CN101755738B - Solid lipid nano spinosad and preparation method and application thereof - Google Patents
Solid lipid nano spinosad and preparation method and application thereof Download PDFInfo
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- CN101755738B CN101755738B CN 200910110088 CN200910110088A CN101755738B CN 101755738 B CN101755738 B CN 101755738B CN 200910110088 CN200910110088 CN 200910110088 CN 200910110088 A CN200910110088 A CN 200910110088A CN 101755738 B CN101755738 B CN 101755738B
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- pleocidin
- spinosad
- solid lipid
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- 150000002632 lipids Chemical class 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 53
- 239000007787 solid Substances 0.000 title claims abstract description 43
- JFLRKDZMHNBDQS-UCQUSYKYSA-N CC[C@H]1CCC[C@@H]([C@H](C(=O)C2=C[C@H]3[C@@H]4C[C@@H](C[C@H]4C(=C[C@H]3[C@@H]2CC(=O)O1)C)O[C@H]5[C@@H]([C@@H]([C@H]([C@@H](O5)C)OC)OC)OC)C)O[C@H]6CC[C@@H]([C@H](O6)C)N(C)C.CC[C@H]1CCC[C@@H]([C@H](C(=O)C2=C[C@H]3[C@@H]4C[C@@H](C[C@H]4C=C[C@H]3C2CC(=O)O1)O[C@H]5[C@@H]([C@@H]([C@H]([C@@H](O5)C)OC)OC)OC)C)O[C@H]6CC[C@@H]([C@H](O6)C)N(C)C Chemical compound CC[C@H]1CCC[C@@H]([C@H](C(=O)C2=C[C@H]3[C@@H]4C[C@@H](C[C@H]4C(=C[C@H]3[C@@H]2CC(=O)O1)C)O[C@H]5[C@@H]([C@@H]([C@H]([C@@H](O5)C)OC)OC)OC)C)O[C@H]6CC[C@@H]([C@H](O6)C)N(C)C.CC[C@H]1CCC[C@@H]([C@H](C(=O)C2=C[C@H]3[C@@H]4C[C@@H](C[C@H]4C=C[C@H]3C2CC(=O)O1)O[C@H]5[C@@H]([C@@H]([C@H]([C@@H](O5)C)OC)OC)OC)C)O[C@H]6CC[C@@H]([C@H](O6)C)N(C)C JFLRKDZMHNBDQS-UCQUSYKYSA-N 0.000 title claims abstract description 38
- 239000005930 Spinosad Substances 0.000 title claims abstract description 38
- 229940014213 spinosad Drugs 0.000 title claims abstract description 38
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- -1 capillary Chemical compound 0.000 claims description 67
- 238000000034 method Methods 0.000 claims description 57
- 230000008569 process Effects 0.000 claims description 51
- 239000005912 Lufenuron Substances 0.000 claims description 45
- 229960000521 lufenuron Drugs 0.000 claims description 45
- 239000000843 powder Substances 0.000 claims description 43
- 239000000203 mixture Substances 0.000 claims description 41
- 239000005906 Imidacloprid Substances 0.000 claims description 39
- 229940056881 imidacloprid Drugs 0.000 claims description 39
- 239000004562 water dispersible granule Substances 0.000 claims description 37
- 239000000375 suspending agent Substances 0.000 claims description 32
- NWWZPOKUUAIXIW-DHZHZOJOSA-N (E)-thiamethoxam Chemical compound [O-][N+](=O)/N=C/1N(C)COCN\1CC1=CN=C(Cl)S1 NWWZPOKUUAIXIW-DHZHZOJOSA-N 0.000 claims description 31
- WOWBFOBYOAGEEA-UHFFFAOYSA-N diafenthiuron Chemical compound CC(C)C1=C(NC(=S)NC(C)(C)C)C(C(C)C)=CC(OC=2C=CC=CC=2)=C1 WOWBFOBYOAGEEA-UHFFFAOYSA-N 0.000 claims description 30
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 claims description 30
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims description 28
- 238000009736 wetting Methods 0.000 claims description 25
- PWPJGUXAGUPAHP-UHFFFAOYSA-N lufenuron Chemical compound C1=C(Cl)C(OC(F)(F)C(C(F)(F)F)F)=CC(Cl)=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F PWPJGUXAGUPAHP-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims description 14
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 14
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 239000005995 Aluminium silicate Substances 0.000 claims description 9
- 239000004480 active ingredient Substances 0.000 claims description 9
- 235000012211 aluminium silicate Nutrition 0.000 claims description 9
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 9
- 239000012752 auxiliary agent Substances 0.000 claims description 8
- 229920001732 Lignosulfonate Polymers 0.000 claims description 7
- 229920001285 xanthan gum Polymers 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000009472 formulation Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 4
- LWEAHXKXKDCSIE-UHFFFAOYSA-M 2,3-di(propan-2-yl)naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S([O-])(=O)=O)=C(C(C)C)C(C(C)C)=CC2=C1 LWEAHXKXKDCSIE-UHFFFAOYSA-M 0.000 claims description 4
- CDMGNVWZXRKJNS-UHFFFAOYSA-N 2-benzylphenol Chemical compound OC1=CC=CC=C1CC1=CC=CC=C1 CDMGNVWZXRKJNS-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000007884 disintegrant Substances 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 230000000361 pesticidal effect Effects 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 2
- 229920000858 Cyclodextrin Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 230000002528 anti-freeze Effects 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims description 2
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 2
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 2
- 229930182490 saponin Natural products 0.000 claims description 2
- 150000007949 saponins Chemical class 0.000 claims description 2
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000001694 spray drying Methods 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000002562 thickening agent Substances 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 155
- 238000006303 photolysis reaction Methods 0.000 abstract description 20
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 16
- 239000000575 pesticide Substances 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 6
- 230000000749 insecticidal effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 109
- 238000002474 experimental method Methods 0.000 description 46
- 238000005338 heat storage Methods 0.000 description 34
- 238000012360 testing method Methods 0.000 description 31
- 230000004071 biological effect Effects 0.000 description 30
- 238000005538 encapsulation Methods 0.000 description 30
- 230000000857 drug effect Effects 0.000 description 22
- 238000010521 absorption reaction Methods 0.000 description 17
- 238000013112 stability test Methods 0.000 description 17
- 230000000694 effects Effects 0.000 description 16
- 239000000463 material Substances 0.000 description 16
- 238000002835 absorbance Methods 0.000 description 15
- 238000004128 high performance liquid chromatography Methods 0.000 description 15
- 239000006101 laboratory sample Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 15
- 108010053950 Teicoplanin Proteins 0.000 description 13
- BJNLLBUOHPVGFT-QRZIFLFXSA-N teichomycin Chemical compound CCCCCCCCCC(=O)N[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC(C(=C1)OC=2C(=CC(=CC=2)[C@@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@H]2C(N[C@H](C3=CC(O)=CC(O[C@@H]4[C@H]([C@@H](O)[C@H](O)[C@@H](CO)O4)O)=C3C=3C(O)=CC=C(C=3)[C@@H](NC3=O)C(=O)N2)C(O)=O)=O)Cl)=C(OC=2C(=CC(C[C@H](C(N4)=O)NC(=O)[C@H](N)C=5C=C(O6)C(O)=CC=5)=CC=2)Cl)C=C1[C@H]3NC(=O)[C@@H]4C1=CC6=CC(O)=C1 BJNLLBUOHPVGFT-QRZIFLFXSA-N 0.000 description 13
- 241000256247 Spodoptera exigua Species 0.000 description 12
- 239000003814 drug Substances 0.000 description 9
- 239000008187 granular material Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 241001414989 Thysanoptera Species 0.000 description 7
- 239000003643 water by type Substances 0.000 description 7
- 241001414720 Cicadellidae Species 0.000 description 6
- 240000008067 Cucumis sativus Species 0.000 description 6
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 6
- 241000238631 Hexapoda Species 0.000 description 6
- 241000500437 Plutella xylostella Species 0.000 description 6
- 244000269722 Thea sinensis Species 0.000 description 6
- 229920005551 calcium lignosulfonate Polymers 0.000 description 6
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002917 insecticide Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000004563 wettable powder Substances 0.000 description 3
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 239000000825 pharmaceutical preparation Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 230000008685 targeting Effects 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000254173 Coleoptera Species 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000255777 Lepidoptera Species 0.000 description 1
- 241000238814 Orthoptera Species 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- 241000868102 Saccharopolyspora spinosa Species 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000002164 acetylcholinergic effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229960003692 gamma aminobutyric acid Drugs 0.000 description 1
- BTCSSZJGUNDROE-UHFFFAOYSA-N gamma-aminobutyric acid Chemical compound NCCCC(O)=O BTCSSZJGUNDROE-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000003120 macrolide antibiotic agent Substances 0.000 description 1
- 229940041033 macrolides Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
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- 239000000693 micelle Substances 0.000 description 1
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- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002088 nanocapsule Substances 0.000 description 1
- 239000007908 nanoemulsion Substances 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 229960003512 nicotinic acid Drugs 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 230000003151 ovacidal effect Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention applies to the technical field of pesticide preparations, provides a solid lipid nano spinosad, and also provides a preparation method of the solid lipid nano spinosad and application of the solid lipid nano spinosad on pesticide preparations. Compared with a compound preparation prepared by directly taking nano spinosad raw pesticide as the raw material, the pesticide preparation of the solid lipid nano spinosad has enhanced cold and hot storage chemical stability, reduced photolysis rate, prolonged efficacy period, reduced dosage and obviously improved insecticidal effect.
Description
Technical field
The invention belongs to technical field of pesticide preparations, relate in particular to a kind of solid lipid nano spinosad and preparation method thereof and the application on pesticidal preparations.
Background technology
It is a kind of macrolides harmless boilogical insecticide that extracts in thorn sugared many born of the same parents bacterium (Saccharopolysporaspinosa) zymotic fluid that multiple killing teichomycin has another name called pleocidin (Spinosad).
Pleocidin has insect tags and stomach poison function fast, and blade is had stronger osmosis, can kill subepidermal insect, and the longevity of residure is long, and some insects are had certain ovicidal action.Without systemic action.Can effectively preventing Lepidoptera, diptera and thrips insect, can prevent and treat well also that in coleoptera and orthoptera, some takes food the insect insects of blade in a large number, poor to the control efficiency of sucking pest and mite class.
Its mechanism of action is considered to the acting body of nicotinic acid acetylcholinergic receptor, can sustained activation target insect acetylcholine nicotine receptor, but its binding site is different from nicotine and Imidacloprid.Pleocidin also can affect the GABA acceptor, and its desinsection speed can compare favourably with chemical pesticide.Safe, and with present common insecticide without cross resistance, be the biological insecticides of low toxicity, efficient, low-residual, existing efficient insecticidal properties has again the characteristic of beneficial insect and mammalian safe is arranged, and is the insecticide of a kind of low toxicity, efficient, wide spectrum.
Pleocidin is widely used in composite with other agricultural chemicals, to increase insecticidal spectrum, improves preventive effect and cost performance.publication number CN101380004 Chinese invention patent application discloses with lufenuron and pleocidin composition pesticide and the preparation method as active component, the Patent Application Publication of publication number CN101180959 with capillary and pleocidin composition pesticide and the preparation method as active component, the Patent Application Publication of publication number CN101305723 with capillary and pleocidin composition pesticide and the preparation method as active component, the Patent Application Publication of publication number CN101248798 with diafenthiuron and pleocidin composition pesticide and the preparation method as active component, the Patent Application Publication of publication number CN101305723 with Diacloden and pleocidin composition pesticide and the preparation method as active component.But because pleocidin is seen light and easily decomposed, hydrolysis is very fast, and in water, the half life period is 1 day; In soil half life period 9-10 days, the barrier that the chemical stability after making it composite and the photodissociation in use procedure become its combination application technique development of restriction.The preparation that experiment showed, above composition exists seriously decomposition in the cold and hot storage process of active component pleocidin, photodissociation in use procedure, degradation problem under drug effect.
Nanometer technology is a new technique, nanosecond science and technology belong to the forward position cross discipline, nanometer technology and Application of micron are comprised nanoparticle (Nanoparticles, NP) in the system of field of pharmaceutical preparations, nanocapsule (Nanocapstles, NC), nano-micelle (Nanomicelle, NM), lipid nanometer body (Nano-liposemes, NL) and nanometer microemulsion (Nano-emulsion, NE) etc.Wherein NP generally refers to by natural or macromolecular material is made, and granularity is at nanoscale (1.0-500nm) solid colloid particulate, or is called colloid bearer (colloidal.carriers).Active component is positioned at inside particles by dissolving, package action.This novel pharmaceutical preparation has slow-release function, can improve medicine stability, dispersiveness, service efficiency and drug effect simultaneously.Solid lipid nano (Solid lipid nanopartides, SLN) be with natural or synthetic lipoid as carrier matrix, active ingredient is wrapped in lipoid core.At present, there is no the report that solid lipid nano spinosad prepares and be applied to pesticidal preparations both at home and abroad.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art, a kind of novel solid lipid nano spinosad is provided, described solid lipid nano spinosad comprises the component of following weight portion proportioning: pleocidin 1-15 part, capric acid 30-80 part, polyvinyl alcohol 5-25 part, preferably include the component of following weight portion proportioning: pleocidin 4-12 part, capric acid 70-80 part, polyvinyl alcohol 16-18 part.
Another object of the present invention is, a kind of preparation method of described solid lipid nano spinosad is provided, this preparation method comprises the following steps: pleocidin and capric acid are dissolved in organic solvent together, and the concentration of pleocidin is 1%-15%, and the concentration of capric acid is 30%-80%; The polyvinyl alcohol water is made into the aqueous solution that concentration is 0.1%-10%; With above-mentioned organic solution and polyvinyl alcohol water solution in proportion 1: 3-1: 10 mix, and make mixed liquor emulsification by stirring or vibration or high shear, then use littleization of ultrasonic, and stirring after 1-20 hour again, drying namely gets described solid lipid nano spinosad.
Wherein, described organic solvent is chloroform or ethyl acetate; Described dry boulton process or freeze-drying or the spray drying process of adopting.
The solid lipid nano spinosad that makes is called again the female powder of pleocidin solid lipid nano granule or solid lipid nano spinosad or referred to as nano spinosad following.
Another purpose of the present invention is to provide the application of described solid lipid nano spinosad on the preparation pesticidal preparations.
Described solid lipid nano spinosad preparation can be contained water dispersible granules, suspending agent or the wetting powder of pleocidin.
Described water dispersible granules, suspending agent or wetting powder comprise effective constituents A and B, A is solid lipid nano spinosad, B is for increasing as required the active ingredient of other non-solid lipid nanometer, B is any in lufenuron, capillary, Imidacloprid, diafenthiuron, Diacloden, and A and B weight ratio are A: B=1: 1-800.
solid lipid nano spinosad is during for the preparation of water dispersible granules, and it forms and also comprise the surfactant that accounts for weight of formulation 1%-10%, the auxiliary agent of 1%-5%, the disintegrant of 0%-15%, the adhesive of 1%-5%, the carrier of 1%-80% except active ingredient, described surfactant comprises lignosulfonates, lauryl sodium sulfate, fatty acid sulphate, aliphatic alcohol polyethenoxy, nekal, one or more in the alkylpolyoxyethylene phosphate, described auxiliary agent comprises Ben-zylphenol Polyoxyethyl Ether, Tea Saponin, one or more in alkylphenol polyoxyethylene, described disintegrant comprises bentonite, ammonium sulfate, urea, one or more in magnesium sulfate, described adhesive comprises polyethylene glycol, cyclodextrin, starch, a kind of in sodium silicate, described carrier comprises diatomite, kaolin, white carbon, a kind of in nacrite.
Solid lipid nano spinosad is during for the preparation of suspending agent, and it forms and also comprise the surfactant that accounts for weight of formulation 1%-10%, the auxiliary agent of 1%-5%, the carrier of 1%-80% except active ingredient; Described surfactant is one or more in the phosphate, fatty alcohol-polyoxyethylene ether, lignosulfonates, naphthalenesulfonate formaldehyde condensation compound of JFC, 603#, 600#, alkylphenol polyoxyethylene, alkylphenol polyoxyethylene; Described auxiliary agent comprises antifreeze ethylene glycol, thickener xanthans, defoamer silicone; Described carrier is water.
Solid lipid nano spinosad is during for the preparation of wetting powder, and it forms and also include the surfactant that accounts for weight of formulation 1%-10%, the carrier of 1%-80% except active ingredient; Described surfactant comprises lignosulfonates, lauryl sodium sulfate, fatty acid sulphate, aliphatic alcohol polyethenoxy, nekal, Ben-zylphenol Polyoxyethyl Ether, alkylphenol polyoxyethylene, pull open one or more in powder, and described carrier comprises a kind of in kaolin, precipitated calcium carbonate, clay, white carbon.
The inventor studies and finds that this lipid carrier is with biocompatible lipoid carrier matrix, have many advantages: the blade face compatibility is good, be conducive to absorption and the transportation of medicine, good targeting is arranged, can improve the chemical stability of medicine, improve compound property, be conducive to the ultraviolet light photodissociation, the prolong drug lasting period, significantly promote drug effect.Prepare the solid lipid nano granule of pleocidin with capric acid as carrier matrix, have stability high, toxicity is low, and technique is simple, and cost is relatively low, the advantage of energy large-scale production.Show by cold and hot storage stability test, ultraviolet light stability test and the test of pesticide effectiveness: good by the agriculture chemical compounding composition chemical stability of the inventive method preparation with solid lipid nano spinosad of the present invention, resolution ratio is low under UV-irradiation, and drug effect has significant lifting.
Applying solid lipid nanometer pleocidin of the present invention has been compared following advantage with the complex composition preparation of the former powder production of direct employing pleocidin:
(1) cold and hot storage stability significantly promotes, through the time stabilization time, storage life, shelf-life extend.
(2) stability of ultraviolet light significantly promoted, can reduce the ultraviolet light photodissociation in the medication process, keep better drug effect.
(3) lipid nanometer type pleocidin has better compatibility to plant leaf blade, is more conducive to targeting dilivery, improves absorption ratio.
(4) when the foliage-spray, the biochemical degradation metabolism under the blade top layer of lipid nanometer pleocidin slows down, and bin stability significantly promotes, and has extended the drug effect phase.
During (5) as Ji Shi or seed dressing, lipid nanometer pleocidin stability promotes, and the drug effect phase extends, and control efficiency significantly promotes.
(6) dosage reduces, and is conducive to delaying drug resistance and environmental protection.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
One, the preparation of the female powder of solid lipid nano spinosad
Embodiment 1 4% contains the female powder of solid lipid nano spinosad
The content of pleocidin is 40 gram/kilograms
The content of capric acid is 785 gram/kilograms
Polyvinyl alcohol content is 165 gram/kilograms
97% former medicine 41.5 grams of pleocidin and 785 gram capric acid are dissolved in 100 gram chloroforms together, then mix with 2200 gram 7.5% polyvinyl alcohol water solutions, by stirring or vibration or high shear, mixed liquor is mixed and be the emulsification shape, then use littleization of ultrasonic, make it become the 100-500 nano_scale particle, then stir 2 hours female powder of last obtained by freeze drying solid lipid nano type pleocidin.
Embodiment 2
The female powder of 8% solid lipid nano spinosad
The content of pleocidin is 80 gram/kilograms
The content of capric acid is 760 gram/kilograms
Polyvinyl alcohol content is 160 gram/kilograms
97% former medicine 82.5 grams of pleocidin and 760 gram capric acid are dissolved in 200 gram chloroforms together, then mix with 2000 gram 8% polyvinyl alcohol water solutions, by stirring or vibration or high shear, mixed liquor is mixed to the emulsification shape, then use littleization of ultrasonic, make it become the 100-500 nano_scale particle, stir after 3.5 hours obtained by freeze drying again.
Embodiment 3
The female powder of 12% solid lipid nano spinosad
The content of pleocidin is 120 gram/kilograms
The content of capric acid is 700 gram/kilograms
Polyvinyl alcohol content is 180 gram/kilograms
97% former medicine 124 grams of pleocidin and 700 gram capric acid are dissolved in 300 gram chloroforms together, then mix with 2000 gram 9% polyvinyl alcohol water solutions, by stirring or vibration or high shear, mixed liquor is mixed to the emulsification shape, then use littleization of ultrasonic, make it become the 100-500 nano_scale particle, stir after 5 hours obtained by freeze drying again.
Two, composition preparation and the living effect of surveying
Following examples pesticide active ingredient used except have indicate all by 100% purity meter, in practical operation, convert according to the actual purity of former medicine used, difference is adjusted with filler or water.
Embodiment 4 30% lufenuron lipid nanometer pleocidin water dispersible granules preparation methods
Lufenuron 26% (weight)
12% lipid nanometer pleocidin (embodiment 3), 34% (weight) (pleocidin folding hundred 4%)
Sodium lignin sulfonate 10% (weight)
Lauryl sodium sulfate 5% (weight)
Diatomite is supplied 100% (weight)
Said mixture is evenly mixed, and air-flow crushing adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain product.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
30% lufenuron lipid nanometer many sterilized waters dispersible granule and 30% common many sterilized waters of lufenuron dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get the heat storage in 54 ℃ of constant temperature ovens of 2 encapsulation samples, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot resolution ratio of storing sample in 14 days.Experimental result such as following table.
Table 4-1
The cold and hot storage stability of lufenuron lipid nanometer pleocidin and common lufenuron pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 4-2
Lufenuron lipid nanometer pleocidin and common lufenuron pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of beet armyworm, carried out drug effect test of field zone for clear and definite lufenuron lipid nanometer pleocidin water dispersible granules and common lufenuron pleocidin.
Process 10000 times of 1:30% lufenuron lipid nanometer pleocidin water dispersible granules
Process 2: 10000 times of common 30% lufenuron pleocidin water dispersible granules
Process 3: blank
The effect of table 4-3 different disposal control beet armyworm
Embodiment 5 15% lufenuron lipid nanometer multiple killing teichomycin suspending agent preparation methods
12% lipid nanometer multiple killing teichomycin (embodiment 3), 42% (weight) (pleocidin folding hundred 5%)
Lufenuron 10% (weight)
Ethylene glycol 14% (weight)
Xanthans 0.5% (weight)
Alkylphenol polyoxyethylene 10% (weight)
Silicone 0.5% (weight)
Water complements to 100% (weight)
After mixing in ball mill ball milling 2～3 hours, make particle diameter all namely form preparation below 5um.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
15% lufenuron lipid nanometer multiple killing teichomycin suspending agent and 15% common lufenuron multiple killing teichomycin suspending agent are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Took out later on the contrast resolution ratio of processing the cold storage sample of sample determination and heat storage sample in 14 days.Experimental result such as following table.
Table 5-1
The cold and hot storage stability of lufenuron lipid nanometer pleocidin and common lufenuron pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 5-2
Lufenuron lipid nanometer pleocidin and common lufenuron pleocidin ultraviolet light stability inferior are relatively
2, biological effect experiment
To the control efficiency difference of beet armyworm, carried out drug effect test of field zone for clear and definite lufenuron lipid nanometer pleocidin suspension and common lufenuron pleocidin suspension.
Process 6000 times of 1:15% lufenuron lipid nanometer multiple killing teichomycin suspending agents
Process 2: 6000 times of common 15% lufenuron multiple killing teichomycin suspending agents
Process 3: blank
The effect of table 5-3 different disposal control beet armyworm
Embodiment 6 30% lufenuron lipid nanometer pleocidin wetting powder preparation methods
Lufenuron 28% (weight)
8% lipid nanometer pleocidin (embodiment 2), 25% (weight) (pleocidin folding hundred 2%)
Calcium lignosulfonate 13% (weight)
Lauryl sodium sulfate 3% (weight)
Pull open powder 5% (weight)
Kaolin is supplied 100% (weight)
Mentioned component is mixed, cross 325 mesh sieves and namely get product after air-flow crushing.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
30% lufenuron lipid nanometer pleocidin wetting powder and 30% common lufenuron pleocidin wetting powder are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
Table 6-1
The cold and hot storage stability of lufenuron lipid nanometer pleocidin and common lufenuron pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
The ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 6-2
Lufenuron lipid nanometer pleocidin and common lufenuron pleocidin ultraviolet light stability inferior are relatively
2, biological effect experiment
To the control efficiency difference of beet armyworm, carried out drug effect test of field zone for clear and definite lufenuron lipid nanometer pleocidin water dispersible granules and common lufenuron pleocidin.
Process 8000 times of 1:30% lufenuron lipid nanometer pleocidin wetting powders
Process 2: 8000 times of common 30% lufenuron pleocidin wetting powders
Process 3: blank
The effect of table 6-3 different disposal control beet armyworm
Embodiment 7 30% many sterilized waters of capillary lipid nanometer dispersible granule preparation methods
Capillary 26% (weight)
12% lipid nanometer pleocidin (embodiment 3), 34% (weight) (pleocidin folding hundred 4%)
Sodium lignin sulfonate 10% (weight)
Lauryl sodium sulfate 5% (weight)
Diatomite is supplied
Said mixture is evenly mixed, and air-flow crushing adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain product.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
30% capillary lipid nanometer many sterilized waters dispersible granule and 30% common many sterilized waters of capillary dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 7-1 capillary lipid nanometer pleocidin and common capillary pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 7-2 capillary lipid nanometer pleocidin and common capillary pleocidin ultraviolet light stability inferior are relatively
2, biological effect experiment
To the control efficiency difference of beet armyworm, carried out drug effect test of field zone for clear and definite lufenuron lipid nanometer pleocidin water dispersible granules and common lufenuron pleocidin.
Process 5000 times of many sterilized waters of 1:30% capillary lipid nanometer dispersible granules
Process 2: 5000 times of common 30% many sterilized waters of capillary dispersible granules
Process 3: blank
The effect of table 7-3 different disposal control beet armyworm
Embodiment 8 10% lipid nanometer pleocidin capillary suspending agent preparation methods
12% lipid nanometer pleocidin (embodiment 3), 42% (weight) (pleocidin folding hundred 5%)
Capillary 5%, (weight)
Alkylphenol polyoxyethylene 4%, (weight)
Xanthans 0.2% (weight)
Water is supplied 100% (weight)
After mixing in ball mill ball milling 2～3 hours, particle diameter is got final product below 5um.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
10% lipid nanometer pleocidin capillary suspending agent and 10% common pleocidin capillary suspending agent are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 8-1 capillary lipid nanometer pleocidin and common capillary pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 8-2 capillary lipid nanometer pleocidin and common capillary pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of beet armyworm, carried out drug effect test of field zone for clear and definite lufenuron lipid nanometer pleocidin water dispersible granules and common lufenuron pleocidin.
Process 3000 times of 1:10% lipid nanometer pleocidin capillary suspending agents
Process 2: 3000 times of common 10% pleocidin capillary suspending agents
Process 3: blank
The effect of table 8-3 different disposal control beet armyworm
Embodiment 9 30% capillary lipid nanometer pleocidin wetting powder preparation methods
Capillary 28% (weight)
8% lipid nanometer pleocidin (embodiment 2), 25% (weight) (pleocidin folding hundred 2%)
Calcium lignosulfonate 13% (weight)
Lauryl sodium sulfate 3% (weight)
Pull open powder 5% (weight)
Kaolin is supplied 100% (weight)
Mentioned component is mixed, cross 325 mesh sieves and namely get product after air-flow crushing.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
30% capillary lipid nanometer pleocidin wetting powder and 30% common capillary pleocidin wetting powder are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 9-1 capillary lipid nanometer pleocidin and common capillary pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 9-2 capillary lipid nanometer pleocidin and common capillary pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of beet armyworm, carried out drug effect test of field zone for clear and definite lufenuron lipid nanometer pleocidin water dispersible granules and common lufenuron pleocidin.
Process 4000 times of the many sterilization wettable powders of 1:30% capillary lipid nanometer
Process 2: 4000 times of the common 30% many sterilization wettable powders of capillary
Process 3: blank
The effect of table 9-3 different disposal control beet armyworm
Embodiment 10 21% lipid nanometer pleocidin imidacloprid water dispersible granule preparation methods
12% lipid nanometer multiple killing teichomycin (embodiment 3) 8.5% (pleocidin folding hundred 1%)
Imidacloprid 20% (weight)
Calcium lignosulfonate 6% (weight)
Lauryl sodium sulfate 4% (weight)
Diatomite adds to 100% weight
The present embodiment stability and biological effect test
1, cold and hot storage stability test
21% lipid nanometer pleocidin imidacloprid water dispersible granule and 21% common pleocidin imidacloprid water dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Took out later on the contrast resolution ratio of processing the cold storage sample of sample determination and heat storage sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 10-1 Imidacloprid lipid nanometer pleocidin and common Imidacloprid pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 10-2 Imidacloprid lipid nanometer pleocidin and common Imidacloprid pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of cucumber thrips, carried out drug effect test of field zone for clear and definite Imidacloprid lipid nanometer pleocidin water dispersible granules and common Imidacloprid pleocidin.
Process 4000 times of 1:21% lipid nanometer pleocidin imidacloprid water dispersible granules
Process 2: 4000 times of common 21% pleocidin imidacloprid water dispersible granules
Process 3: blank
The effect of table 10-3 different disposal control cucumber thrips
Embodiment 11 32% lipid nanometer pleocidin imidacloprid suspending agent preparation methods
12% lipid nanometer multiple killing teichomycin (embodiment 3) 17% (pleocidin folding hundred 2%)
Imidacloprid 30% (weight)
Alkylphenol polyoxyethylene 10% (weight)
Xanthans 0.3% (weight)
Water adds to 100% (weight)
After mixing in ball mill ball milling 2～3 hours, particle diameter is got final product below 5um.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
32% lipid nanometer pleocidin imidacloprid suspending agent and 32% common pleocidin imidacloprid suspending agent are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and (doing cold storage in ℃ refrigerator, getting 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table
The cold and hot storage stability of table 11-1 Imidacloprid lipid nanometer pleocidin and common Imidacloprid pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 11-2 Imidacloprid lipid nanometer pleocidin and common Imidacloprid pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of cucumber thrips, carried out drug effect test of field zone for clear and definite Imidacloprid lipid nanometer pleocidin water dispersible granules and common Imidacloprid pleocidin.
Process 8000 times of 1:32% lipid nanometer pleocidin imidacloprid suspending agents
Process 2: 8000 times of common 32% pleocidin imidacloprid suspending agents
Process 3: blank
The effect of table 11-3 different disposal control cucumber thrips
Embodiment 12 25% lipid nanometer pleocidin imidacloprid wettable powder preparation methods
Imidacloprid 20% (weight)
12% lipid nanometer pleocidin (embodiment 3), 42% (weight) (pleocidin folding hundred 5%)
Calcium lignosulfonate 13% (weight)
Lauryl sodium sulfate 3% (weight)
Pull open powder 5% (weight)
Kaolin is supplied 100% (weight)
Mentioned component is mixed, cross 325 mesh sieves and namely get product after air-flow crushing.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
25% lipid nanometer pleocidin imidacloprid wettable powder and 25% common pleocidin imidacloprid wettable powder are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 12-1 Imidacloprid lipid nanometer pleocidin and common Imidacloprid pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 12-2 Imidacloprid lipid nanometer pleocidin and common Imidacloprid pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of cucumber thrips, carried out drug effect test of field zone for clear and definite Imidacloprid lipid nanometer pleocidin water dispersible granules and common Imidacloprid pleocidin.
Process 9000 times of 1:25% lipid nanometer pleocidin imidacloprid wettable powders
Process 2: 9000 times of common 25% pleocidin imidacloprid wettable powders
Process 3: blank
The effect of table 12-3 different disposal control cucumber thrips
Embodiment 13 30% lipid nanometer pleocidin diafenthiuron water dispersible granule preparation methods
Diafenthiuron 26% (weight)
12% lipid nanometer pleocidin (embodiment 3), 34% (weight) (pleocidin folding hundred 4%)
Sodium lignin sulfonate 10% (weight)
Lauryl sodium sulfate 5% (weight)
Diatomite is supplied 100% (weight)
Said mixture is evenly mixed, and air-flow crushing adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain product.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
30% lipid nanometer pleocidin diafenthiuron water dispersible granule and 30% common pleocidin diafenthiuron water dispersible granule are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 13-1 diafenthiuron lipid nanometer pleocidin and common diafenthiuron pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 13-2 diafenthiuron lipid nanometer pleocidin and common diafenthiuron pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To diamond-back moth control efficiency difference, carried out drug effect test of field zone for clear and definite diafenthiuron lipid nanometer pleocidin water dispersible granules and common diafenthiuron pleocidin.
Process 3000 times of 1:30% lipid nanometer pleocidin diafenthiuron water dispersible granules
Process 2: 3000 times of common 30% pleocidin diafenthiuron water dispersible granules
Process 3: blank
The effect of table 13-3 different disposal control diamond-back moth
Embodiment 14 30% lipid nanometer pleocidin diafenthiuron suspending agent preparation methods
12% lipid nanometer multiple killing teichomycin (embodiment 3), 42% (weight) (pleocidin folding hundred 5%)
Diafenthiuron 25% (weight)
Alkylphenol polyoxyethylene 13% (weight)
Ethylene glycol 5% (weight)
Xanthans 0.3% (weight)
Organic silicone 0.5% (weight)
Water 100% (weight)
After mixing in ball mill ball milling 2～3 hours, particle diameter is all got final product below 5um.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
30% lipid nanometer pleocidin diafenthiuron suspending agent and 30% common pleocidin diafenthiuron suspending agent are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Took out later on the contrast resolution ratio of processing the cold storage sample of sample determination and heat storage sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 14-1 diafenthiuron lipid nanometer pleocidin and common diafenthiuron pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 14-2 diafenthiuron lipid nanometer pleocidin and common diafenthiuron pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of diamond-back moth, carried out drug effect test of field zone for clear and definite diafenthiuron lipid nanometer pleocidin water dispersible granules and common diafenthiuron pleocidin.
Process 4000 times of 1:30% lipid nanometer pleocidin diafenthiuron suspending agents
Process 2: 4000 times of common 30% pleocidin diafenthiuron suspending agents
Process 3: blank
The effect of table 14-3 different disposal control diamond-back moth
Embodiment 15 30% lipid nanometer pleocidin diafenthiuron wetting powder preparation methods
Diafenthiuron 25% (weight)
12% lipid nanometer pleocidin (embodiment 3), 42% (weight) (pleocidin folding hundred 5%)
Calcium lignosulfonate 13% (weight)
Lauryl sodium sulfate 3% (weight)
Pull open powder 5% (weight)
Kaolin is supplied 100% (weight)
Mentioned component is mixed, cross 325 mesh sieves and namely get product after air-flow crushing.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
30% lipid nanometer pleocidin diafenthiuron wetting powder and 30% common pleocidin diafenthiuron wetting powder are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 15-1 diafenthiuron lipid nanometer pleocidin and common diafenthiuron pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 15-2 diafenthiuron lipid nanometer pleocidin and common diafenthiuron pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of diamond-back moth, carried out drug effect test of field zone for clear and definite diafenthiuron lipid nanometer pleocidin wetting powder and common diafenthiuron pleocidin.
Process 3000 times of 1:30% lipid nanometer pleocidin diafenthiuron wetting powders
Process 2: 3000 times of common 30% pleocidin diafenthiuron wetting powders
Process 3: blank
The effect of table 15-3 different disposal control diamond-back moth
Embodiment 16 21% lipid nanometer pleocidin Diacloden water dispersible granules preparation methods
12% lipid nanometer multiple killing teichomycin (embodiment 3) 8.5% (pleocidin folding hundred 1%)
Diacloden 20% (weight)
Lignosulfonates 13% (weight)
Lauryl sodium sulfate 2% (weight)
Diatomite adds to 100% weight
The present embodiment stability and biological effect test
1, cold and hot storage stability test
21% lipid nanometer pleocidin Diacloden water dispersible granules and 21% common pleocidin Diacloden water dispersible granules are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 16-1 Diacloden lipid nanometer pleocidin and common Diacloden pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 16-2 Diacloden lipid nanometer pleocidin and common Diacloden pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To tea lesser leafhopper control efficiency difference, carried out drug effect test of field zone for clear and definite Diacloden lipid nanometer pleocidin water dispersible granules and common Diacloden pleocidin.
Process 4000 times of 1:21% lipid nanometer pleocidin Diacloden water dispersible granules
Process 2: 4000 times of common 21% pleocidin Diacloden water dispersible granules
Process 3: blank
The effect of table 16-3 different disposal control tea lesser leafhopper
Embodiment 17 32% lipid nanometer pleocidin Diacloden suspending agent preparation methods
12% lipid nanometer multiple killing teichomycin (embodiment 3) 17% (pleocidin folding hundred 2%)
Diacloden 30% (weight)
Alkylphenol polyoxyethylene 10% (weight)
Silicone 0.3% (weight)
Xanthans 0.3% (weight)
Water adds to 100% (weight)
Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with the multiple killing teichomycin Diacloden suspending agent that makes 32% after the sand mill sand milling.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
32% lipid nanometer pleocidin Diacloden suspending agent and 32% common pleocidin Diacloden suspending agent are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Took out later on the contrast resolution ratio of processing the cold storage sample of sample determination and heat storage sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 17-1 Diacloden lipid nanometer pleocidin and common Diacloden pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 17-2 Diacloden lipid nanometer pleocidin and common Diacloden pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To the control efficiency difference of tea lesser leafhopper, carried out drug effect test of field zone for clear and definite Diacloden lipid nanometer pleocidin water dispersible granules and common Diacloden pleocidin.
Process 6000 times of 1:32% lipid nanometer pleocidin Diacloden suspending agents
Process 2: 6000 times of common 32% pleocidin Diacloden suspending agents
Process 3: blank
The effect of table 17-3 different disposal control tea lesser leafhopper
Embodiment 18 25% lipid nanometer pleocidin Diacloden wetting powder preparation methods
Diacloden 20% (weight)
12% lipid nanometer pleocidin (embodiment 3), 42% (weight) (pleocidin folding hundred 5%)
Calcium lignosulfonate 13% (weight)
Lauryl sodium sulfate 3% (weight)
Pull open powder 5% (weight)
Kaolin is supplied 100% (weight)
Mentioned component is mixed, cross 325 mesh sieves and namely get product after air-flow crushing.
The present embodiment stability and biological effect test
1, cold and hot storage stability test
25% lipid nanometer pleocidin Diacloden wetting powder and 25% common pleocidin Diacloden wetting powder are carried out cold and hot storage experiment simultaneously with more stable property.
Laboratory sample is cutd open the bottle encapsulation with 6 peaces, get 2 encapsulation samples and do the heat storage in 54 ℃ of constant temperature ovens, get 2 and do cold storage in 0 ℃ of refrigerator, get 2 and at room temperature place.Measured later on cold storage sample and hot contrast resolution ratio of storing sample in 14 days.Experimental result such as following table.
The cold and hot storage stability of table 18-1 Diacloden lipid nanometer pleocidin and common Diacloden pleocidin relatively
Annotate: component content * 100% to be detected in cold and hot storage contrast resolution ratio=(composition to be detected in component content to be detected in cold storage sample-Re storage sample)/cold storage sample; Cold storage sample was stored 14 days under 0 ℃ of condition, and heat storage sample detects after storing 14 days under 54 ℃ of conditions.
2, ultraviolet light photolysis experiments
Uviol lamp while treatment with irradiation sample with 2 parallel 30W, ultraviolet lamp tube center position liquid level of solution distance is 40cm, measure the absorbance of each material and calculate remaining pleocidin content under its different irradiations at corresponding ultraviolet absorption peak place respectively with ultraviolet specrophotometer and high performance liquid chromatography, conclusion sees the following form.
Table 18-2 Diacloden lipid nanometer pleocidin and common Diacloden pleocidin ultraviolet light stability inferior are relatively
3, biological effect experiment
To tea lesser leafhopper control efficiency difference, carried out drug effect test of field zone for clear and definite Diacloden lipid nanometer pleocidin water dispersible granules and common Diacloden pleocidin.
Process 6000 times of 1:25% lipid nanometer pleocidin Diacloden wetting powders
Process 2: 6000 times of common 25% pleocidin Diacloden wetting powders
Process 3: blank
The effect of table 18-3 different disposal control tea lesser leafhopper
The above is only preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. solid lipid nano spinosad, it is characterized in that, the component that comprises following weight portion proportioning: pleocidin 4-12 part, capric acid 70-80 part, polyvinyl alcohol 16-18 part, described solid lipid nano spinosad preparation method is as follows: comprise the following steps: pleocidin and capric acid are dissolved in organic solvent together, and the concentration of pleocidin is 1%-15%, and the concentration of capric acid is 30%-80%; The polyvinyl alcohol water is made into the aqueous solution that concentration is 0.1%-10%; With above-mentioned organic solution and polyvinyl alcohol water solution in proportion 1: 3-1: 10 mix, and make mixed liquor emulsification by stirring or vibration or high shear, then use littleization of ultrasonic, and stirring after 1-20 hour again, drying namely gets described solid lipid nano spinosad.
2. the preparation method of solid lipid nano spinosad according to claim 1, is characterized in that, described organic solvent is chloroform or ethyl acetate; Described dry boulton process or freeze-drying or the spray drying process of adopting.
3. the application of solid lipid nano spinosad claimed in claim 1 on the preparation pesticidal preparations.
4. application according to claim 3, is characterized in that, described solid lipid nano spinosad preparation contained water dispersible granules, suspending agent or the wetting powder of pleocidin.
5. application according to claim 4, it is characterized in that, described water dispersible granules, suspending agent or wetting powder comprise effective constituents A and B, A is solid lipid nano spinosad, B is any in lufenuron, capillary, Imidacloprid, diafenthiuron, Diacloden, and A and B weight ratio are A: B=1: 1-800.
6. application according to claim 5, it is characterized in that, solid lipid nano spinosad is during for the preparation of water dispersible granules, and it forms and also comprise the surfactant that accounts for weight of formulation 1%-10%, the auxiliary agent of 1%-5%, the disintegrant of 0%-15%, the adhesive of 1%-5%, the carrier of 1%-80% except active ingredient, described surfactant comprises lignosulfonates, lauryl sodium sulfate, fatty acid sulphate, aliphatic alcohol polyethenoxy, nekal, one or more in the alkylpolyoxyethylene phosphate, described auxiliary agent comprises Ben-zylphenol Polyoxyethyl Ether, Tea Saponin, one or more in alkylphenol polyoxyethylene, described disintegrant comprises bentonite, ammonium sulfate, urea, one or more in magnesium sulfate, described adhesive comprises polyethylene glycol, cyclodextrin, starch, a kind of in sodium silicate, described carrier comprises diatomite, kaolin, white carbon, a kind of in nacrite.
7. application according to claim 5, is characterized in that, solid lipid nano spinosad is during for the preparation of suspending agent, and it forms and also comprise the surfactant that accounts for weight of formulation 1%-10%, the auxiliary agent of 1%-5%, the carrier of 1%-80% except active ingredient; Described surfactant is one or more in the phosphate, fatty alcohol-polyoxyethylene ether, lignosulfonates, naphthalenesulfonate formaldehyde condensation compound of JFC, 603#, 600#, alkylphenol polyoxyethylene, alkylphenol polyoxyethylene; Described auxiliary agent comprises antifreeze ethylene glycol, thickener xanthans, defoamer silicone; Described carrier is water.
8. application according to claim 5, is characterized in that, solid lipid nano spinosad is during for the preparation of wetting powder, and it forms and also include the surfactant that accounts for weight of formulation 1%-10%, the carrier of 1%-80% except active ingredient; Described surfactant comprises lignosulfonates, lauryl sodium sulfate, fatty acid sulphate, aliphatic alcohol polyethenoxy, nekal, Ben-zylphenol Polyoxyethyl Ether, alkylphenol polyoxyethylene, pull open one or more in powder, and described carrier comprises a kind of in kaolin, precipitated calcium carbonate, clay, white carbon.
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| CN101720766B (en) * | 2009-12-29 | 2012-08-22 | 华南农业大学 | Insecticidal composition of tea saponin and pleocidin |
| CN102450269A (en) * | 2011-12-27 | 2012-05-16 | 辽宁师范大学 | Triazolone nanometer colloid suspending agent and preparation method thereof |
| CN102726378B (en) * | 2012-06-09 | 2015-11-18 | 广东中迅农科股份有限公司 | Spinosad water dispersible granule and preparation method thereof |
| EP2877027A1 (en) * | 2012-07-27 | 2015-06-03 | Novartis Tiergesundheit AG | New treatment of fish with a nanosus pens ion of lufenuron or hexaflumuron |
| EP3148331B1 (en) * | 2014-05-30 | 2020-12-23 | OMS Investments, Inc. | Methods of making nano-sized water-based dispersion compositions |
| JP2021523944A (en) * | 2018-05-15 | 2021-09-09 | フラッグシップ パイオニアリング イノベーションズ シックス，エルエルシー | Pest control composition and its use |
| CN109673630A (en) * | 2018-12-20 | 2019-04-26 | 浙江省食品药品检验研究院 | A kind of lipid nano particle and preparation method thereof with controlling plant diseases function |
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