: uniformly mixing the magnoline and the nuciferine in proportion, completely dissolving the mixture by using a solvent, sequentially adding an emulsifier, a thickening agent and a preservative, and uniformly stirring to obtain the officinal magnolia and nuciferine missible oil.
5. The magnolia officinalis base and nuciferine pharmaceutical composition as claimed in claim 2, wherein: the wettable powder of the composition comprises the following components in percentage by mass: 1-20% of magnoline, 1-20% of nuciferine, 1-5% of wetting agent, 1-10% of dispersing agent, 0.5-10% of penetrating agent and the balance of filler.
6. The method of preparing a magnolia officinalis base and nuciferine pharmaceutical composition as claimed in claim 5, wherein: the method comprises the following steps: mixing the magnoline, the nuciferine, the wetting agent, the dispersing agent, the penetrating agent and the filler, crushing the mixture by using an airflow crusher, and then uniformly mixing the crushed mixture to obtain the magnoline and nuciferine wettable powder.
7. The magnolia officinalis base and nuciferine pharmaceutical composition as claimed in claim 2, wherein: the suspending agent of the composition comprises the following components in percentage by mass: 1-20% of magnoline, 1-20% of nuciferine, 1-10% of dispersing agent, 1-10% of emulsifier, 0.1-5% of wetting agent, 0.5-5% of thickening agent, 0.1-2% of defoaming agent, 0.1-5% of antifreezing agent and the balance of distilled water.
8. The method for preparing the officinal magnolia base and nuciferine pharmaceutical composition according to claim 7, wherein the steps of: the method comprises the following steps: uniformly mixing the dispersing agent, the emulsifying agent, the wetting agent, the thickening agent, the defoaming agent and the antifreezing agent, adding the magnoline and the nuciferine, and uniformly stirring until the magnoline and the nuciferine are completely dissolved to obtain the magnoline and nuciferine suspending agent.
9. The magnolia officinalis base and nuciferine pharmaceutical composition as claimed in claim 2, wherein: the composition comprises the following water dispersible granules in percentage by mass: 1-20% of magnoline, 1-20% of nuciferine, 40-80% of carrier, 1-10% of dispersing agent, 1-10% of wetting agent, 0.5-10% of disintegrating agent and the balance of filler.
10. The method of preparing a magnolia officinalis base and nuciferine pharmaceutical composition as claimed in claim 9, wherein: the method comprises the following steps: uniformly mixing the magnoline, the nuciferine, the carrier, the dispersing agent and the disintegrating agent, then crushing, mixing with the wetting agent dissolved by adding water to obtain a suspension, drying the suspension, and then mixing with the diatomite at a high speed for granulation to obtain the magnoline and nuciferine water dispersible granules.
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