CN105494431B - A kind of lipopeptid-nano-titanium dioxide compound formulation and its preparation method and application - Google Patents
A kind of lipopeptid-nano-titanium dioxide compound formulation and its preparation method and application Download PDFInfo
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- CN105494431B CN105494431B CN201510991377.2A CN201510991377A CN105494431B CN 105494431 B CN105494431 B CN 105494431B CN 201510991377 A CN201510991377 A CN 201510991377A CN 105494431 B CN105494431 B CN 105494431B
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- 239000000203 mixture Substances 0.000 title claims abstract description 72
- 238000009472 formulation Methods 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910001868 water Inorganic materials 0.000 claims abstract description 49
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 241000196324 Embryophyta Species 0.000 claims abstract description 36
- 230000001580 bacterial effect Effects 0.000 claims abstract description 24
- 230000012010 growth Effects 0.000 claims abstract description 12
- -1 nano-titanium dioxide compound Chemical class 0.000 claims abstract description 6
- 230000001737 promoting effect Effects 0.000 claims abstract description 4
- 238000000855 fermentation Methods 0.000 claims description 57
- 230000004151 fermentation Effects 0.000 claims description 57
- 239000007788 liquid Substances 0.000 claims description 51
- 239000000843 powder Substances 0.000 claims description 46
- 240000003768 Solanum lycopersicum Species 0.000 claims description 39
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 33
- 238000001556 precipitation Methods 0.000 claims description 32
- 239000011573 trace mineral Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 20
- 239000010936 titanium Substances 0.000 claims description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- 235000013619 trace mineral Nutrition 0.000 claims description 17
- 238000004458 analytical method Methods 0.000 claims description 15
- 241000193744 Bacillus amyloliquefaciens Species 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 11
- 239000002609 medium Substances 0.000 claims description 11
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 10
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 244000068988 Glycine max Species 0.000 claims description 6
- 235000010469 Glycine max Nutrition 0.000 claims description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 5
- 229910052564 epsomite Inorganic materials 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 5
- 235000019698 starch Nutrition 0.000 claims description 5
- 239000008107 starch Substances 0.000 claims description 5
- 230000003519 ventilatory effect Effects 0.000 claims description 5
- 239000012138 yeast extract Substances 0.000 claims description 5
- 239000001963 growth medium Substances 0.000 claims description 3
- 150000008547 L-phenylalanines Chemical class 0.000 claims description 2
- 210000004209 hair Anatomy 0.000 claims description 2
- 235000007688 Lycopersicon esculentum Nutrition 0.000 abstract description 32
- 230000000694 effects Effects 0.000 abstract description 14
- 230000009471 action Effects 0.000 abstract description 3
- 241000227653 Lycopersicon Species 0.000 abstract 3
- 238000012545 processing Methods 0.000 description 19
- 238000002474 experimental method Methods 0.000 description 15
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 description 15
- 241000894006 Bacteria Species 0.000 description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 14
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 14
- 150000003839 salts Chemical class 0.000 description 14
- 229910052719 titanium Inorganic materials 0.000 description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 12
- 201000010099 disease Diseases 0.000 description 12
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 12
- 229910052927 chalcanthite Inorganic materials 0.000 description 11
- 229910052603 melanterite Inorganic materials 0.000 description 11
- 244000052769 pathogen Species 0.000 description 10
- 230000001717 pathogenic effect Effects 0.000 description 10
- 239000002244 precipitate Substances 0.000 description 9
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 9
- 229910000368 zinc sulfate Inorganic materials 0.000 description 9
- 239000011686 zinc sulphate Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 239000001103 potassium chloride Substances 0.000 description 6
- 235000011164 potassium chloride Nutrition 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000004913 activation Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000002265 prevention Effects 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 4
- 241000589771 Ralstonia solanacearum Species 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 230000002401 inhibitory effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 208000024891 symptom Diseases 0.000 description 4
- 239000007836 KH2PO4 Substances 0.000 description 3
- 108010028921 Lipopeptides Proteins 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 3
- 244000144992 flock Species 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000001935 peptisation Methods 0.000 description 3
- 108090000765 processed proteins & peptides Proteins 0.000 description 3
- 238000002390 rotary evaporation Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 241000193830 Bacillus <bacterium> Species 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 229910003077 Ti−O Inorganic materials 0.000 description 2
- 229910003088 Ti−O−Ti Inorganic materials 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000012620 biological material Substances 0.000 description 2
- 239000003876 biosurfactant Substances 0.000 description 2
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 235000013877 carbamide Nutrition 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 235000019691 monocalcium phosphate Nutrition 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 229960005190 phenylalanine Drugs 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 1
- 108010062877 Bacteriocins Proteins 0.000 description 1
- 241000726221 Gemma Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 108010093096 Immobilized Enzymes Proteins 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 239000012901 Milli-Q water Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropyl alcohol Natural products CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 description 1
- 241000813090 Rhizoctonia solani Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- 230000001857 anti-mycotic effect Effects 0.000 description 1
- 239000002543 antimycotic Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000001408 fungistatic effect Effects 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000008223 sterile water Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- 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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
-
- 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
- A01N63/00—Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
- A01N63/10—Animals; Substances produced thereby or obtained therefrom
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
Abstract
The invention discloses lipopeptid nano-titanium dioxide compound formulations, which is characterized in that said preparation includes the component of following mass percent：Lipopeptid 0.075%~0.15%, nano-titanium dioxide 0.2%~0.3%, Zn2+0.0069%~0.0092%, Fe2+0.005%~0.007%, Cu2+0.0052%~0.0091% and Mn2+0.005%~0.0083%, remaining is water.Application the invention also discloses the preparation method of above-mentioned lipopeptid nano-titanium dioxide compound formulation and its in control of plant bacterial wilt and in promoting tomato plant strain growth.Lipopeptid nano-titanium dioxide compound formulation prepared by the present invention, can improve the stability of lipopeptid, extend the action time of lipopeptid after the combination of nano-titanium dioxide and lipopeptid, to the preferable control effect that has of bacterial wilt of tomato, and can promote tomato plant strain growth.
Description
Technical field
The invention belongs to microbial pesticide preparation field, be related to a kind of lipopeptid-nano-titanium dioxide compound formulation and its
Preparation method and application.
Background technology
Bacterial wilt of tomato is that a kind of whole world caused by Ralstonia solanacearum (Ralstonia solanacearum) is wide
The bacillary soil-borne disease of general distribution.The petiole appearance of early stage, plant lower blade is sagging, and rear blade is withered gradually,
There is adventitious root in stem simultaneously, and plant is quickly wilted simultaneously gradually withered.The light then underproduction 20%~40%, up to 60% or more when serious
Even have no harvest.There are larger hereditary variations for Ralstonia solanacearum, there is no effective chemical prevention and control method at present.Common prevention
Measure such as resistance breeding, field removing, shift of crops, integrated management etc. due to bacterial wilt disease system complexity and effect very
It is micro-.
Bacillus (Bacillus spp.) has complicated physiological characteristics diversity and substrate diversity, can produce
Raw high patience gemma and various antibacterial substances such as polypeptide and lipopeptid class and bacteriocin class antibiotic.Lipopeptide surfactant is made
For a kind of biosurfactant (biosurfactant), permeability of cell membrane can be changed, the antimycotic and suppression with wide spectrum
The activity of part bacterium processed, studies have shown that certain lipopeptid substance Rhizoctonia solanis and Ralstonia solanacearum show good antagonism
Activity can utilize its to prevent bacterial wilt, but its chemical instability, physics and enzyme unstability limit lipopeptid class table
The development and application of face activating agent Related product.Meanwhile higher production cost and lower yield also limit the work of lipopeptid
Industry metaplasia is produced.
In recent years, interaction prepares composite wood between biomaterial and organic film, organic granular, inorganic clay material
Material has caused the abundant novel, heat of sizable interest, especially inorganic nano submicron order material structure surely in academia
Qualitative excellent, surface-active is adjustable, cheap, biomaterial and inorganic nano material it is effective compound, can tie up very well
Hold the structure of large biological molecule, and it is possible to can assign biological substance new excellent specific property.Nano-titanium dioxide has many
Excellent physics and chemical characteristic, such as high-specific surface area, more surface atoms and good stability, can be used as albumen
The carrier of matter, pesticide, insecticide, and being capable of fixing metal ions.Nano-titanium dioxide is capable of providing a suitable micro-loop
Border maintains the bioactivity and stability of fixed enzyme and protein with immobilized enzyme and other protein.It is related studies have shown that
Nano-titanium dioxide has certain inhibiting effect for bacterial growth, in addition, nano-titanium dioxide can also promote plant to give birth to
It is long.
Trace element is required for plant, studies have shown that foliage-spray liquid microelement can be to the growth of plant
Some positive effects are played with yield.
Invention content
The technical problem to be solved in the invention is to provide a kind of lipopeptid-nano-titanium dioxide compound formulation.
The present invention also technical problems to be solved are to provide the preparation side of above-mentioned lipopeptid-nano-titanium dioxide compound formulation
Method.
The present invention also wants technical problems to be solved to be to provide above-mentioned lipopeptid-nano-titanium dioxide compound formulation to prevent
Application in bacterial wilt of tomato.
The last technical problems to be solved of the present invention are to provide above-mentioned lipopeptid-nano-titanium dioxide compound formulation and are promoting
Application on tomato plant strain growth.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of lipopeptid-nano-titanium dioxide compound formulation, said preparation include the component of following mass percent：
Lipopeptid 0.075%~0.15%；
Nano-titanium dioxide 0.2%~0.3%；
Trace elements zn2+0.0069%~0.0092%, Fe2+0.005%~0.007%, Cu2+0.0052%~
0.0091% and Mn2+0.005%~0.0083%；
Remaining is water.
Wherein, the lipopeptid is prepared as follows to obtain：
(1a) activates bacillus amyloliquefaciens, obtains seed liquor；The bacillus amyloliquefaciens of all energy fermenting and producing lipopeptids
It may be used to the lipopeptid in the production present invention, it is common preferably by China Committee for Culture Collection of Microorganisms in of the invention
The Bacillus amyloliquefaciens strain XZ-173 of microorganism center preservation, preserving number are CGMCC No.4160, the specific letter of the bacterial strain
Breath discloses in the Chinese patent application No. is 201010608579.1；
The method of specific activation bacillus amyloliquefaciens is as follows：By the Bacillus amyloliquefaciens strain of freezing in LB
Flat lining out is placed in activation in 30 DEG C of incubators, and picking single bacterium colony is inoculated in LB liquid medium, at 30 DEG C, 170rpm's
Under the conditions of cultivate for 24 hours, obtain fermentation seed liquid；
Seed liquor is transferred in fermentation medium by (1b), is adjusted relative humidity in fermentation tank and is more than 80%, fermentation production fat
Peptide；
(1c) after fermentation, the mixture that fermentation is obtained is with water according to according to 1g：10mL ratios are uniformly mixed, from
The heart collects supernatant, and it is 1~3 to adjust supernatant pH with hydrochloric acid, stands, then centrifuge, collects precipitation, and precipitation is extracted with dichloromethane,
Rotate removal dichloromethane again, residue water dissolution and to adjust pH be 7.0 is finally freeze-dried to obtain lipopeptid powder.
Wherein, the nano-titanium dioxide is prepared as follows to obtain：
(2a) titanium sulfate is soluble in water by the concentration of 0.1mol/L, and the ammonia spirit of 2~3mol/L is added, makes the pH of solution
It is 6~8, obtains mixture；
(2b) centrifuges mixture, collects precipitation, precipitation is washed with water；
The precipitation that step (2b) obtains is dispersed in water by (2c), and the aqueous hydrogen peroxide solution that volume ratio is 30% is added,
Make Ti in solution4+And H2O2Molar ratio be 1：3~5, it stirs evenly, stands 15~20 hours, obtain peroxo titanic acid sol；
Peroxo titanic acid sol is formed xerogel by (2d) in 60~75 DEG C of drying, by xerogel grind into powder, 400~
It is calcined 1~2 hour under the conditions of 600 DEG C, obtains nano titanium dioxide powder.
Wherein, the nano-titanium dioxide grain size is 10~40nm.
Titanium dioxide have large specific surface area, adsorption capacity is strong, stability is good and the skin effect of other nanometer materials,
Surface has many activated centres, can be effectively combined together lipopeptid and trace element ion using titanium dioxide, very well
Ground maintains the structure of lipopeptid, improves the stability of trace element ion, and has preferably played the biological nature of lipopeptid.
Wherein, the trace element is Zn2+Salt, Fe2+Salt, Cu2+Salt and Mn2+Any one or a few mixed in salt
Close object.
The Zn2+Salt, Fe2+Salt, Cu2+Salt and Mn2+Salt can be the sulfate, nitrate or hydrochloride of above-mentioned ion
Deng preferably sulfuric acid salt.
Preferably, the trace element is Zn2+Salt, Fe2+Salt, Cu2+Salt and Mn2+The mixture of salt, the Zn2+
Salt, Fe2+Salt, Cu2+Salt and Mn2+The preferred ZnSO of mixture of salt4、FeSO、CuSO4And MnSO4Mixture, further preferably
ZnSO4·7H2O、FeSO4·7H2O、CuSO4·5H2O and MnSO4·H2The content of O distinguish 0.3~0.4g/L, 0.25~
The mixture of 0.35g/L, 0.2~0.35g/L and 0.15~0.25g/L, most preferably ZnSO4·7H2O、FeSO4·7H2O、
CuSO4·5H2O and MnSO4·H2The content of O is the mixture of 0.35g/L, 0.3g/L, 0.24g/L and 0.18g/L.
The preparation method of above-mentioned lipopeptid-nano-titanium dioxide compound formulation, this method comprises the following steps：
(1) preparation of lipopeptid：
(1a) activates bacillus amyloliquefaciens, obtains seed liquor；
Seed liquor is transferred in fermentation medium by (1b), is adjusted relative humidity in fermentation tank and is more than 80%, fermentation production fat
Peptide；
(1c) after fermentation, the mixture that fermentation is obtained is with water according to 1g：10mL ratios are uniformly mixed, and are centrifuged, and are received
Collect supernatant, it is 1~3 to adjust supernatant pH with hydrochloric acid, and it is to stand 12h at 2,4 DEG C, then centrifuge preferably to adjust pH, collects precipitation, sinks
Shallow lake is extracted with dichloromethane, then rotates removal dichloromethane, residue water dissolution and adjust pH be 7.0, be finally freeze-dried
Lipopeptid powder；
(2) preparation of nano-titanium dioxide：
(2a) titanium sulfate is soluble in water by the concentration of 0.1mol/L, and the ammonia spirit of 2~3mol/L is added, makes the pH of solution
It is 6~8, preferably adjusts the pH of solution and obtain mixture for 7；
(2b) centrifuges mixture, collects precipitation, precipitation is washed with water；
The precipitation that step (2b) obtains is dispersed in water by (2c), and the aqueous hydrogen peroxide solution that volume ratio is 30% is added,
Make Ti in solution4+And H2O2Molar ratio be 1：3~5, Ti4+And H2O2Molar ratio be preferably 1:4, it stirs evenly, standing 15~
20 hours, time of repose was preferably 15h, obtains peroxo titanic acid sol；
Peroxo titanic acid sol is dried at 60~75 DEG C and forms xerogel by (2d), and drying formation is dry solidifying preferably at 75 DEG C
Xerogel grind into powder is calcined 1~2 hour under the conditions of 400~600 DEG C, preferably calcines 1h under the conditions of 500 DEG C by glue,
Obtain nano titanium dioxide powder；
(3) preparation of liquid microelement：Trace element is dissolved in the water, trace element water-soluble liquid is obtained；
(4) lipopeptid-nano-titanium dioxide compound formulation obtains：In the trace element water-soluble liquid obtained to step (3), successively
Step (1) obtained lipopeptid is added and nano-titanium dioxide that step (2) obtains, stirring shakes up, 20~40 DEG C, 150~
Under the conditions of 250rpm, 10~30h is vibrated, preferably 30 DEG C, 170rpm oscillations are for 24 hours to get to the compound system of lipopeptid-nano-titanium dioxide
Agent.
In step (1b), equal proportion is prepared the fermentation medium as follows：Weigh 4.5~6kg Huangs
Bean powder, 3~4.5kg stalks, 0.15~0.2kg starch and 0.15~0.2kg yeast extracts, are put into fermentation tank, and addition 1~
2L inorganic salt solutions, it is 7~8 to adjust pH, and the moisture content for adjusting culture medium is 40%~60%, and the inorganic salt solution is matched
Fang Wei：1.0g/L KH2PO4、0.5g/L MgSO4·7H2O、0.5g/L KCl、2×10-3G/L L-phenylalanines, 5 × 10-3g/
L MnSO4、0.16×10-3g/L CuSO4、0.15×10-3g/L FeSO4。
In step (1b), fermentation process use temperature-variable fermentation, during the fermentation keep ventilatory capacity be 0.1~0.5vvm,
Tank pressure is 0.01~0.05Mpa, and first stage fermentation temperature is 25~40 DEG C, fermentation 20~for 24 hours, and the fermentation temperature of second stage
It is 28~40 DEG C, fermentation 16~for 24 hours, and ensure that the temperature of second stage fermentation is 0~7 DEG C higher than first stage temperature；It is preferred that
It first ferments at 30 DEG C for 24 hours, then ferment at 37 DEG C 20h.
In step (3), Preferable scheme is that by ZnSO4·7H2O、FeSO4·7H2O、CuSO4·5H2O and MnSO4·H2O
By following concentration it is soluble in water：0.3~0.4g/L ZnSO4·7H2O, 0.25~0.35g/L FeSO4·7H2O, 0.2~
0.35g/LCuSO4·5H2O and 0.15~0.25g/LMnSO4·H2O, most preferably by ZnSO4·7H2O、FeSO4·7H2O、
CuSO4·5H2O and MnSO4·H2O's is soluble in water by following concentration：0.35g/L ZnSO4·7H2O、0.3g/L FeSO4·
7H2O、0.24g/L CuSO4·5H2O and 0.18g/L MnSO4·H2O。
The protection model applied in the present invention of the above-mentioned lipopeptid-nano-titanium dioxide compound formulation in control of plant bacterial wilt
Within enclosing.
The protection applied in the present invention of the above-mentioned lipopeptid-nano-titanium dioxide compound formulation on promoting tomato plant strain growth
Within the scope of.
Advantageous effect：
1, it is detected by infrared spectrum, nano-titanium dioxide prepared by the present invention is effectively tied with lipopeptid and trace element ion
It is combined, not only maintains the structure of lipopeptid well, improve the stability of trace element ion, and preferably play
The biological nature of lipopeptid.Experiments have shown that lipopeptid provided by the invention-nano-titanium dioxide compound formulation is to bacterial wilt of tomato
Control effect is micro- obviously higher than trace element solution, lipopeptid-trace element complex liquid or nano-titanium dioxide-is used alone
Secondary element complex liquid illustrates that the combination of nano-titanium dioxide and lipopeptid in lipopeptid-nano-titanium dioxide compound formulation can be more preferable
Ground improves the stability of lipopeptid, extends the action time of lipopeptid, the lipopeptid-nano-titanium dioxide compound formulation can effectively improve
The control effect of bacterial wilt of tomato.
2. lipopeptid prepared by the present invention-nano-titanium dioxide compound formulation through overtesting, can promote tomato overground part and
The growth of underground part has significant difference, illustrates that the lipopeptid-nano-titanium dioxide compound formulation can promote compared with the control group
Tomato plant strain growth.
3. it is to utilize solid fermentation that the present invention, which prepares one of lipopeptid-nano-titanium dioxide compound formulation raw material lipopeptid substance,
Agricultural wastes are come what is produced, and the present invention uses analysis for soybean powder and stalk mixture as primary solids fermentation substrate, not only effectively
The yield for improving lipopeptid substance, has saved production cost, also reduces environmental pressure, improves the utilization rate of resource.
4. lipopeptid produced by the invention-nano-titanium dioxide compound formulation has environmental pollution small, low toxicity, safety, production
At low cost, prevention and the good advantage of growth-promoting effect are suitble to tomato planting region large area to use.
Description of the drawings
Fig. 1 nano-titanium dioxides X-ray diffraction (XRD) figure.
Fig. 2 nano-titanium dioxides transmission electron microscope (TEM) figure.
Fig. 3 nano-titanium dioxides scanning electron microscope (SEM) figure.
Fig. 4 samples infrared spectrum (FT-IR) figure, a represents nano titanium dioxide powder in figure, and b represents nano-titanium dioxide-
Powder after micro- complex liquid centrifugal drying, c represent the powder after lipopeptid-nano-titanium dioxide compound formulation centrifugal drying
End.
Fig. 5 lipopeptids to the fungistatic effect figure of tomato bacterial wilt pathogen (A.2000mg/L；B.1500mg/L；C.1000mg/
L)。
The greenhouses Fig. 6 controlling experiment respectively handles disease index (DI) variation diagram, and * indicates that, there are significant difference, NS expressions are not deposited
In significant difference (p<0.05).
The greenhouses Fig. 7 controlling experiment respectively handles overground part dry weight, different lowercase letter significant difference (p<0.05).
The greenhouses Fig. 8 controlling experiment respectively handles underground part dry weight, different lowercase letter significant difference (p<0.05).
The greenhouses Fig. 9 growth-promoting tests each processing overground part underground part dry weight and fresh weight of plant seedlings (A. overground part fresh weights；B. underground part fresh weight；C.
Overground part dry weight；D. underground part dry weight), different lowercase letter significant difference (p<0.05).
Specific implementation mode
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without sheet described in detail in claims should will not be limited
Invention.
Analysis for soybean powder and stalk first dry 12h in 60 DEG C of baking ovens and remove most of moisture, and 20 mesh sieve, mistake are crossed in grind away, crushing
Sample after sieve, which places into oven, dries 48h to constant weight for 60 DEG C, preserves for use.
Embodiment 1：
The preparation method of lipopeptid-nano-titanium dioxide compound formulation：(1) prepared by lipopeptid powder：By the Xie Dian of freezing
Afnyloliquefaciens strain X Z-173 (China Committee for Culture Collection of Microorganisms's common micro-organisms center, CGMCC
No.4160), lining on LB tablets, be placed in activation in incubator, picking single bacterium colony is inoculated in LB liquid medium, at 30 DEG C,
It is cultivated under conditions of 170rpm for 24 hours, obtains fermentation seed liquid；Weigh 4.5kg analysis for soybean powder, 3kg stalks, 0.15kg starch and
0.15kg yeast extracts are put into 50L fermentation tanks, and 1L inorganic salt solutions are added, and it is 7 to adjust substrate pH, ensures that moisture content is
40%, rotating speed is set as 50rpm stirrings 60min and mixes well matrix, is sterilized；Wherein, inorganic salt solution includes (g/L)：KH2PO4
1.0, MgSO4·7H2O 0.5, KCl 0.5, L-phenylalanine 2 × 10-3, MnSO4 5×10-3, CuSO4 0.16×10-3,
FeSO4 0.15×10-3；After temperature in fermentation tank is cooling and keeps stablizing, aseptically press 5% (v/w, mL/g's)
Amount access seed liquor, stirs evenly, and adjusts relative humidity in tank and is more than 80%, ventilatory capacity 0.1vvm and tank press 0.01Mpa, preceding
Temperature is set as 25 DEG C and ferments for 24 hours, and temperature is set as 28 DEG C of fermentation 16h afterwards for 24 hours；The matrix after fermentation is weighed with water by 1:10
The ratio of (w/v, g/mL) mixes, shaken at room temperature 1h, and centrifugation removal insoluble matter, it is 1 to add HCl to pH in supernatant, is gone out
Existing white flock precipitate, stand at low temperature is overnight, then collects precipitation with 10000rpm centrifugations 20min, and precipitation is carried out with dichloromethane
Extracting, rotary evaporation remove organic solvent, residue water dissolution and to adjust pH be neutral, are freeze-dried to obtain lipopeptid powder；
(2) prepared by nano titanium dioxide powder：Titanium sulfate is soluble in water by the concentration of 0.1mol/L, it is added 2mol/L's
Ammonia spirit generate white precipitate, make solution last pH be 6, solution centrifugation after, precipitation be washed with water remove for several times it is remaining
NH4 +And SO4 2-, then white precipitate is dispersed in water, 30% aqueous hydrogen peroxide solution (Ti is added4+And H2O2Molar ratio
It is 1：3) stirring makes precipitation peptization, and pertitanic acid (PTA) colloidal sol of yellow is formed after stablizing 15 hours, and PTA colloidal sols are dried at 60 DEG C
Form obtains nano titanium dioxide powder in 1 hour after grinding at xerogel with 400 DEG C of calcinings；
(3) prepared by liquid microelement：By ZnSO4·7H2O, FeSO4·7H2O, CuSO4·5H2O and MnSO4·H2O is dissolved in
Liquid microelement, wherein ZnSO are obtained in water4·7H2O, FeSO4·7H2O, CuSO4·5H2O and MnSO4·H2The content of O is distinguished
0.3g/L, 0.25g/L, 0.2g/L and 0.15g/L；
(4) lipopeptid-nano-titanium dioxide compound formulation obtains：Lipopeptid and nano-silica are sequentially added into liquid microelement
Change titanium, wherein the content of lipopeptid is 0.075%, and the content of nano-titanium dioxide is 0.2%, stirring shake up after on shaking table with
20 DEG C, 150rpm vibrates 10h to get to lipopeptid-nano-titanium dioxide compound formulation.
Embodiment 2：
The preparation method of the compound biological prevention and control agent of lipopeptid-nano-titanium dioxide：(1) prepared by lipopeptid powder：By freezing
Bacillus amyloliquefaciens (Bacillus amyloliquefaciens) strain X Z-173 is lined on LB tablets, is placed in incubator
Interior activation, picking single bacterium colony are inoculated in LB liquid medium, are cultivated at 30 DEG C, under conditions of 170rpm for 24 hours, obtain fermentation seed
Liquid；6kg analysis for soybean powder, 4.5kg stalks, 0.2kg starch and 0.2kg yeast extracts are weighed, is put into 50L fermentation tanks, 2L is added
Inorganic salt solution, it is 8 to adjust substrate pH, moisture content 60%, and rotating speed, which is set as 70rpm stirrings 80min, mixes well matrix, goes out
Bacterium；Wherein, inorganic salt solution includes (g/L)：KH2PO41.0, MgSO4·7H2O 0.5, KCl 0.5, L-phenylalanine 2 × 10-3, MnSO4 5×10-3, CuSO4 0.16×10-3, FeSO4 0.15×10-3；Wait for that temperature is cooling in fermentation tank and keeps stable
Afterwards, the amount for aseptically pressing 25% (v/w, mL/g) accesses seed liquor, stirs evenly, and adjusts relative humidity in tank and is more than
80%, ventilatory capacity 0.5vvm and tank press 0.05Mpa, temperature to be set as 40 DEG C of fermentation 48h；The matrix after fermentation is weighed with water by 1:10
The ratio of (w/v, g/mL) mixes, shaken at room temperature 2h, and centrifugation removal insoluble matter, it is 3 to add HCl to pH in supernatant, is gone out
Existing white flock precipitate, stand at low temperature is overnight, then collects precipitation with 10000rpm centrifugations 20min, and precipitation is carried out with dichloromethane
Extracting, rotary evaporation remove organic solvent, residue water dissolution and to adjust pH be neutral, are freeze-dried to obtain lipopeptid powder；
(2) prepared by nano titanium dioxide powder：Titanium sulfate is soluble in water by the concentration of 0.1mol/L, it is added 3mol/L's
Ammonia spirit generate white precipitate, make solution last pH be 8, solution centrifugation after, precipitation be washed with water remove for several times it is remaining
NH4 +And SO4 2-, then white precipitate is dispersed in water, 30% aqueous hydrogen peroxide solution (Ti is added4+And H2O2Molar ratio
It is 1：5) stirring makes precipitation peptization, and pertitanic acid (PTA) colloidal sol of yellow is formed after stablizing 20 hours, and PTA colloidal sols are dried at 75 DEG C
Form obtains nano titanium dioxide powder in 2 hours after grinding at xerogel with 600 DEG C of calcinings；
(3) prepared by liquid microelement：By ZnSO4·7H2O, FeSO4·7H2O, CuSO4·5H2O and MnSO4·H2O is dissolved in
Liquid microelement, wherein ZnSO are obtained in water4·7H2O, FeSO4·7H2O, CuSO4·5H2O and MnSO4·H2The content of O is distinguished
0.4g/L, 0.35g/L, 0.35g/L and 0.25g/L；
(4) lipopeptid-nano-titanium dioxide compound formulation obtains：Lipopeptid and nano-silica are sequentially added into liquid microelement
Change titanium, wherein the content of lipopeptid is 0.15%, and the content of nano-titanium dioxide is 0.3%, stirring shake up after on shaking table with 40
DEG C, 250rpm vibrates 30h to get to lipopeptid-nano-titanium dioxide compound formulation.
Embodiment 3：
The preparation method of the compound biological prevention and control agent of lipopeptid-nano-titanium dioxide：(1) prepared by lipopeptid powder：By freezing
Bacillus amyloliquefaciens (Bacillus amyloliquefaciens) strain X Z-173 is lined on LB tablets, is placed in incubator
Interior activation, picking single bacterium colony are inoculated in LB liquid medium, are cultivated at 30 DEG C, under conditions of 170rpm for 24 hours, as fermentation seed
Liquid；5.67kg analysis for soybean powder, 3.67kg stalks, 0.17kg starch and 0.18kg yeast extracts are weighed, is put into 50L fermentation tanks,
1L inorganic salt solutions are added, it is 7.5 to adjust substrate pH, moisture content 55%, and it is fully mixed that rotating speed is set as 70rpm stirrings 60min
Even matrix, sterilizing；Wherein, inorganic salt solution includes (g/L)：KH2PO41.0, MgSO4·7H2O 0.5, KCl 0.5, L- phenylpropyl alcohol
Propylhomoserin 2 × 10-3, MnSO4 5×10-3, CuSO4 0.16×10-3, FeSO4 0.15×10-3；Wait for that temperature cooling is simultaneously in fermentation tank
It keeps after stablizing, the amount for aseptically pressing 10% (v/w, mL/g) accesses seed liquor, stirs evenly, and adjusts relatively wet in tank
Degree is more than 80%, and ventilatory capacity 0.3vvm and tank press 0.03Mpa, preceding temperature to be for 24 hours set as 30 DEG C and ferment, for 24 hours afterwards set temperature
For 37 DEG C of fermentation 20h；The matrix after fermentation is weighed with water by 1:The ratio of 10 (w/v, g/mL) mixes, shaken at room temperature 1h, centrifugation
Insoluble matter is removed, it is 2.0 that HCl to pH is added in supernatant, white flock precipitate occurs, and 4 DEG C stand overnight, then with
10000rpm centrifuges 20min and collects precipitation, and precipitation is stripped with dichloromethane, and rotary evaporation removes organic solvent, residue
With water dissolution and to adjust pH be neutral, is freeze-dried to obtain lipopeptid powder；
(2) prepared by nano titanium dioxide powder：Titanium sulfate is soluble in water by the concentration of 0.1mol/L, it is added 3mol/L's
Ammonia spirit generate white precipitate, make solution last pH be 7, solution centrifugation after, precipitation be washed with water remove for several times it is remaining
NH4 +And SO4 2-, then white precipitate is dispersed in water, 30% aqueous hydrogen peroxide solution (Ti is added4+And H2O2Molar ratio
It is 1：4) stirring makes precipitation peptization, and pertitanic acid (PTA) colloidal sol of yellow is formed after stablizing 15 hours, and PTA colloidal sols are dried at 75 DEG C
Form obtains nano titanium dioxide powder in 1 hour after grinding at xerogel with 500 DEG C of calcinings；
(3) prepared by liquid microelement：By ZnSO4·7H2O, FeSO4·7H2O, CuSO4·5H2O and MnSO4·H2O is dissolved in
Liquid microelement, wherein ZnSO are obtained in water4·7H2O, FeSO4·7H2O, CuSO4·5H2O and MnSO4·H2The content of O is distinguished
0.35g/L, 0.3g/L, 0.24g/L and 0.18g/L；
(4) lipopeptid-nano-titanium dioxide compound formulation obtains：Lipopeptid and nano-silica are sequentially added into liquid microelement
Change titanium, wherein the content of lipopeptid is 0.1%, and the content of nano-titanium dioxide is 0.25%, stirring shake up after on shaking table with 30
DEG C, 170rpm oscillations are for 24 hours to get to lipopeptid-nano-titanium dioxide compound formulation.
Embodiment 4：
Using ultra-pure water, titanium sulfate (chemistry is pure), ammonium hydroxide (analysis is pure), hydrogen peroxide (analysis is pure) and sulfate (analysis
It is pure) according to the preparation method of embodiment 3 to obtain lipopeptid, nano-titanium dioxide, liquid microelement and lipopeptid-nano-titanium dioxide multiple
Close preparation.
1, the preparation of nano-titanium dioxide-trace element complex liquid
Be added nano-titanium dioxide into liquid microelement, stirring shake up after on shaking table with 30 DEG C, 170rpm oscillations
For 24 hours to get to nano-titanium dioxide-trace element complex liquid.The mass percent of nano-titanium dioxide is in the complex liquid
0.25%.
2, structural characterization
2.1X- x ray diffractions (XRD) are analyzed：
Nano titanium dioxide powder is divided using Japanese Rigaku companies D/MAX-2500/PC x-ray diffractometers
Analysis.As shown in Figure 1, PDF card JCPDS 21-1272 are consulted, 25.3 °, 37.8 °, 48.0 °, 53.8 ° marked in XRD spectrum
With the characteristic peak at 62.8 ° (2 θ) correspond to respectively anatase (101), (004), (200), (105) and (204) crystal face, simultaneously
There is no characteristic peaks to show that brockite and rutile are not present in sample at 27.4 ° and 30.8 °, the results showed for preparing receives
Rice titania powder is Detitanium-ore-type.
2.2 transmission electron microscopes (TEM) and scanning electron microscope (SEM) analysis：
Use S-4800 hairs of Japanese JEOL companies JEM-2100F 200kV transmission electron microscopes and Hitachi, Japan
It penetrates scanning electron microscope the appearance and size of nano titanium dioxide powder is observed and analyzed.As shown in Figure 2 and Figure 3, nanometer
Titania powder is formed by the nanoparticle aggregation of 10~40nm of many.
2.3 infrared spectrums (FT-IR) are analyzed：
Nano-titanium dioxide-trace element complex liquid and lipopeptid-nano-titanium dioxide compound formulation carry out centrifugation point respectively
It is for several times with milli-Q water precipitation, then dry at 60 DEG C from rear, it is after grinding that nano-titanium dioxide-trace element is compound
Agent, lipopeptid-nano-titanium dioxide compound formulation powder and nano titanium dioxide powder KBr tablettings, using Thermo Fisher
IS10 infrared spectrometers analyze the variation of main functional group, 500~4000cm of wave-number range-1。
As shown in figure 4, curve (a) and (b) compare it is found that nano-titanium dioxide-trace element complex liquid is by processing
The powder obtained afterwards is in 3083cm-1And 3730cm-1There is new peak in place, is the characteristic absorption of O-H groups, but 3083cm-1
The characteristic absorption for the O-H groups that the peak at place connects for hydrogen bond, while 476cm-1And 1135cm-1The spy of the Ti-O-Ti and Ti-O at place
Sign absorption peak has been displaced to 482cm respectively-1And 1125cm-1Place, shows micro in nano-titanium dioxide-trace element complex liquid
Element ion is combined together with nano-titanium dioxide.
Curve (a) and (c) compare it is found that the powder that lipopeptid-nano-titanium dioxide compound formulation obtains later by processing
In 1457cm-1, 1542cm-1, 1649cm-1, 1717cm-1, 2851cm-1、2921cm-1, 3188cm-1、3621cm-1, 3735cm-1
There is new peak in place, C=O, CH2, hydrogen in respectively CH3, amide bands of a spectrum II (N-H or C-N), amide bands of a spectrum I (C=O), ketone
The O-H of key connection, the characteristic absorption of other O-H, while 476cm-1And 1135cm-1The characteristic absorption of the Ti-O-Ti and Ti-O at place
Peak has been displaced to 468cm respectively-1And 1122cm-1Place, shows lipopeptid, trace element in lipopeptid-nano-titanium dioxide compound formulation
Ion is combined together with nano-titanium dioxide.
Embodiment 5：Lipopeptid and lipopeptid-nano-titanium dioxide compound formulation examine the inhibitory activity of tomato bacterial wilt pathogen
It surveys.
1, prepared by tomato bacterial wilt pathogen bacterium solution.
The picking tomato bacterial wilt pathogen on TTC tablets accesses in liquid NA culture mediums, 30 DEG C, the training of 170rpm shaking tables
It supports to logarithmic phase, bacteria suspension is diluted to 10 with sterile water6~107Experiment pathogen bacteria suspension is made in CFU/mL.
2, inhibitory activity detects.By 121 DEG C of nano titanium dioxide powder, 20min sterilizings, after lipopeptid is added in liquid microelement
0.22 μm of filter membrane degerming is crossed, lipopeptid-nano-titanium dioxide compound formulation is aseptically prepared.By 200 μ of pathogen bacteria suspension
L is spread evenly across on NA culture medium flat plates, then draw 100 μ L various concentrations lipopeptide solutions (200mg/L, 500mg/L,
750mg/L, 1000mg/L, 1500mg/L, 2000mg/L) it injects on tablet in Oxford cup, 30 DEG C of cultures for 24 hours, observe antibacterial shape
Condition simultaneously measures inhibition zone size, is repeated 3 times.As shown in table 1 and Fig. 5, lipopeptid has stronger suppression to tomato bacterial wilt pathogen
Effect processed, inhibition zone are apparent.
It is 10 aseptically to prepare containing bacteria suspension concentration6The pathogen of CFU/mL and the lipopeptid-of various concentration are received
Rice titanium dioxide compound formulation centrifugal drying after powder (0,0.15mg/mL, 0.3mg/mL, 0.6mg/mL, 1.2mg/mL,
2.4mg/mL, 4.8mg/mL) NA fluid nutrient medium test tubes, 30 DEG C under dark or illumination condition, 170rpm shaking table cultures 24
Hour, measure the minimal inhibitory concentration (MIC) of powder.The result shows that under dark or illumination condition, lipopeptid-nano-titanium dioxide
The MIC of powder after compound formulation centrifugal drying is 1.2mg/mL.
Bacteriostasis of the 1 various concentration lipopeptide solution of table to tomato bacterial wilt pathogen
Embodiment 6：
Using ultra-pure water, titanium sulfate (chemistry is pure), ammonium hydroxide (analysis is pure), hydrogen peroxide (analysis is pure) and sulfate (analysis
It is pure) according to the preparation method of embodiment 3 to obtain lipopeptid, nano-titanium dioxide, liquid microelement and lipopeptid-nano-titanium dioxide multiple
Preparation is closed, nano-titanium dioxide-trace element complex liquid is obtained according to the preparation method of embodiment 4.
1, the preparation of lipopeptid-trace element complex liquid
Be added lipopeptid into liquid microelement, stirring shake up after on shaking table with 30 DEG C, 170rpm oscillations for 24 hours to get to
Lipopeptid-trace element complex liquid.The mass percent of lipopeptid is 0.1% in the complex liquid.
2, greenhouse controlling experiment of the lipopeptid-nano-titanium dioxide compound formulation to bacterial wilt of tomato
Controlling experiment in Jiangsu Province's solid organic castoff recycling Hi-Tech Key Laboratory greenhouse into
Row, experiment set 5 processing, and scheme is as follows：(1) Control takes 10ml ultra-pure waters to be uniformly sprayed on the blade face of every plant of tomato seedling
And basal part of stem, as a contrast；(2) MS takes 10ml liquid microelements to be uniformly sprayed on blade face and the basal part of stem of every plant of tomato seedling；
(3) LFA takes 10ml lipopeptids-trace element complex liquid to be uniformly sprayed on blade face and the basal part of stem of every plant of tomato seedling；(4) LFB,
10ml nano-titanium dioxides-trace element complex liquid is taken uniformly to be sprayed on blade face and the basal part of stem of every plant of tomato seedling；(5) LFC,
10ml lipopeptids-nano-titanium dioxide compound formulation is taken uniformly to be sprayed on blade face and the basal part of stem of every plant of tomato seedling.Each processing
30 basins, the dress 2kg soil per basin, apply equivalent nitrogen, phosphorus, potassium fertilizer (including：Urea, calcium superphosphate, potassium chloride), per 1 plant of pot transplanting
Tomato seedling.Transplanting pours into tomato bacterial wilt pathogen bacteria suspension after 7 days in soil, and cause of disease bacteria concentration is made to reach 106CFU/g soil
More than, it fills bacterium and processing 1 time is carried out by above-mentioned 5 processing schemes to tomato seedling after 24 hours.
It presses severity Scaling standard within the 4th, 8,12,16,20,24,28 day after treatment, records incidence, count each processing
Disease index (DI) and control effect, and statistical disposition respectively handles plant above ground portion, underground part dry weight after 28 days.
Severity Scaling standard and disease index computational methods are as follows：
0 grade：Plant is normal；1 grade：25% blade below of plant shows as wilting symptom；
2 grades：The blade of plant 26%~50% shows as wilting symptom；
3 grades：The blade of plant 51%~75% shows as wilting symptom；
4 grades：76% or more blade of plant shows as wilting symptom or plant is dead.
Disease index (DI)=[∑ (each disease grade plant number × at different levels to represent numerical value)]/(investigate total strain number × highest level
Numerical value) × 100%
Control effect=(control disease index-processing disease index)/control disease index × 100%
3, greenhouse growth-promoting experiment of the lipopeptid-nano-titanium dioxide compound formulation to bacterial wilt of tomato
Growth-promoting experiment in Jiangsu Province's solid organic castoff recycling Hi-Tech Key Laboratory greenhouse into
Row, experiment set 5 processing, and scheme is as follows：(1) Control takes 10ml ultra-pure waters to be uniformly sprayed on the blade face of every plant of tomato seedling
And basal part of stem, as a contrast；(2) MS takes 10ml liquid microelements to be uniformly sprayed on blade face and the basal part of stem of every plant of tomato seedling；
(3) LFA takes 10ml lipopeptids-trace element complex liquid to be uniformly sprayed on blade face and the basal part of stem of every plant of tomato seedling；(4) LFB,
10ml nano-titanium dioxides-trace element complex liquid is taken uniformly to be sprayed on blade face and the basal part of stem of every plant of tomato seedling；(5) LFC,
10ml lipopeptids-nano-titanium dioxide compound formulation is taken uniformly to be sprayed on blade face and the basal part of stem of every plant of tomato seedling.Each processing
15 basins, the dress 2kg soil per basin, apply equivalent nitrogen, phosphorus, potassium fertilizer (including：Urea, calcium superphosphate, potassium chloride), per 1 plant of pot transplanting
Tomato seedling.Transplanting carries out processing 1 time to tomato seedling after 7 days by above-mentioned 5 processing schemes.After processing 30 days, statistics is everywhere
Manage plant plant height, stem thickness, SPAD values and overground part underground part dry weight and fresh weight of plant seedlings.
4, result and analysis:
As shown in table 2 and Fig. 6, as the growth of tomato plant is taken compared with other processing and sprays lipopeptid-nanometer two
The disease index of titanium oxide compound formulation is very low, after processing at the 28th day with respect to control effect be 67.47%, compared to its elsewhere
The control effect of reason has significant difference, illustrates nano-titanium dioxide and lipopeptid in lipopeptid-nano-titanium dioxide compound formulation
In conjunction with the stability that can preferably improve lipopeptid, extend the action time of lipopeptid, the lipopeptid-nano-titanium dioxide compound formulation
Bacterial wilt of tomato can be effectively prevented.
As shown in Figure 7 and Figure 8, after being handled 28 days in greenhouse controlling experiment, take that spray lipopeptid-nano-titanium dioxide compound
The plant above ground portion of preparation and underground part dry weight are higher than other processing, and have significant difference compared with the control, illustrate the fat
Peptide-nano-titanium dioxide compound formulation can promote tomato plant strain growth while control of plant bacterial wilt.
As shown in table 3 and Fig. 9, after being handled 30 days in the experiment of greenhouse growth-promoting, take that spray lipopeptid-nano-titanium dioxide compound
Plant plant height, stem thickness, SPAD values and the overground part underground part dry weight and fresh weight of plant seedlings of preparation are higher than other processing, and in addition to SPAD values
Outside, other values all have significant difference compared with Control, illustrate that the lipopeptid-nano-titanium dioxide compound formulation can promote
Tomato plant strain growth takes spraying lipopeptid-nano-titanium dioxide compound formulation and can advantageously promote compared with other processing modes
Tomato plant strain growth.
Control effect of the 2 greenhouse controlling experiment different disposal of table to bacterial wilt of tomato
Note：Different lowercase letter significant difference (p<0.05)
The plant height, stem thickness and SPAD values of plant are respectively handled in 3 greenhouse growth-promoting experiment of table
Note：Different lowercase letter significant difference (p<0.05).
Claims (6)
1. a kind of lipopeptid-nano-titanium dioxide compound formulation, which is characterized in that said preparation includes the group of following mass percent
Point：
Lipopeptid 0.075%~0.15%；
Nano-titanium dioxide 0.2%~0.3%；
Trace elements zn2+0.0069%~0.0092%, Fe2+0.005%~0.007%, Cu2+0.0052%~0.0091%
And Mn2+0.005%~0.0083%；
Remaining is water；
Wherein, the preparation method of the lipopeptid is as follows：
(1a) activates bacillus amyloliquefaciens, obtains seed liquor, and the bacillus amyloliquefaciens are bacillus amyloliquefaciens CGMCC
No.4160；
Seed liquor is transferred in fermentation medium by (1b), is adjusted relative humidity in fermentation tank and is more than 80%, fermentation production lipopeptid；
(1c) after fermentation, the mixture that fermentation is obtained is with water according to 1g：10mL ratios are uniformly mixed, centrifugation, in collection
Clearly, it is 1~3 to adjust supernatant pH with hydrochloric acid, stands, then centrifuge, collects precipitation, precipitation is extracted with dichloromethane, then is rotated
Except dichloromethane, residue water dissolution and adjust pH be 7.0, be finally freeze-dried to obtain lipopeptid powder；
The preparation method of the nano-titanium dioxide is as follows：
(2a) titanium sulfate is soluble in water by the concentration of 0.1mol/L, and the ammonia spirit of 2~3mol/L is added, and it is 6 to make the pH of solution
~8, obtain mixture；
(2b) centrifuges mixture, collects precipitation, precipitation is washed with water；
The precipitation that step (2b) obtains is dispersed in water by (2c), and the aqueous hydrogen peroxide solution that volume ratio is 30% is added, makes molten
Ti in liquid4+And H2O2Molar ratio be 1：3~5, it stirs evenly, stands 15~20 hours, obtain peroxo titanic acid sol；
Peroxo titanic acid sol is formed xerogel by (2d) in 60~75 DEG C of drying, by xerogel grind into powder, 400~600
It is calcined 1~2 hour under the conditions of DEG C, obtains nano titanium dioxide powder.
2. the preparation method of lipopeptid described in claim 1-nano-titanium dioxide compound formulation, which is characterized in that this method packet
Include following steps：
(1) preparation of lipopeptid：
(1a) activates bacillus amyloliquefaciens, obtains seed liquor；
Seed liquor is transferred in fermentation medium by (1b), is adjusted relative humidity in fermentation tank and is more than 80%, fermentation production lipopeptid；
(1c) after fermentation, the mixture that fermentation is obtained is with water according to 1g：10mL ratios are uniformly mixed, centrifugation, in collection
Clearly, it is 1~3 to adjust supernatant pH with hydrochloric acid, stands, then centrifuge, collects precipitation, precipitation is extracted with dichloromethane, then is rotated
Except dichloromethane, residue water dissolution and adjust pH be 7.0, be finally freeze-dried to obtain lipopeptid powder；
(2) preparation of nano-titanium dioxide：
(2a) titanium sulfate is soluble in water by the concentration of 0.1mol/L, and the ammonia spirit of 2~3mol/L is added, and it is 6 to make the pH of solution
~8, obtain mixture；
(2b) centrifuges mixture, collects precipitation, precipitation is washed with water；
The precipitation that step (2b) obtains is dispersed in water by (2c), and the aqueous hydrogen peroxide solution that volume ratio is 30% is added, makes molten
Ti in liquid4+And H2O2Molar ratio be 1：3~5, it stirs evenly, stands 15~20 hours, obtain peroxo titanic acid sol；
Peroxo titanic acid sol is formed xerogel by (2d) in 60~75 DEG C of drying, by xerogel grind into powder, 400~600
It is calcined 1~2 hour under the conditions of DEG C, obtains nano titanium dioxide powder；
(3) preparation of liquid microelement：Trace element is dissolved in the water, trace element water-soluble liquid is obtained；
(4) lipopeptid-nano-titanium dioxide compound formulation obtains：In the trace element water-soluble liquid obtained to step (3), sequentially add
The nano-titanium dioxide that the lipopeptid and step (2) that step (1) obtains obtain, stirring shakes up, in 20~40 DEG C, 150~250rpm
Under the conditions of, 10~30h of oscillation is to get to lipopeptid-nano-titanium dioxide compound formulation.
3. preparation method according to claim 2, which is characterized in that in step (1b), the fermentation medium according to
Following method equal proportion is prepared：Weigh 4.5~6kg analysis for soybean powder, 3~4.5kg stalks, 0.15~0.2kg starch and 0.15
~0.2kg yeast extracts, are put into fermentation tank, and 1~2L inorganic salt solutions are added, and it is 7~8 to adjust pH, adjusts culture medium
Moisture content is 40%~60%, the inorganic salt solution, and formula is：1.0g/L KH2PO4、0.5g/L MgSO4·7H2O、
0.5g/L KCl、2×10-3G/L L-phenylalanines, 5 × 10-3g/L MnSO4、0.16×10-3g/L CuSO4、0.15×10- 3g/L FeSO4。
4. preparation method according to claim 2, which is characterized in that in step (1b), fermentation process uses temperature-variable fermentation,
It is 0.1~0.5vvm to keep ventilatory capacity during the fermentation, tank pressure is 0.01~0.05Mpa, and first stage fermentation temperature is 25
~40 DEG C, fermentation 20~for 24 hours, the fermentation temperature of second stage is 28~40 DEG C, fermentation 16~for 24 hours, and ensure second stage hair
The temperature of ferment is 0~7 DEG C higher than first stage temperature.
5. lipopeptid described in claim 1-application of the nano-titanium dioxide compound formulation in control of plant bacterial wilt.
6. application of the lipopeptid described in claim 1-nano-titanium dioxide compound formulation on promoting tomato plant strain growth.
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