CN106644640A - Preparation method and application of pesticide pyraclostrobin supported sample as well as application of pesticide pyraclostrobin supported sample in fluorescent tracing of pathogenic bacteria of asparagus stem blight - Google Patents
Preparation method and application of pesticide pyraclostrobin supported sample as well as application of pesticide pyraclostrobin supported sample in fluorescent tracing of pathogenic bacteria of asparagus stem blight Download PDFInfo
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- CN106644640A CN106644640A CN201611209030.9A CN201611209030A CN106644640A CN 106644640 A CN106644640 A CN 106644640A CN 201611209030 A CN201611209030 A CN 201611209030A CN 106644640 A CN106644640 A CN 106644640A
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- Prior art keywords
- pyraclostrobin
- sample
- agricultural chemicals
- preparation
- load
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Links
- 239000005869 Pyraclostrobin Substances 0.000 title claims abstract description 73
- HZRSNVGNWUDEFX-UHFFFAOYSA-N pyraclostrobin Chemical compound COC(=O)N(OC)C1=CC=CC=C1COC1=NN(C=2C=CC(Cl)=CC=2)C=C1 HZRSNVGNWUDEFX-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 235000005340 Asparagus officinalis Nutrition 0.000 title abstract description 7
- 239000000575 pesticide Substances 0.000 title abstract 8
- 244000052616 bacterial pathogen Species 0.000 title abstract 4
- 244000003416 Asparagus officinalis Species 0.000 title description 4
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000000523 sample Substances 0.000 claims description 69
- 239000003905 agrochemical Substances 0.000 claims description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- 239000012876 carrier material Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- NCZAACDHEJVCBX-UHFFFAOYSA-N [Si]=O.[C] Chemical compound [Si]=O.[C] NCZAACDHEJVCBX-UHFFFAOYSA-N 0.000 claims description 18
- 239000002096 quantum dot Substances 0.000 claims description 17
- 235000014676 Phragmites communis Nutrition 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 238000010926 purge Methods 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 9
- 244000039328 opportunistic pathogen Species 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 241000894006 Bacteria Species 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000012488 sample solution Substances 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000001507 sample dispersion Methods 0.000 claims description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 238000005464 sample preparation method Methods 0.000 claims 5
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000377 silicon dioxide Substances 0.000 abstract description 5
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 241000234427 Asparagus Species 0.000 abstract 3
- 239000003814 drug Substances 0.000 description 24
- 238000002474 experimental method Methods 0.000 description 12
- 239000011148 porous material Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 230000004071 biological effect Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000012738 dissolution medium Substances 0.000 description 4
- 239000003480 eluent Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002574 poison Substances 0.000 description 3
- 231100000614 poison Toxicity 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000233866 Fungi Species 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000007306 functionalization reaction Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 244000052769 pathogen Species 0.000 description 2
- 230000001717 pathogenic effect Effects 0.000 description 2
- 150000003217 pyrazoles Chemical class 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- UXAMZEYKWGPDBI-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)Br(C)(C)C Chemical compound C(CCCCCCCCCCCCCCC)Br(C)(C)C UXAMZEYKWGPDBI-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- CVWONAYPVZHJFE-UHFFFAOYSA-N [C+4].[O-2].[O-2].[Ti+4].[Si+4] Chemical compound [C+4].[O-2].[O-2].[Ti+4].[Si+4] CVWONAYPVZHJFE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- CBMPTFJVXNIWHP-UHFFFAOYSA-L disodium;hydrogen phosphate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].OP([O-])([O-])=O.OC(=O)CC(O)(C(O)=O)CC(O)=O CBMPTFJVXNIWHP-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- -1 pyraclostrobin small molecule Chemical class 0.000 description 1
- 230000003578 releasing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Zoology (AREA)
- Hematology (AREA)
- Environmental Sciences (AREA)
- Wood Science & Technology (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Pest Control & Pesticides (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Biomedical Technology (AREA)
- Urology & Nephrology (AREA)
- Agronomy & Crop Science (AREA)
- Cell Biology (AREA)
- Microbiology (AREA)
- Dispersion Chemistry (AREA)
- Biotechnology (AREA)
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- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Optics & Photonics (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
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Abstract
The invention discloses a preparation method and an application of a pesticide pyraclostrobin supported sample as well as the application of the pesticide pyraclostrobin supported sample in fluorescent tracing of pathogenic bacteria of asparagus stem blight. The preparation method of the pesticide pyraclostrobin supported sample comprises the following steps: (1) preparation of a supporter material: a mesoporous silica carbon quantum dot material is prepared as the supporter material; (2) the pesticide pyraclostrobin is supported on the mesoporous silica carbon quantum dot material, and the pesticide pyraclostrobin supported sample is obtained. The prepared pesticide pyraclostrobin supported system can support and release pyraclostrobin, can be used for inhibiting the pathogenic bacteria of asparagus stem blight and can be applied to fluorescent tracing of the pathogenic bacteria of asparagus stem blight.
Description
Technical field
The present invention relates to agricultural chemicals load applied technical field, more particularly to loads the preparation side of agricultural chemicals pyraclostrobin sample
Method, purposes and its in reed stem wilt opportunistic pathogen fluorescent tracing application.
Background technology
Mesoporous silicon dioxide nano has the mesoporous knot of the peculiar properties such as light, electricity, magnetic, high-sequential and continuously adjustabe control
Structure, big specific surface area, surface functional group is easy to a series of advantages such as modification, excellent biocompatibility, causes people
Extensive concern.Carbon quantum dot is most important one kind in fluorescence carbon nanomaterial, relative to traditional semiconductor-quantum-point and
Organic dyestuff, fluorescent carbon quantum dot has the advantages that little particle diameter, the high and low poison of chemical inertness and is easy to functionalization, is widely used in
Biological medicine research.Carbon quantum dot is entrained on mesoporous silicon oxide, the two respective advantage can be given full play to, as load
Body material, does not have the application report in terms of conveying agricultural chemicals.
The content of the invention
In view of this, the invention reside in providing a kind of preparation method of load agricultural chemicals pyraclostrobin sample so that prepare
Out loading agricultural chemicals pyraclostrobin sample can load and discharge agricultural chemicals pyraclostrobin, can be used to suppress reed stem wilt disease
Opportunistic pathogen, and can be used for fluorescent tracing of the medicine-carried system in reed stem wilt pathogen.
The present invention is achieved through the following technical solutions：
The preparation method of load agricultural chemicals pyraclostrobin sample, comprises the steps：
(1) preparation of carrier material：Mesoporous silicon oxide carbon quantum dot material is prepared as carrier material；
(2) agricultural chemicals pyraclostrobin is supported in mesoporous silicon oxide carbon quantum dot material, agricultural chemicals pyrazoles ether must be loaded
Bacterium ester sample.
The preparation method of above-mentioned load agricultural chemicals pyraclostrobin sample, in step (1), comprises the steps：
(1-1) cetyl trimethylammonium bromide is soluble in water, stirring adds sodium hydroxide solution, heating；
(1-2) tetraethyl orthosilicate, ethyl acetate and 3- aminopropyl-triethoxies are added in the solution obtained to step (1-1)
Silane, stirring；
(1-3) mixed solution obtained in step (1-2) is centrifuged, the solid ethanol purge obtained after centrifugation, then is divided
Dissipate in ethanol, obtain alcohol suspension；
(1-4) saturation hydrochloride aqueous solution, stirring is added to remove cetyl three in the solution obtained to step (1-3)
Methyl bromide ammonium；
(1-5) solution centrifugal that will be obtained in step (1-4), the solid ethanol purge obtained after centrifugation is dried overnight,
It is subsequently placed in Muffle furnace and calcines, obtains mesoporous silicon oxide carbon quantum dot material.
The preparation method of above-mentioned load agricultural chemicals pyraclostrobin sample, in step (1-1)：By cetyl trimethyl bromine
When change ammonium is dissolved in water, cetyl trimethylammonium bromide is 0.2 with the mass volume ratio of water:96g/mL；Sodium hydroxide solution
Concentration is 2mol/L, and cetyl trimethylammonium bromide is 2/7g/mL with sodium hydroxide solution mass volume ratio；By mixed liquor plus
Heat is to 80 DEG C.
The preparation method of above-mentioned load agricultural chemicals pyraclostrobin sample, in step (1-2)：The addition of tetraethyl orthosilicate
It is 2 with the ratio of the addition volume of sodium hydroxide solution:1, the addition of ethyl acetate and the addition body of sodium hydroxide solution
The ratio of product is 3:0.7,3- aminopropyl triethoxysilane is 1 with the ratio of the addition volume of tetraethyl orthosilicate:4；In 80 DEG C of bars
2h is stirred under part；In step (1-3)：With ethanol purge 3 times.
The preparation method of above-mentioned load agricultural chemicals pyraclostrobin sample, in step (1-4)：Saturation hydrochloride aqueous solution
Addition is 40 μ L, and under the conditions of 60 DEG C 3h is stirred.
The preparation method of above-mentioned load agricultural chemicals pyraclostrobin sample, in step (1-5)：The solid that centrifugation is obtained is used
Ethanol purge 2 times, dries overnight under the conditions of 60 DEG C；Then under the conditions of 400 DEG C, it is placed in Muffle furnace and calcines 2h.
The preparation method of above-mentioned load agricultural chemicals pyraclostrobin sample, in step (2), comprises the steps：
(2-1) mesoporous silicon oxide carbon quantum dot material and pyraclostrobin active compound are added in 50mL methyl alcohol, ultrasound；
(2-2) it is centrifuged, and deionized water cleaning lower floor solid；
(2-3) drying load agricultural chemicals pyraclostrobin sample.
The preparation method of above-mentioned load agricultural chemicals pyraclostrobin sample, in step (2-1)：Mesoporous silicon oxide carbon quantum
Point material and pyraclostrobin active compound mass ratio are 1:2；In step (2-2)：Deionized water is cleaned 3 times；In step (2-3)
In：Drying temperature is 40 DEG C.
The preparation method of above-mentioned load agricultural chemicals pyraclostrobin sample, according to above-mentioned preparation method load agricultural chemicals is prepared
Pyraclostrobin sample, load agricultural chemicals pyraclostrobin sample is used to suppress reed stem wilt opportunistic pathogen.
The application of load agricultural chemicals pyraclostrobin sample fluorescent tracing in reed stem wilt opportunistic pathogen, comprises the steps：
(1) obtain loading agricultural chemicals pyraclostrobin sample according to above-mentioned preparation method；
(2) load agricultural chemicals pyraclostrobin sample dispersion being obtained into sample solution in sterilized water, sample concentration is 0.2～
10mg/L processes reed stem wilt opportunistic pathogen mycelium with sample solution, using confocal laser scanning microscope.
The invention has the beneficial effects as follows：
Mesoporous silicon dioxide nano has the mesoporous knot of the peculiar properties such as light, electricity, magnetic, high-sequential and continuously adjustabe control
Structure, big specific surface area, surface functional group is easy to a series of advantages such as modification, excellent biocompatibility.Carbon quantum dot is
Most important one kind in fluorescence carbon nanomaterial, relative to traditional semiconductor-quantum-point and organic dyestuff, with particle diameter it is little, change
The advantages of learning the high and low poison of inertia and be easy to functionalization.The present invention has synthesized the meso-porous titanium dioxide silicon-carbon with embedded carbon quantum dot
Quanta point material, it combines both advantages, can load agricultural chemicals pyraclostrobin, has been successfully set up with photoluminescent property
Nanometer medicine-carried system, have studied releasing properties of the mesoporous silicon oxide carbon quantum dot material under condition of different pH, and in suppression
Bacterium experiment in by the photoluminescent property of carbon quantum dot come spike nanometer medicine-carried system on mycelial impact.
Description of the drawings
Fig. 1 carries the infrared spectrum (Py of medicine sample and carrier material and active compound：Pyraclostrobin active compound；MSN-CDs：It is mesoporous
Silica carbon quantum dot material；MSN-CDs-Py：Pyraclostrobin carries medicine sample)；
The fluorescence spectra of Fig. 2 carrier materials；
The nitrogen adsorption curve of Fig. 3 carrier materials and load medicine sample；
The graph of pore diameter distribution of Fig. 4 carrier materials and load medicine sample；
The thermal gravimetric analysis curve of Fig. 5 carrier materials and load medicine sample and active compound；
The transmission electron microscope picture (A) of Fig. 6-1 carrier materials；
The scanning electron microscope (SEM) photograph (B) of Fig. 6-2 carrier materials；
Fig. 7-1 carries the transmission electron microscope picture (A) of medicine sample；
Fig. 7-2 carries the scanning electron microscope (SEM) photograph (B) of medicine sample；
The atomic force microscopy diagram of Fig. 8 carrier materials；
The release profiles of sample under Fig. 9 condition of different pH；
Figure 10 1 is withered for the asparagus stem of CK groups；2 is withered to carry the asparagus stem of medicine sample treatment, wherein A- fluorograms；B- light fields
Figure；The stacking chart of C- fluorescence and light field.
Specific embodiment
For the scheme in the clear explanation present invention, preferred embodiment is given below and is described with reference to the accompanying drawings.
The present embodiment loads the preparation method of agricultural chemicals pyraclostrobin sample, comprises the steps：
(1) preparation of carrier material：Mesoporous silicon oxide carbon quantum dot material is prepared as carrier material；
(1-1) cetyl trimethylammonium bromide is soluble in water, stirring adds sodium hydroxide solution, heating；By 16
When alkyl trimethyl ammonium bromide is dissolved in water, cetyl trimethylammonium bromide is 0.2 with the mass volume ratio of water:96g/mL；Hydrogen
The concentration of sodium hydroxide solution is 2mol/L, and cetyl trimethylammonium bromide is 2/7g/ with sodium hydroxide solution mass volume ratio
mL；Mixed liquor is heated into 80 DEG C.
(1-2) tetraethyl orthosilicate, ethyl acetate and 3- aminopropyl-triethoxies are added in the solution obtained to step (1-1)
Silane, stirring；The addition of tetraethyl orthosilicate is 2 with the ratio of the addition volume of sodium hydroxide solution:1, ethyl acetate plus
It is 3 to enter amount with the ratio of the addition volume of sodium hydroxide solution:0.7,3- aminopropyl triethoxysilane and tetraethyl orthosilicate
The ratio of addition volume is 1:4；2h is stirred under the conditions of 80 DEG C.
(1-3) mixed solution obtained in step (1-2) is centrifuged, the solid obtained after centrifugation ethanol purge 3 times, then
In being scattered in ethanol, alcohol suspension is obtained.
(1-4) 40 μ L saturation hydrochloride aqueous solutions are added in the solution obtained to step (1-3), is stirred under the conditions of 60 DEG C
3h, removes cetyl trimethylammonium bromide.
(1-5) solution centrifugal that will be obtained in step (1-4), the solid obtained after centrifugation ethanol purge 2 times, at 60 DEG C
Under the conditions of dry overnight, be then placed in Muffle furnace under the conditions of 400 DEG C and calcine 2h, obtain mesoporous silicon oxide carbon quantum dot material
Material.
(2) agricultural chemicals pyraclostrobin is supported in mesoporous silicon oxide carbon quantum dot material, agricultural chemicals pyrazoles ether must be loaded
Bacterium ester sample.
(2-1) mesoporous silicon oxide carbon quantum dot material and pyraclostrobin active compound are added in 50mL methyl alcohol, ultrasound；
Mesoporous silicon oxide carbon quantum dot material and pyraclostrobin active compound mass ratio are 1:2.
(2-2) it is centrifuged, and deionized water cleaning lower floor solid, deionized water cleaning 3 times.
(2-3) drying load agricultural chemicals pyraclostrobin sample, drying temperature is 40 DEG C.
The present embodiment preparation method prepares load agricultural chemicals pyraclostrobin sample, can be used to suppress reed stem wilt former
Bacterium.
Load agricultural chemicals pyraclostrobin sample dispersion manufactured in the present embodiment is obtained into sample solution, sample in sterilized water
Concentration is 0.2～10mg/L, and with sample solution reed stem wilt opportunistic pathogen mycelium is processed, and is seen using laser confocal microscope
Examine.
The property representation of mesoporous silicon oxide carbon quantum dot material manufactured in the present embodiment, load agricultural chemicals pyraclostrobin sample
The property representation of product and the test by the photoluminescent property of carbon quantum dot come spike nanometer medicine-carried system on mycelial impact
As follows (in herein below, mesoporous silicon oxide carbon quantum dot material is referred to as carrier material, loads agricultural chemicals medicine pyraclostrobin sample
Referred to as carry medicine sample)：
(1) drugloading rate and entrapment efficiency determination are tested
Load medicine sample is weighed, methanol solution is added, the pyraclostrobin agricultural chemicals in ultrasound wash-out load is carried out, every time ultrasound
40min, draws after centrifugation and continue after the eluent of upper strata ultrasound wash-out, co-elute 5 times, merges the eluent that obtains, constant volume in
In the volumetric flask of 25mL, the eluent of 1mL is drawn with pipettor, after crossing 0.22 μm of organic system filter membrane, enter high performance liquid chromatography
The content of pyraclostrobin in detection eluent.Calculate the drugloading rate and envelop rate for carrying medicine sample respectively according to formula.
Wherein, test result indicate that, carry medicine sample drugloading rate be 12.98% ± 0.95, envelop rate is 15.90%.
(2) infrared experiment
By the infared spectrum shown in Fig. 1, pyraclostrobin is 1546,1481 and 1358cm-1The characteristic peak at place is equal
Can see on medicine sample is carried, illustrate that pyraclostrobin has successfully been loaded on a support material.And be located at 1088,966,804,
467cm-1The characteristic peak at place is the functional group of carrier material.
(3) fluorescence spectrum experiments
Carrier material is weighed, with ultra-pure water the suspension that concentration is 1mg/mL is configured to, using XRF it is surveyed
Photoluminescent property.By the fluorogram shown in Fig. 2, under the conditions of excitation wavelength is 360nm, carrier material is at 448nm
Launch wavelength under have absworption peak, it was demonstrated that the material has photoluminescent property.
(4) specific surface area and pore size determination
The specific surface area of carrier material can be characterized with aperture by Brunauer-Emmett-Teller (BET) methods.
It can be seen from nitrogen adsorption-desorption isothermal curve shown in Fig. 3, the thermoisopleth of carrier material meets typical VI thermoisopleths spy
Levy, illustrate that carrier material has meso-hole structure, the analysis result that the conclusion is tested with transmission electron microscope is consistent.Calculate according to BET method
The specific surface area of the carrier material for drawing is 433.10m2/ g, and the specific surface area for carrying medicine sample is only 190.66m2/ g, thus
Can illustrate that pyraclostrobin has successfully been carried on carrier material.(schemed by carrier material and the pore size distribution curve for carrying medicine sample
4) understand, the average pore size of carrier material is 4.82nm, belongs to mesoporous category；And the average pore size for carrying medicine sample is 6.57nm,
More than the average pore size of carrier material, it may be possible to because most of mesoporous on carrier is occupied by pyraclostrobin small molecule, from
And cause average pore size to increase.
(5) thermogravimetric analysis experiment
Thermogravimetric analysis experiment is carried out to carrier material, load medicine sample and pyraclostrobin active compound using thermogravimetric analyzer, such as
Shown in Fig. 5.
(6) microscopic appearance
Appropriate sample is weighed, after being disperseed with ultra-pure water, ESEM and transmission electron microscope observing is carried out after sample preparation.By Fig. 6-
1st, Fig. 6-2, Fig. 7-1 and Fig. 7-2 can be seen that carrier material is the smooth spheric granules in surface, and uniform in size, and average grain diameter is
180 ± 6nm, and the particle diameter of medicine sample is carried compared with carrier material, particle diameter increases little.
(7) AFM experiments
Take carrier material to be scattered in ethanol, draw one and drip hanging drop on the mica sheet for processing, treat that solvent volatilizees
After dry, sample strip is placed on monitor station carries out atomic force microscope observation.As shown in figure 8, i.e. the atomic force of carrier material shows
Micro mirror figure, can draw the statistical distribution of the Terrain Elevation of carrier material in figure, and it can be seen that carrier material is surface
Smooth is spherical, and this is consistent with the experimental result of ESEM.
(8) release experiment
Release experiment is carried out using Bag filter method.Intercepted length is 7cm, and molecular cut off is 12000 bag filter, is added
The sample of 5ml dissolution mediums is dissolved in, whole bag filter is placed in the dissolution medium of 200ml, on 200rpm, the shaking table of room temperature
Carry out release experiment.Per at regular intervals, after sampling 1ml, after crossing 0.22 μm of water system filter membrane, enter high performance liquid chromatography detection
The amount of the pyraclostrobin for discharging.After per sub-sampling, the dissolution medium of 1ml is added.Calculated according to formula and carry medicine sample
Accumulative release rate.
Wherein, V:Each sample volume, 1ml；Ci:The concentration of i ＆ lt sampling, mg/ml；V0:The totality of dissolution medium
Product, 200ml；Cn:The concentration of n-th sampling, mg/ml；m:Carry the quality of pyraclostrobin in medicine sample, mg.
Dissolution medium (volume fraction)：The Tween-80 of cushioning liquid+0.5% of the difference pH of 30% ethanol+70%.
The cushioning liquid of pH=5.0 and 7.0 is prepared by disodium hydrogen phosphate-citric acid, and the cushioning liquid of pH=9.0 is by sweet ammonia
Acid and NaOH are prepared.
(9) biological activity determination experiment：
Weigh carrier material, carry medicine sample and pyraclostrobin active compound, in being scattered in sterilized water, be made into mother liquor, carry out reed
The withered fungi Inhibition test of bamboo shoot stem.Biological activity determination experiment is carried out using band poison flat band method, mother liquor is diluted to quantitative PDA
A series of different concentration, respectively 0.2,0.5,1,2,5, the sample concentration that added of 10ppm, i.e. flat board it is different, connect bacteria cake
After carry out biological activity determination experiment.The growth diameter of bacterium colony is recorded per 24h, different samples are calculated to asparagus stem according to formula
Withered inhibiting rate.
Result of the test is as shown in Figure 9.
(10) fluorescence experiments that medicine sample is acted on fungi are carried
The mycelium crossed by sample treatment during biological activity determination is tested takes out a fritter, and sample preparation is placed in laser copolymerization
Observe under focusing microscope, result of the test is as shown in Figure 10.
Above-described embodiment is only intended to clearly illustrate the invention example, and not has to the invention
The restriction of body embodiment.For those of ordinary skill in the field, can also make on the basis of the above description
The change or variation of other multi-forms.There is no need to be exhaustive to all of embodiment.It is all the present invention
Spirit and principle within extend out it is any obvious change or variation still in the invention claim guarantor
Among shield scope.
Claims (10)
1. the preparation method of agricultural chemicals pyraclostrobin sample is loaded, it is characterised in that comprised the steps：
(1) preparation of carrier material：Mesoporous silicon oxide carbon quantum dot material is prepared as carrier material；
(2) agricultural chemicals pyraclostrobin is supported in mesoporous silicon oxide carbon quantum dot material, agricultural chemicals pyraclostrobin must be loaded
Sample.
2. the preparation method of agricultural chemicals pyraclostrobin sample is loaded, it is characterised in that in step (1), comprised the steps：
(1-1) by cetyl trimethylammonium bromide in water, stirring adds sodium hydroxide solution, heating；
(1-2) tetraethyl orthosilicate, ethyl acetate and 3- aminopropyl-triethoxy silicon are added in the solution obtained to step (1-1)
Alkane, stirring；
(1-3) mixed solution obtained in step (1-2) is centrifuged, the solid ethanol purge obtained after centrifugation is redispersed in
In ethanol, alcohol suspension is obtained；
(1-4) saturation hydrochloride aqueous solution, stirring is added to remove cetyl trimethyl in the solution obtained to step (1-3)
Ammonium bromide；
(1-5) overnight, then the solution centrifugal that will be obtained in step (1-4), the solid ethanol purge obtained after centrifugation dries
It is placed in Muffle furnace and calcines, obtains mesoporous silicon oxide carbon quantum dot material.
3. it is according to claim 2 load agricultural chemicals pyraclostrobin sample preparation method, it is characterised in that in step
(1-1) in：When cetyl trimethylammonium bromide is dissolved in into water, cetyl trimethylammonium bromide is with the mass volume ratio of water
0.2:96g/mL；The concentration of sodium hydroxide solution is 2mol/L, cetyl trimethylammonium bromide and sodium hydroxide solution quality
Volume ratio is 2/7g/mL；Mixed liquor is heated into 80 DEG C.
4. it is according to claim 3 load agricultural chemicals pyraclostrobin sample preparation method, it is characterised in that in step
(1-2) in：The addition of tetraethyl orthosilicate is 2 with the ratio of the addition volume of sodium hydroxide solution:1, the addition of ethyl acetate
Amount is 3 with the ratio of the addition volume of sodium hydroxide solution:0.7,3- aminopropyl triethoxysilane adds with tetraethyl orthosilicate
The ratio for entering amount volume is 1:4；2h is stirred under the conditions of 80 DEG C；In step (1-3)：With ethanol purge 3 times.
5. it is according to claim 4 load agricultural chemicals pyraclostrobin sample preparation method, it is characterised in that in step
(1-4) in：The addition of saturation hydrochloride aqueous solution is 40 μ L, and under the conditions of 60 DEG C 3h is stirred.
6. it is according to claim 5 load agricultural chemicals pyraclostrobin sample preparation method, it is characterised in that in step
(1-5) in：By the solid that obtains of centrifugation ethanol purge 2 times, dry overnight under the conditions of 60 DEG C；Then under the conditions of 400 DEG C,
It is placed in Muffle furnace and calcines 2h.
7. according to the preparation method of the arbitrary described load agricultural chemicals pyraclostrobin sample of claim 1-6, it is characterised in that
In step (2), comprise the steps：
(2-1) mesoporous silicon oxide carbon quantum dot material and pyraclostrobin active compound are added in 50mL methyl alcohol, ultrasound；
(2-2) it is centrifuged, and deionized water cleaning lower floor solid；
(2-3) drying load agricultural chemicals pyraclostrobin sample.
8. it is according to claim 7 load agricultural chemicals pyraclostrobin sample preparation method, it is characterised in that in step
(2-1) in：Mesoporous silicon oxide carbon quantum dot material and pyraclostrobin active compound mass ratio are 1:2；In step (2-2)：
Deionized water is cleaned 3 times；In step (2-3)：Drying temperature is 40 DEG C.
9. the purposes of agricultural chemicals pyraclostrobin sample is loaded, it is characterised in that according to the arbitrary described preparation side of claim 1-8
Method prepares load agricultural chemicals pyraclostrobin sample, and load agricultural chemicals pyraclostrobin sample is used to suppress reed stem wilt former
Bacterium.
10. the application of agricultural chemicals pyraclostrobin sample fluorescent tracing in reed stem wilt opportunistic pathogen is loaded, it is characterised in that included
Following steps：
(1) obtain loading agricultural chemicals pyraclostrobin sample according to the arbitrary described preparation method of claim 1-8；
(2) load agricultural chemicals pyraclostrobin sample dispersion being obtained into sample solution in sterilized water, sample concentration is 0.2～
10mg/L, processes reed stem wilt opportunistic pathogen mycelium, using confocal laser scanning microscope with sample solution.
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| CN109805021A (en) * | 2019-02-11 | 2019-05-28 | 中南大学 | A kind of nano pesticide and its preparation method and application of pH regulation |
| CN109964942A (en) * | 2019-04-11 | 2019-07-05 | 中国农业科学院植物保护研究所 | A kind of load medicine particle and preparation method thereof |
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| CN114027297B (en) * | 2021-11-10 | 2023-09-29 | 山东农业大学 | Intelligent silicon dioxide nano pesticide for preventing and treating pine wilt |
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