CN104585167A - Preparation method for gingko exocarp extract nano capsule - Google Patents
Preparation method for gingko exocarp extract nano capsule Download PDFInfo
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Abstract
The invention discloses a preparation method for a gingko exocarp extract nano capsule. The preparation method comprises the following steps: (1) dissolving 0.3g of ammonium persulfate (an initiator) into 60g of water; (2) weighing and dissolving 1.5g of gingko exocarp extract into mixed monomer; (3) dissolving 18g of OP-50 and 3g of lauryl sodium sulfate into 150g of a 2% polyvinyl alcohol aqueous solution, adding the mixed monomer and dispersing to form emulsion; (4) heating and keeping the emulsion at a temperature of 70 DEG C, adding a first part of the initiator to form seed emulsion; and dropwise adding 4.5g of styrene, 4.5g of butyl acrylate, 3g of acrylic mixed monomer and a second part of the initiator, adding auxiliaries and discharging. The micro capsule does not generate precipitates at a high temperature and a low temperature, and has the characteristics of good physical and chemical stability. By taking water as a dispersion medium, the preparation does not contain or contains a little organic solvent, meets the modern pesticide gent development direction, and is suitable for the current agricultural sustainable development requirements.
Description
Technical field
The present invention relates to a kind of preparation of agricultural chemicals, particularly relate to a kind of preparation of extraction fromginkgoseed coat nano-capsule.
Background technology
The society caused along with agricultural chemicals and ecological problem are subject to the growing interest of people, and using and acting on of chemical pesticide is subjected to general query.80 ~ nineties of 20th century, domestic and international many experts think, the use of chemical pesticide will be walked to be at the end, and instead will be progressively the anti-and integrated controls of biological and ecological methods to prevent plant disease, pests, and erosion, thing etc.But the fact shows, within the foreseeable period of history, agricultural chemicals and chemical control method will be substituted completely.Since two thousand, the Ministry of Agriculture and local governments at all levels put into effect regulations in succession, prohibit the use of many high poison, high residue chemical pesticide (as Furadan, parathion-methyl etc.).According to pesticide industry " 12 " planning, efficient, safety, economy in 2015 and eco-friendly pesticide species will account for more than 50% of gross yield.Therefore, develop efficient to pest, to decompose and catabolite is the field of extensively investigation and application at present to the harmless biopesticide of environment to non-target organism safety, easily
[5], botanical pesticide becomes one of ideal substitute products.
Botanical pesticide refers to some position of utilizing plant or extracts its effective active composition, makes the agricultural chemicals with antibacterial or insecticidal effect.The formation of plant resource active component and the objectivity extensively existed at natural world thereof, it is the result adapted with organic evolution process, there is environmentally friendly nuisanceless, toxicity generally lower, easy degraded, noresidue in crop pest control, not easily making disease worm produce the advantages such as corresponding pesticide resistance, is the pesticide species that production non-polluted farm product should preferentially be selected
[6].
The research and development approach of plant insecticide is a lot, mainly contains following several:
(1) plant that extracting directly enriches in plant resources, with low cost, biological harvest yield is large, active constituent content is high, the active ingredient of its complexity is active strong and be difficult to realize Prof. Du Yucang, then directly plant itself or its extract can be processed into agricultural chemicals commodity.
(2) total man's work biomimetic synthesis is drawn materials afoul for plant resources relative rarity with Chinese medicine, plant corpus intensive amount is very micro-but biologically active is higher and the relatively simple floristics of compound structure, then can adopt Prof. Du Yucang or modify and add other structures, synthesize the compound that its activity is higher or higher, comprise controlled syntheses method and template synthesis method etc.
(3) the composite theory according to drug matching, can make medicament produce obvious synergistic effect or produce new active ingredient after the compatibility that Chinese medicine is scientific and reasonable.Plant great majority in plant insecticide, also for Chinese medicine is drawn materials object, so use for reference theory of traditional Chinese medical science, carry out compositely also can improving its control effect to pest to plant insecticide.
In recent years, extraction and the utilization of focusing on active substance in research gingko episperm was started both at home and abroad.Current experimental study shows, the active substance extracted in gingko episperm has the effect of antiallergy, anti-inflammatory, antibacterial, antiviral, anti-ageing, anti-plant pest.
It is produce pollution-free food that gingko episperm develops as biopesticide, ensures the objective of the struggle of health.Acrylic component in gingko episperm is the main component making biopesticide, on plant pest management, effect is good, prevention and treatment range is wide, free from environmental pollution, non agricultural chemical residuum, to person poultry safety, this agricultural chemicals insect of Long-Time Service can not develop immunity to drugs, its production equipment is simple, and production cost is low.Production practices show, gingko episperm extract control bean aphid worm effect reaches 70%, and control beetle effect reaches 85%, and control twill burglar moth effect reaches 90%, and control cabbage caterpillar, rice borer, cotton aphid effect reach 100%.Control grape powdery mildew, flowers black spot, apple anthracnose, pear scab, peach brown rot effect are all more than 80%.
Microencapsulation of pesticide is exactly utilize microcapsules technology solid, liquid pesticidal etc. to be coated on the small cryptomere preparation formed in cyst material.Microcapsules of Pesticides can be used to reduce agricultural chemicals to the toxicity of people and animals, the range of application etc. that reduces evaporation, extend the lasting period, reduce agricultural chemicals content in the environment, avoid too much poisoning, increase agricultural chemicals.
And also seldom have successful case extraction fromginkgoseed coat and microencapsulation of pesticide combined at present.
Summary of the invention
The present invention is exactly for the problems referred to above, proposes a kind of preparation of extraction fromginkgoseed coat nano-capsule, and these microcapsules all can not produce precipitation and have the good feature of physical and chemical stability in high temperature and low temperature.Said preparation take water as dispersion medium, does not contain or less containing organic solvent, meets current formulations of pesticide developing direction, adapting to the requirement of current agricultural sustainable development.
For reaching above-mentioned technical purpose, present invention employs a kind of preparation of extraction fromginkgoseed coat nano-capsule, comprising the steps:
(1) 0.3g ammonium persulfate (initator) is dissolved in 60g water (divides two parts by 4:1);
(2) 1.5g extraction fromginkgoseed coat is claimed to be dissolved in 21g styrene, 24g butyl acrylate, 0.6g acrylic acid (being liquid) mix monomer;
(3) 18gOP-50,3g lauryl sodium sulfate is dissolved in 150g2% polyvinyl alcohol water solution, puts into container, stir, add the mix monomer being dissolved with extraction fromginkgoseed coat simultaneously, be dispersed into emulsion;
(4) emulsion heating keeps temperature 70 C, adds first part of initator, reacts half an hour, is incubated one hour, obtained seed emulsion; Drip 4.5g styrene, 4.5g butyl acrylate, 3g acrylic acid mix monomer and second part of initator, drip half an hour, be incubated one hour, cooling, adds auxiliary agent discharging.
In the present invention, described auxiliary agent is ethylene glycol.
In the present invention, described auxiliary agent is ethylene glycol and tributyl phosphate mixed aid.
In step of the present invention (3), gelatin can be adopted: sodium alginate=1:2 substitutes polyvinyl alcohol.
In step of the present invention (3), gelatin can be adopted: polyvinyl alcohol=1:2 substitutes polyvinyl alcohol.
The present invention is according to the mechanism of the preparation of pesticide micro capsule; filter out proportioning---the gelatin of good protecting colloid: sodium alginate=1:2; suitable auxiliary agent ratio prepares the nanocapsule formulations of the good extraction fromginkgoseed coat of effect, and these microcapsules all can not produce precipitation and have the good feature of physical and chemical stability in high temperature and low temperature.Said preparation take water as dispersion medium, does not contain or less containing organic solvent, meets current formulations of pesticide developing direction, adapting to the requirement of current agricultural sustainable development.
Accompanying drawing explanation
Shown in Fig. 1 is Fig. 1 Microcapsules Size distribution map in the present invention;
Shown in Fig. 2 is the HPLC spectrogram of Plays product C13:0 of the present invention;
Shown in Fig. 3 is the canonical plotting that in the present invention, reversed-phased high performace liquid chromatographic surveys standard items C13:0;
Shown in Fig. 4 is the HPLC spectrogram of gingko episperm n-hexane extract in the present invention;
Shown in Fig. 5 is the HPLC spectrogram of ginkgoic acid microcapsule formulations in the present invention;
Shown in Fig. 6 be in the present invention extraction fromginkgoseed coat microcapsule formulations variable concentrations to the corrected mortality comparison diagram of diamond-back moth 3 instar larvae;
Embodiment
Embodiment 1
Below in conjunction with the drawings and specific embodiments, the present invention is described in more detail.
First-selection of the present invention needs to carry out water and hangs nano-capsule preparation:
Form by weight: agricultural chemicals: 0.2-5%
Mix monomer: 5-30%
Initator: 0.05-1%
Deionized water: surplus
Additive: 12-25% (preferably)
Next is the screening of emulsifier
(1) CMC (critical micelle concentration)---the minimum emulsifier concentration of micella can be formed
1. with the relation of hydrophobic grouping size: reduce with the increase of hydrophobic grouping carbon number
If 2. alkyl has unsaturated bond, CMC increases
3. on hydrocarbon chain, during polar functionalities, CMC increases
4. when on hydrocarbon chain, hydrogen atom is replaced by fluorine atoms, CMC reduces
5. hydrophilic group is in the middle part of hydrocarbon chain, then CMC is larger
6. ionic emulsifying agent CMC is large compared with nonionic
(2) cloud point
Cloud point is nonionic emulsifier aqueous solution when being heated to uniform temperature, and solution went from clear becomes muddy phenomenon, and be the characteristic parameter of nonionic emulsifier, ionic emulsifying agent does not have cloud point; Cloud point temperature t
c, for positive emulsion polymerisation t
c-t>=10 DEG C. in addition, hydrophilic radical conference causes cloud point to rise.
(3) HLB value
HLB value is large, hydrophily; H-LB value is little, lipophile
(4) three phase point (krafft point)---the characteristic parameter of ionic emulsifying agent
There is true solution, solid, micella three-phase at a certain temperature, this temperature is three phase point simultaneously.In general, three phase point t should be guaranteed during Selective ion mode type emulsifier
klower than reaction temperature and minimum storage temperature t, i.e. t-t
k>=10 DEG C.
A preparation for extraction fromginkgoseed coat nano-capsule, comprises the steps:
(1) 0.3g ammonium persulfate (initator) is dissolved in 60g water (divides two parts by 4:1);
(2) 1.5g extraction fromginkgoseed coat is claimed to be dissolved in 21g styrene, 24g butyl acrylate, 0.6g acrylic acid (being liquid) mix monomer;
(3) 18gOP-50,3g lauryl sodium sulfate is dissolved in 150g2% polyvinyl alcohol water solution, puts into container, stir, add the mix monomer being dissolved with extraction fromginkgoseed coat simultaneously, be dispersed into emulsion;
(4) emulsion heating keeps temperature 70 C, adds first part of initator, reacts half an hour, is incubated one hour, obtained seed emulsion; Drip 4.5g styrene, 4.5g butyl acrylate, 3g acrylic acid mix monomer and second part of initator, drip half an hour, be incubated one hour, cooling, adds auxiliary agent discharging.
In the present invention, described auxiliary agent is ethylene glycol.
In the present invention, described auxiliary agent is ethylene glycol and tributyl phosphate mixed aid.
In step of the present invention (3), gelatin can be adopted: sodium alginate=1:2 substitutes polyvinyl alcohol.
In step of the present invention (3), gelatin can be adopted: polyvinyl alcohol=1:2 substitutes polyvinyl alcohol.
Protectant selection
In vinyl monomer emulsion polymerization systems, animal glue, gelatin, polyvinyl alcohol, polyethylene adjoin the materials such as pyrrolidone, cellulose derivatives, acrylates and all can be used as protecting colloid use, being most widely used especially with polyvinyl alcohol.
Polyvinyl alcohol starts from mid-term nineteen thirties as the application of protecting colloid in vinyl monomer emulsion polymerisation; particularly in the preparation of timber and paper adhesive, the use of protecting colloid can increase emulsion and also be greatly improved in the tack of moistening state, the mechanical property (as: shear strength and yield strength) of film
[60].
Adopting gelatin: the effect that sodium alginate=1:2 substitutes polyvinyl alcohol is best, is secondly gelatin: polyvinyl alcohol=1:2 effect is better, all adopting the effect of polyvinyl alcohol than all adopting gelatin and sodium alginate effective.
The selection of auxiliary agent
The development of China's insecticides adjuvant is from emulsifier research, exploitation.Farm chemical emulgent has the four large classes such as nonionic, anion, cation and zwitterionic surfactant, and the most frequently used is then nonionic, anion or nonionic and anion mixture.Main Types has alkylphenol polyoxyethylene (OPEO-OP, polyoxyethylene nonylphenol ether-NP), Ben-zylphenol Polyoxyethyl Ether (agriculture breast BP, BC), styryl phenol polyethenoxy ether (agriculture breast 600, agriculture breast BS, agriculture breast 1601 and 1602, peaceful newborn No. 32), alkylphenol polyoxyethylene formaldehyde condensation products (Nongru-700 number, peaceful newborn No. 36), castor oil polyoxyethylene ether (BY), fatty alcohol-polyoxyethylene ether (No. 200, agriculture breast), aliphatic alcohol polyethenoxy ester, polyol fatty acid ester and ethylene oxide adduct (Span thereof, Tween series) etc. nonionic surface active agent and alkylbenzenesulfonate (No. 500, agriculture breast, DBS-Ca), fatty alcohol polyoxyethylene ether sulfate (AES).Mainly as emulsification and the dispersion of the emulsion systems such as emulsifiable concentrates for agricultural chemicals, micro emulsion, water and milk, milk powder, suspension emulsion.
The effect adding 0.5g ethylene glycol in the microcapsule formulations finished product that every 20ml obtains is best, and be secondly 0.8g ethylene glycol and 0.2g tributyl phosphate mixed aid, 1.5g ethylene glycol, effect least it is desirable to 1.0g ethylene glycol, and particle diameter is very uneven.
The physical property of microcapsules and sign (can refer to Fig. 1) thereof
The change of size of pesticide micro capsule is larger, but in general requires D
90be less than 50 μm, because the excessive easy blocking spraying equipment of particle diameter, its stability micro-capsule suspension be also greatly affected, easily produce caking and precipitation.Research finds, the principal element affecting microcapsules size distribution has the type, mixing speed etc. of the chemical constitution of emulsification condition, reaction raw materials, polymeric reaction temperature, viscosity, surfactant used.The control of these conditions seems particularly important in the preparation process of microcapsules.Research at present for pesticide micro capsule is also concentrated in these areas mostly.Sign about domain size distribution can be obtained by microscopic examination statistics, also can be surveyed by Malvern Particle Size Analyzer;
Adopt gelatin: the ratio of sodium alginate=1:2 is as the obtained microcapsule formulations grading of protecting colloid at 7 ~ 40 μm, and effect is better.
The mensuration of thermodynamic stability
Test by agricultural chemicals heat storage stability assay method, namely first microcapsule formulations sample to be measured is injected bottle, with cryosel bath, bottle is freezed, and use sealed membrane good seal.The bottle sealed being positioned over temperature is in the constant temperature oven of 54 ± 2 DEG C, takes out after heat storage 14d.Be cooled to room temperature after taking-up, the impurity such as the moisture of bottle outer surface wiped simultaneously and try clean and claim its weight, if the quality of micro-capsule suspension sample to be measured does not change, see and whether can produce flocculent deposit.
Low-temperature stability measures
Test by agricultural chemicals low-temperature stability assay method, get microcapsule formulations sample to be measured and be positioned in 50ml beaker, be positioned in refrigerator and be cooled to 0 DEG C, place and keep Ih, whisk once every 15min, continue 15s at every turn, observe cosmetic variation situation.Then beaker is put back in refrigerator again, keep 0 DEG C of constant temperature to continue to place 7d.After 7d, the beaker that sample is housed is taken out, leaves standstill and return to room temperature.See in temperature return process, whether reagent keeps homogeneous.
The mensuration of microcapsules active ingredient
1 experiment material and method
The preparation of 1.1 ginkgoic acid titers
Precision takes the mono-product 10.0mg of ginkgoic acid C13:0, fully dissolves in constant volume 10mL volumetric flask, be mixed with the contrast solution of 1.0mg/ml, shake up with methyl alcohol, for subsequent use.
The preparation of 1.2 sample solutions
Take 0.1157g ginkgolic acid extract, methyl alcohol dissolves, and is settled to 25mL, shakes up, with the organic filtering with microporous membrane of 0.45um, get filtered fluid and be ginkgolic acid extract sample solution.
Take ginkgo biloba extract microcapsule formulations 0.4765g, with methanol dilution, be settled in 25mL volumetric flask, shake up, with the organic filtering with microporous membrane of 0.45um, get filtered fluid and be ginkgolic acid extract microcapsules sample solution.
Ginkgolic acid analytical method
Adopt high performance liquid chromatography:
Chromatographic column: Waters Xbridge C18 (150mm × 4.6mm, 5 μm);
Mobile phase: methyl alcohol: 3% glacial acetic acid solution (90: 10);
Determined wavelength: 310nm;
Flow velocity: 1mL/min;
Column temperature: 30 DEG C
Ginkgoic acid standard items spectrogram
Adopt high performance liquid chromatography to analyze ginkgoic acid standard items, result, as Fig. 2, shows that total ginkgoic acid can be separated completely under chromatographic condition, and the retention time of ginkgoic acid C13:0 is 15.138min.The mensuration of calibration curve
By the sample liquid of the ginkgoic acid C13:0 standard items of preparation, after organic membrane filtration of 0.45um, sample size 3ul, 5ul, 7ul, 9ul, 11ul, 13ul, measure its peak area.Be calibration curve Fig. 3 with peak area Y (weber) and sample size X (ug), regression equation is Y=0.9481X-0.876, coefficient R
2=0.9993.
The content of ginkgolic acid extract ginkgoic acid
Adopt above-mentioned chromatographic condition to measure the content of ginkgoic acid in gingko episperm n-hexane extract, Fig. 4 is shown in by efficient liquid phase chromatographic analysis collection of illustrative plates, according to document
[62]the computational methods of total ginkgoic acid, show that the content of ginkgoic acid in extract is 35.32%.
The content of ginkgoic acid in microcapsule formulations
Adopt above-mentioned chromatographic condition to measure the content of ginkgoic acid in gingko episperm n-hexane extract microcapsule formulations, Fig. 5 is shown in by efficient liquid phase chromatographic analysis collection of illustrative plates, according to document
[62]the computational methods of total ginkgoic acid, show that the content of ginkgoic acid in extract is 2.22%.
The toxicity test of ginkgo biloba extract microcapsule formulations
Measure the comprehensive virulence of medicament to diamond-back moth and adopt leaching worm leaf dipping method.According to pre-test result, reagent agent is mixed with the aqueous solution of 5 ~ 7 concentration gradients, diamond-back moth third-instar larvae is flooded to the order of high concentration by head by by low concentration, dip time is 5s, the upper unnecessary liquid of polypide is sucked with blotting paper after taking-up, put into the culture dish (Φ 9cm) being covered with filter paper moisturizing, each 10.After having flooded polypide, ready cabbage leaf dish (Φ 1.5cm) is flooded 2 ~ 3s in liquid, has sucked unnecessary liquid with blotting paper after taking-up, dry, put into diamond-back moth process culture dish corresponding with it.Every concentration process repeats 3 times, with clear water process in contrast.Each process culture dish is all placed in incubator, after 72 hours, checks diamondback moth larvae death condition, calculate lethality and corrected mortality.To biologicall test the data obtained, ask virulence regression equation and the lethal concentration of 50 (LC50) of reagent agent with extreme value analysis method.
The mensuration of ginkgoic acid extract insecticidal activity
Get ginkgo biloba extract 2g, preparation variable concentrations gradient solution, adopts 1.1 methods to measure its insecticidal activity.
Data analysis
By Excel and SPSS data processing software analyzing and processing data
Bioassay results
Leaching worm leaf dipping method is adopted to determine 6% extraction fromginkgoseed coat microcapsule formulations to the indoor virulence of diamond-back moth 3 instar larvae, the results are shown in Figure 6, from Fig. 6, can find out that 6% extraction fromginkgoseed coat microcapsule formulations has good insecticidal activity to diamond-back moth 3 instar larvae.After chemicals treatment, 48h shows obvious insecticidal activity, the corrected mortality that each concentration (100mg/L, 200rng/L, 500mg/L, 1000mg/L, 5000mg/L) processes when 48h is respectively 13.3%, 23.3%, 30%, 50%, 66.7%, there is significant difference each other, to 72h, lethality continues to rise, reach 26.7%, 33.3%, 49.4%, 66.7%, 89.3%, between each process, difference is obvious.
As can be seen from the table, ginkgoic acid extract to be processed as after microcapsule formulations the cytotoxicity of diamond-back moth apparently higher than ginkgoic acid extract.This is more conducive to the performance of ginkgoic acid insecticidal activity after illustrating and ginkgoic acid extract being processed as microcapsule formulations.
Claims (5)
1. the preparation of extraction fromginkgoseed coat nano-capsule, is characterized in that, comprises the steps:
(1) 0.3g ammonium persulfate (initator) is dissolved in 60g water (divides two parts by 4:1);
(2) 1.5g extraction fromginkgoseed coat is claimed to be dissolved in 21g styrene, 24g butyl acrylate, 0.6g acrylic acid (being liquid) mix monomer;
(3) 18gOP-50,3g lauryl sodium sulfate is dissolved in 150g2% polyvinyl alcohol water solution, puts into container, stir, add the mix monomer being dissolved with extraction fromginkgoseed coat simultaneously, be dispersed into emulsion;
(4) emulsion heating keeps temperature 70 C, adds first part of initator, reacts half an hour, is incubated one hour, obtained seed emulsion; Drip 4.5g styrene, 4.5g butyl acrylate, 3g acrylic acid mix monomer and second part of initator, drip half an hour, be incubated one hour, cooling, adds auxiliary agent discharging.
2. the preparation of extraction fromginkgoseed coat nano-capsule as claimed in claim 1, it is characterized in that, described auxiliary agent is ethylene glycol.
3. the preparation of extraction fromginkgoseed coat nano-capsule as claimed in claim 1, it is characterized in that, described auxiliary agent is ethylene glycol and tributyl phosphate mixed aid.
4. the preparation of extraction fromginkgoseed coat nano-capsule as claimed in claim 1, is characterized in that, in described step (3), adopts gelatin: sodium alginate=1:2 substitutes polyvinyl alcohol.
5. the preparation of extraction fromginkgoseed coat nano-capsule as claimed in claim 1, is characterized in that, in described step (3), adopts gelatin: polyvinyl alcohol=1:2 substitutes polyvinyl alcohol.
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| CN114053754A (en) * | 2021-11-30 | 2022-02-18 | 南京林业大学 | Two-phase deep eutectic solvent for simultaneously separating and extracting multiple active ingredients from waste ginkgo nut testa and extraction method thereof |
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Cited By (2)
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| CN106538521A (en) * | 2016-10-11 | 2017-03-29 | 常州市鼎日环保科技有限公司 | A kind of preparation method of degradable noresidue fruits and vegetables insecticidal dust |
| CN114053754A (en) * | 2021-11-30 | 2022-02-18 | 南京林业大学 | Two-phase deep eutectic solvent for simultaneously separating and extracting multiple active ingredients from waste ginkgo nut testa and extraction method thereof |
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