CN114885953A - 一种甲维盐-海藻酸钠纳米颗粒缓释农药及其制备方法 - Google Patents
一种甲维盐-海藻酸钠纳米颗粒缓释农药及其制备方法 Download PDFInfo
- Publication number
- CN114885953A CN114885953A CN202210583915.4A CN202210583915A CN114885953A CN 114885953 A CN114885953 A CN 114885953A CN 202210583915 A CN202210583915 A CN 202210583915A CN 114885953 A CN114885953 A CN 114885953A
- Authority
- CN
- China
- Prior art keywords
- emamectin benzoate
- sodium alginate
- slow
- preparation
- release
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000661 sodium alginate Substances 0.000 title claims abstract description 145
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 145
- 239000000575 pesticide Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 103
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 94
- 239000005894 Emamectin Substances 0.000 title claims abstract description 89
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 title claims abstract description 89
- CXEGAUYXQAKHKJ-NSBHKLITSA-N emamectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](NC)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 CXEGAUYXQAKHKJ-NSBHKLITSA-N 0.000 title abstract 5
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical group CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 56
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 56
- 239000003979 granulating agent Substances 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- GCKZANITAMOIAR-XWVCPFKXSA-N dsstox_cid_14566 Chemical compound [O-]C(=O)C1=CC=CC=C1.C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H]([NH2+]C)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 GCKZANITAMOIAR-XWVCPFKXSA-N 0.000 claims description 179
- 238000003756 stirring Methods 0.000 claims description 35
- -1 polyoxyethylene Polymers 0.000 claims description 21
- 239000000839 emulsion Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009775 high-speed stirring Methods 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 claims description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 4
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 claims description 3
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 claims description 3
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 2
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims description 2
- 229920002101 Chitin Polymers 0.000 claims description 2
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- 229920000084 Gum arabic Polymers 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 229920003012 Hydroxypropyl distarch phosphate Polymers 0.000 claims description 2
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 239000005662 Paraffin oil Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 108010073771 Soybean Proteins Proteins 0.000 claims description 2
- 235000010489 acacia gum Nutrition 0.000 claims description 2
- 239000000205 acacia gum Substances 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 150000003973 alkyl amines Chemical class 0.000 claims description 2
- 229940077388 benzenesulfonate Drugs 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000004359 castor oil Substances 0.000 claims description 2
- 235000019438 castor oil Nutrition 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 claims description 2
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims description 2
- 229960001826 dimethylphthalate Drugs 0.000 claims description 2
- 235000013804 distarch phosphate Nutrition 0.000 claims description 2
- 239000001245 distarch phosphate Substances 0.000 claims description 2
- 230000001804 emulsifying effect Effects 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- 229920000591 gum Polymers 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 2
- 235000013825 hydroxy propyl distarch phosphate Nutrition 0.000 claims description 2
- 239000001310 hydroxy propyl distarch phosphate Substances 0.000 claims description 2
- DVROLKBAWTYHHD-UHFFFAOYSA-N hydroxy propyl distarch phosphate Chemical compound OC1C(O)C(OC)OC(CO)C1OC(O)CCOC1C(OC2C(C(O)C(OC3C(C(OP(O)(=O)OC4C(C(O)C(OC)OC4CO)O)C(C)OC3CO)O)OC2COC2C(C(O)C(OC)C(CO)O2)O)O)OC(CO)C(OC)C1O DVROLKBAWTYHHD-UHFFFAOYSA-N 0.000 claims description 2
- 239000001341 hydroxy propyl starch Substances 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 235000013828 hydroxypropyl starch Nutrition 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000002563 ionic surfactant Substances 0.000 claims description 2
- 239000000787 lecithin Substances 0.000 claims description 2
- 235000010445 lecithin Nutrition 0.000 claims description 2
- 229940067606 lecithin Drugs 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920000136 polysorbate Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 229940001941 soy protein Drugs 0.000 claims description 2
- 235000015096 spirit Nutrition 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- 235000010493 xanthan gum Nutrition 0.000 claims description 2
- 239000000230 xanthan gum Substances 0.000 claims description 2
- 229920001285 xanthan gum Polymers 0.000 claims description 2
- 229940082509 xanthan gum Drugs 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 241000978776 Senegalia senegal Species 0.000 claims 1
- 230000009885 systemic effect Effects 0.000 abstract description 21
- 230000000749 insecticidal effect Effects 0.000 abstract description 18
- 238000006303 photolysis reaction Methods 0.000 abstract description 15
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 15
- 230000008901 benefit Effects 0.000 abstract description 10
- 230000002688 persistence Effects 0.000 abstract description 10
- 230000004044 response Effects 0.000 abstract description 7
- 239000002904 solvent Substances 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 34
- 238000013268 sustained release Methods 0.000 description 27
- 239000012730 sustained-release form Substances 0.000 description 27
- 240000008042 Zea mays Species 0.000 description 18
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 18
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 16
- 235000005822 corn Nutrition 0.000 description 16
- 241000196324 Embryophyta Species 0.000 description 15
- 239000000523 sample Substances 0.000 description 15
- 239000003090 pesticide formulation Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 9
- 241000346285 Ostrinia furnacalis Species 0.000 description 8
- 231100000225 lethality Toxicity 0.000 description 8
- 241000607479 Yersinia pestis Species 0.000 description 7
- 241000238631 Hexapoda Species 0.000 description 5
- 241001477931 Mythimna unipuncta Species 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 235000010443 alginic acid Nutrition 0.000 description 4
- 229920000615 alginic acid Polymers 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000000875 corresponding effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010494 dissociation reaction Methods 0.000 description 3
- 230000005593 dissociations Effects 0.000 description 3
- 230000002045 lasting effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 235000019198 oils Nutrition 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000001338 self-assembly Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- IBSREHMXUMOFBB-JFUDTMANSA-N 5u8924t11h Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O3)C=C[C@H](C)[C@@H](C(C)C)O4)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C.C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 IBSREHMXUMOFBB-JFUDTMANSA-N 0.000 description 2
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 2
- 239000005660 Abamectin Substances 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 2
- 229950008167 abamectin Drugs 0.000 description 2
- 229940072056 alginate Drugs 0.000 description 2
- 229960001126 alginic acid Drugs 0.000 description 2
- 239000000783 alginic acid Substances 0.000 description 2
- 150000004781 alginic acids Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000000502 dialysis Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000004495 emulsifiable concentrate Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 235000009973 maize Nutrition 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000375 suspending agent Substances 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- AEMOLEFTQBMNLQ-AZLKCVHYSA-N (2r,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-AZLKCVHYSA-N 0.000 description 1
- AEMOLEFTQBMNLQ-SYJWYVCOSA-N (2s,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-SYJWYVCOSA-N 0.000 description 1
- WCXDHFDTOYPNIE-RIYZIHGNSA-N (E)-acetamiprid Chemical compound N#C/N=C(\C)N(C)CC1=CC=C(Cl)N=C1 WCXDHFDTOYPNIE-RIYZIHGNSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 244000215068 Acacia senegal Species 0.000 description 1
- 239000005875 Acetamiprid Substances 0.000 description 1
- 241000512259 Ascophyllum nodosum Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000005946 Cypermethrin Substances 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 241001057636 Dracaena deremensis Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 1
- 239000005906 Imidacloprid Substances 0.000 description 1
- 241000255777 Lepidoptera Species 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 229960005424 cypermethrin Drugs 0.000 description 1
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 description 1
- TUTWLYPCGCUWQI-UHFFFAOYSA-N decanamide Chemical compound CCCCCCCCCC(N)=O TUTWLYPCGCUWQI-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229940056881 imidacloprid Drugs 0.000 description 1
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000003120 macrolide antibiotic agent Substances 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000002088 nanocapsule Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 150000004804 polysaccharides Chemical class 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000000384 rearing effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 235000011067 sorbitan monolaureate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 238000004885 tandem mass spectrometry Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/22—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明公开一种甲维盐‑海藻酸钠纳米颗粒缓释农药及其制备方法,属于农药制剂技术领域。该甲维盐‑海藻酸钠纳米颗粒缓释农药包括以下重量份数的原料:甲维盐1‑15份、固体成粒剂0.5‑6份、表面活性剂1‑10份、分散剂0.5‑10份;其中,固体成粒剂为海藻酸钠。由以上原料制备得到的甲维盐‑海藻酸钠纳米颗粒缓释农药具有很好的抗光解性能、缓释功效,以及同时具备优异的内吸传导性、温度响应特性和杀虫持效性,具有高效、持效、环保和低用量的优点。且该制备方法工艺过程简单,设备投资小,主要溶剂为水,价格低廉,生产成本低。
Description
技术领域
本发明属于农药制剂技术领域,具体涉及一种甲维盐-海藻酸钠纳米颗粒缓释农药及其制备方法。
背景技术
随着我国农业生产的发展,由于农药使用量的增加,农药残留问题越来越严重,对环境生态和人们的健康带来很大的影响。除了加快研发高效、低毒的新型农药产品外,通过改进现有农药的剂型和配方,充分发挥现有农药药效,也是现代农业持续发展和环境保护的另一有效途径。
甲氨基阿维菌素苯甲酸盐(简称甲维盐)是通过阿维菌素的半合成获得的一种大环内酯化合物。作为一种生物农药,它具有超高效,低毒,无污染的特点,已广泛应用于全球水稻,蔬菜,果树,棉花等作物的鳞翅目害虫防治。然而,由于在其分子中存在共轭二烯双键结构,当暴露于阳光下它很容易被光解而失去原有药效。因此,为了减缓其光降解作用,在甲氨基阿维菌素苯甲酸盐制剂中往往加入一些抗氧化剂或防晒剂,以提高其抗光解性能。但结果表明这些方法只能适当改善甲氨基阿维菌素苯甲酸盐制剂的光稳定性,并不足以更有效地提高其抗光解性能,同时还进一步增加了制剂成本。
纳米农药由于具有优良的溶解润湿性、抗光解、抗氧化性、叶面沾附及对目标昆虫渗透性等优点,为提高农药的生物利用度提供了一条有效途径。发明专利CN103931611A公开了一种含有纳米甲维盐颗粒混悬液及其制备方法,根据该方法制备得到的甲维盐颗粒形貌为较规则的类球形,粒径为纳米级。发明专利CN106417269A公开了一种脂溶性农药的水基型纳米粒子水分散制剂及其制备方法,此方法可应用于农药阿维菌素。然而以上所公开的甲维盐纳米制剂或存在载药量低、难以产业化,或制备工艺复杂、成本高,或抗光解能力较弱等缺点。
发明专利CN109006845A公开了一种甲维盐纳米颗粒抗光解缓释农药及制备方法,该甲维盐纳米颗粒农药的主要成分为甲维盐和木质素磺酸盐,具有很好的抗光解能力和缓释能力,且该制备方法的工艺简单,主要溶剂为水,价格低廉,以及设备投资小,生产成本低。但是该甲维盐纳米颗粒农药在温度响应特性、杀虫持效性和内吸传导性等方面存在不足,使得农药的选择性、持效性等效果不好,难以实现减施增效的目的。因此,有必要研究出一种具备抗光解能力和缓释能力,且同时具备优异的内吸传导性、温度响应特性和杀虫持效性的甲维盐纳米颗粒农药。
海藻酸钠是一种天然多糖,是从褐藻类的海带或马尾藻中提取碘和甘露醇之后的副产物,其分子由β-D-甘露糖醛酸(β-D-mannuronic,M)和α-L-古洛糖醛酸(α-L-guluronic,G)按(1→4)键连接而成。海藻酸钠已经在食品工业和医药领域得到广泛应用。近年来发现海藻酸钠还是一种农业优质增产剂,它具有刺激植物体内防御酶活性,增强植物对环境的抗变能力,均衡调节植物生长及促进植物根系和种子发育的功效。通过海藻酸或海藻酸钠的结构修饰可以得到不同的功能化产物,实现不同的用途。
近年来,以海藻酸钠作为纳米农药制剂制备中的农药分子载体,取得了一些研究成果。如利用海藻酸钠为载体,氯化钙作为交联剂,制备农药吡虫啉、啶虫脒和氯氰菊酯纳米制剂,研究结果表明纳米制剂比普通制剂具有更好的杀虫活性和缓释性能。通过海藻酸钠制备纳米制剂,一般是利用油滴界面上的络合形成海藻酸盐纳米胶囊,或利用水溶液中的络合形成海藻酸盐纳米团聚体的方式进行。
然而目前还没发现有海藻酸钠与甲维盐制成纳米制剂的相关报道,因此,本申请提供一种甲维盐-海藻酸钠纳米制剂,该纳米制剂的制备是利用海藻酸钠中的羧基负离子和甲维盐中的甲氨基正离子的静电吸引去自组装形成纳米颗粒,使得该纳米制剂具备抗光解能力和缓释能力的同时,还具备优异的内吸传导性、温度响应特性和杀虫持效性。
发明内容
针对以上问题,本发明提供一种甲维盐-海藻酸钠纳米颗粒缓释农药及其制备方法,该甲维盐-海藻酸钠纳米颗粒缓释农药具有很好的抗光解性能、缓释功效,以及同时具备优异的内吸传导性、温度响应特性和杀虫持效性,且该制备方法工艺过程简单、生产成本低。
本发明通过以下技术方案实现:
一种甲维盐-海藻酸钠纳米颗粒缓释农药,包括如下重量份数的原料:甲维盐1-15份、固体成粒剂0.5-6份、表面活性剂1-10份、分散剂0.5-10份;其中,固体成粒剂为海藻酸钠。
作为技术方案的优选,所述表面活性剂为非离子表面活性剂吐温、司本、BY-125、卵磷脂、烷基酚聚氧乙烯醚、乳化剂603、高碳脂肪醇聚氧乙烯醚、脂肪酸聚氧乙烯酯、蓖麻油聚氧乙烯醚、聚氧乙烯烷基胺、失水山梨醇酯、蔗糖酯、聚氧乙烯烷基醇酰胺、苯乙烯基苯酚聚氧乙烯醚、聚醚中的任一种或几种。
作为技术方案的优选,所述表面活性剂为离子型表面活性剂聚丙烯酰胺、烷基苯磺酸钠、烷基硫酸酯盐、烷基磷酸酯盐中的任一种或几种。
作为技术方案的优选,所述分散剂为甲壳素、阿拉伯树胶、黄原胶、甲基纤维素、羧甲基纤维素钠、羟乙基纤维素、羟丙基淀粉醚、羟丙基二淀粉磷酸酯、乙酰化二淀粉磷酸酯、NS-500LQ、J-601、达润DSV、SP-SC29、明胶、大豆蛋白胶、聚丙烯酰胺、聚乙烯醇、聚乙烯吡咯烷酮、聚氧化乙烯、聚丙烯酸酯共聚乳液中的任一种或几种。
一种如上所述的甲维盐-海藻酸钠纳米颗粒缓释农药的制备方法,按照重量份数称取原料,并按照如下步骤制备:
(1)将固体成粒剂溶解于水中,搅拌至完全溶解,得到固体成粒剂溶液;
(2)将步骤(1)的固体成粒剂溶液加热至50-80℃,然后加入表面活性剂,经高速搅拌乳化10-60min后,得到固体成粒剂乳液;
(3)将甲维盐溶解于有机溶剂中,搅拌至完全溶解,得到甲维盐溶液;
(4)将步骤(3)的甲维盐溶液在高速搅拌下逐渐加入步骤(2)的固体成粒剂乳液中,继续搅拌10-120min,得到混合物;
(5)将步骤(4)得到的混合物低温超声分散10-120min,然后加入分散剂,经高速搅拌10-60min后,得到甲维盐-海藻酸钠纳米颗粒缓释农药。
作为技术方案的优选,步骤(3)中,所述有机溶剂为二氯甲烷、乙酸乙酯、乙酸仲丁酯、乙酸异丁酯、乙酸正丁酯、环己酮、邻苯二甲酸苄丁酯、邻苯二甲酸二乙酯、邻苯二甲酸二甲酯、二乙二醇丁醚、二乙二醇乙醚、二乙二醇甲醚、四氢呋喃、正己烷、环己酮、乙腈、二甲苯、杜邦DBE、索尔维Green25、索尔维ADMA810、POLARCLEAN、RPDE、二甲亚砜、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、癸酰胺、叔丁基甲基醚、异丙醚、石蜡油、石脑油、溶剂油、植物油中的任一种或几种。
作为技术方案的优选,步骤(5)中,所述低温超声分散为将混合物在0-5℃、650W的超声粉碎仪中进行分散。
与现有技术相比,本发明的优点及有益效果为:
1、现有技术利用海藻酸钠制备纳米农药采用的技术是交联包裹技术,过程中要加入交联剂,如氯化钙、戊二醛等。而本发明利用带正电荷的甲维盐阳离子和带负电荷的海藻酸钠阴离子通过电荷吸引自组装的方式结合构成甲维盐-海藻酸钠纳米颗粒,然后再加入分散剂使制剂进一步稳定,制备出一种基于正负电荷吸引而形成的甲维盐-海藻酸钠纳米颗粒缓释农药。由于甲维盐被海藻酸钠吸附包裹,减缓了它的溶解析出及光照,因此该甲维盐-海藻酸钠纳米颗粒缓释农药具有很好的抗光解性能、缓释功效,此外,该纳米制剂还具备优异的内吸传导性、温度响应特性和杀虫持效性。申请人在研发实验中同时表明:本发明利用带正电荷的甲维盐阳离子和带负电荷的海藻酸钠阴离子通过电荷吸引自组装的方式结合构成甲维盐-海藻酸钠纳米颗粒的原理仅仅适用于农药甲维盐,不适用于其它活性农药。海藻酸钠与其它农药分子通过交联形成的纳米农药也会具备抗光解及缓释性能,但是不能够增强农药的内吸性。
2、本发明的甲维盐-海藻酸钠纳米颗粒缓释农药的基本基质材料是来源于植物的天然海藻酸制备得到的海藻酸钠,分子具有很强的亲水性,对甲维盐包裹形成甲维盐-海藻酸钠纳米颗粒后,可以大大提高甲维盐原药的內吸传导性。采用“内吸活性试验—连续浸液法”(NY/T1154.4-2006)对本发明的甲维盐-海藻酸钠纳米颗粒缓释农药进行内吸传导性测试的结果表明,本发明的甲维盐-海藻酸钠纳米制剂具有很好的植物体内的内吸传导性。甲维盐-海藻酸钠纳米制剂中甲维盐纳米颗粒具有非常好内吸传导性的主要原因是:一方面由于甲维盐-海藻酸钠纳米制剂中的甲维盐纳米颗粒粒径很小,仅为30-50纳米,有利于甲维盐纳米颗粒在植物中的渗透;另一方面是由于海藻酸钠是一种内源性植物高分子,其结构中存在大量的羟基,在植物内部羟基与水分子形成分子间氢键,然后通过植物中水分子的蒸腾作用,实现将纳米颗粒转运到植物不同部位的效果。这样,就大大增强了甲维盐的内吸传导性。农药能被作物很好地吸收并在体内传导,可以增强农药对目标靶点害虫的选择性,提高农药防治病虫害的效果。
3、本发明的测试结果表明,本发明的甲维盐-海藻酸钠纳米制剂具备优异的温度响应释放特性,其中的甲维盐成分的释放与温度呈正相关,由于本发明的甲维盐-海藻酸钠纳米制剂是通过甲维盐与海藻酸钠的静电吸附形成,温度升高有利于它们的解离,因此释放速率与温度呈正相关,温度升高有利于纳米颗粒中甲维盐与海藻酸钠的解离释放,而温度升高也是害虫增加的活跃期,此时纳米制剂中甲维盐的释放速度加快有利于杀虫效率的提高,达到延长持效期、减少用药次数、提高农药有效利用率的目的,实现农药的减施增效,具有高效、持效、环保和低用量的优点。
4、本发明的甲维盐-海藻酸钠纳米颗粒缓释农药的基本基质材料是海藻酸钠,海藻酸钠在农业上具有促进农作物生长的作用,同时也是一种绿色环保无害的天然高分子材料,资源丰富,成本低廉,可生物降解,具有很好的经济效益和环保效益。
5、本发明的甲维盐-海藻酸钠纳米颗粒缓释农药的制备方法具有工艺过程简单,设备投资小,生产过程无三废产生的优点,以及该方法所用的溶剂主要为水,价格低廉环保。
附图说明
图1为甲维盐-海藻酸钠纳米颗粒缓释农药制剂的透射电镜分析图。
图2为甲维盐-海藻酸钠纳米颗粒缓释农药制剂在25℃下的释放曲线图。
图3为甲维盐-海藻酸钠纳米颗粒缓释农药制剂在45℃下的释放曲线图。
图4为甲维盐-海藻酸钠纳米颗粒缓释农药制剂在25℃和45℃的释放曲线对比图。
图5为甲维盐-海藻酸钠纳米颗粒缓释农药制剂抗紫外光分解曲线图。
图6为甲维盐-海藻酸钠纳米颗粒缓释农药制剂对黏虫的杀虫持效性柱形图。
图7为甲维盐-海藻酸钠纳米颗粒缓释农药制剂在玉米中的内吸传导性柱形图。
图8为不同浓度甲维盐-海藻酸钠纳米颗粒缓释农药制剂浸泡玉米根24小时后所采集玉米叶对三龄期玉米螟的杀虫致死率柱形图。
图2、图3、图4、图5、图6、图7和图8中的EB-SA为甲维盐-海藻酸钠纳米颗粒缓释农药制剂,EB-EC为普通甲维盐乳油。
具体实施方式
下面通过实施例对本发明做进一步地详细说明,这些实施例仅用来说明本发明,并不限制本发明的保护范围。
实施例1制备1%甲维盐-海藻酸钠纳米颗粒缓释农药制剂
1%甲维盐-海藻酸钠纳米颗粒缓释农药制剂的制备步骤如下:
(1)将食品级海藻酸钠0.7Kg溶解于81.8Kg水中,经搅拌3h完全溶解后,得到海藻酸钠溶液;
(2)将步骤(1)的海藻酸钠溶液加热至70℃,然后加入3.0Kg乳化剂吐温-60,继续高速搅拌乳化20min后,得到海藻酸钠乳液;
(3)将1.5Kg含量71%的甲维盐溶解于5Kg乙酸仲丁酯和5Kg N,N-二甲基乙酰胺组成的混合有机溶剂中,搅拌至完全溶解,得到甲维盐溶液;
(4)将步骤(3)的甲维盐溶液在高速搅拌下逐渐加入步骤(2)的海藻酸钠乳液中,继续搅拌20min,得到混合物;
(5)将步骤(4)得到的混合物低温超声分散25min,然后加入分散剂达润DSV3.0Kg,经高速搅拌30min后,得到稳定的含量1%甲维盐-海藻酸钠纳米颗粒缓释农药制剂。
实施例2制备3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂
3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂的制备步骤如下:
(1)将食品级海藻酸钠1.2Kg溶解于75.3Kg水中,经搅拌5h完全溶解后,得到海藻酸钠溶液;
(2)将步骤(1)的海藻酸钠溶液加热至70℃,然后加入4.0Kg乳化剂司本-20,继续高速搅拌乳化25min后,得到海藻酸钠乳液;
(3)将4.4Kg含量71%的甲维盐溶解于6Kg乙酸异丁酯和6Kg邻苯二甲酸苄丁酯组成的混合有机溶剂中,搅拌至完全溶解,得到甲维盐溶液;
(4)将步骤(3)的甲维盐溶液在高速搅拌下逐渐加入步骤(2)的海藻酸钠乳液中,继续搅拌30min,得到混合物;
(5)将步骤(4)得到的混合物低温超声分散25min,然后加入分散剂SP-SC293.5Kg,经高速搅拌30min后,得到稳定的含量3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂。
实施例3制备5%甲维盐-海藻酸钠纳米颗粒缓释农药制剂
5%甲维盐-海藻酸钠纳米颗粒缓释农药制剂的制备步骤如下:
(1)将食品级海藻酸钠1.3Kg溶解于68.5Kg水中,经搅拌4h完全溶解后,得到海藻酸钠溶液;
(2)将步骤(1)的海藻酸钠溶液加热至70℃,然后加入4.0Kg乳化剂BY-125,继续高速搅拌乳化20min后,得到海藻酸钠乳液;
(3)将7.2Kg含量71%的甲维盐溶解于7Kg乙酸乙酯和8Kg环己酮组成的混合有机溶剂中,搅拌至完全溶解,得到甲维盐溶液;
(4)将步骤(3)的甲维盐溶液在高速搅拌下逐渐加入步骤(2)的海藻酸钠乳液中,继续搅拌20min,得到混合物;
(5)将步骤(4)得到的混合物低温超声分散25min,然后加入分散剂J-601 4.0Kg,经高速搅拌40min后,得到稳定的含量5%甲维盐-海藻酸钠纳米颗粒缓释农药制剂。
实施例4制备7%甲维盐-海藻酸钠纳米颗粒缓释农药制剂
7%甲维盐-海藻酸钠纳米颗粒缓释农药制剂的制备步骤如下:
(1)将食品级海藻酸钠1.6Kg溶解于62.1Kg水中,经搅拌5h完全溶解后,得到海藻酸钠溶液;
(2)将步骤(1)的海藻酸钠溶液加热至80℃,然后加入4.8Kg乳化剂603,继续高速搅拌乳化20min后,得到海藻酸钠乳液;
(3)将7.2Kg含量71%的甲维盐溶解于7Kg乙酸乙酯和8Kg二乙二醇丁醚组成的混合有机溶剂中,搅拌至完全溶解,得到甲维盐溶液;
(4)将步骤(3)的甲维盐溶液在高速搅拌下逐渐加入步骤(2)的海藻酸钠乳液中,继续搅拌40min,得到混合物;
(5)将步骤(4)得到的混合物低温超声分散50min,然后加入分散剂NS-500LQ4.8Kg,经高速搅拌60min后,得到稳定的含量7%甲维盐-海藻酸钠纳米颗粒缓释农药制剂。
实施例5制备10%甲维盐-海藻酸钠纳米颗粒缓释农药制剂
10%甲维盐-海藻酸钠纳米颗粒缓释农药制剂的制备步骤如下:
(1)将食品级海藻酸钠1.8Kg溶解于51.4Kg水中,经搅拌8h完全溶解后,得到海藻酸钠溶液;
(2)将步骤(1)的海藻酸钠溶液加热至80℃,然后加入5.0Kg蔗糖酯,继续高速搅拌乳化60min后,得到海藻酸钠乳液;
(3)将14.3Kg含量71%的甲维盐溶解于12Kg N,N-二甲基乙酰胺和10Kg环己酮组成的混合有机溶剂中,搅拌至完全溶解,得到甲维盐溶液;
(4)将步骤(3)的甲维盐溶液在高速搅拌下逐渐加入步骤(2)的海藻酸钠乳液中,继续搅拌72min,得到混合物;
(5)将步骤(4)得到的混合物低温超声分散50min,然后加入分散剂聚乙烯醇5.5Kg,经高速搅拌60min后,得到稳定的含量10%甲维盐-海藻酸钠纳米颗粒缓释农药制剂。
一、甲维盐-海藻酸钠纳米颗粒缓释农药制剂的透射电镜分析
将实施例1、实施例2、实施例3、实施例4和实施例5制备的甲维盐-海藻酸钠纳米颗粒缓释农药制剂用蒸馏水稀释至1%的溶液,用1mL一次性注射器吸取液体一滴滴到含有碳支持膜的铜网上,用3%的磷钨酸染色,在室温下自然风干,将样品放入透射电子显微镜(日立医疗系统(苏州)有限公司,型号:HT7700)样品室中,进行观察和拍照。结果见图1,图1为甲维盐-海藻酸钠纳米颗粒缓释农药制剂的透射电镜分析图。
从图1中可以看到,制剂中甲维盐-海藻酸钠为球形颗粒,表面光滑,粒径在20-50nm之间。
二、甲维盐-海藻酸钠纳米颗粒缓释农药制剂中甲维盐成分释放试验
采用透析袋扩散法测定纳米制剂的甲维盐释放曲线。称量一定量的实施例2制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品放入透析袋(北京格林博远生物科技有限公司,MD10 mm),以相应的普通3%的甲维盐乳油作为对照,然后加入几颗小玻璃珠,两端用绳子扎紧,放入100mL的敞口瓶。往瓶中加入100mL的50%甲醇水混合溶剂,每个样品平行三个样,然后置于预设置温度的摇床中(转速180r/min)。在预先设定的时间间隔进行取样,每次取样后更换新鲜溶剂,放回摇床中重新释放。释出液采用紫外可见光谱仪(岛津企业管理(中国)有限公司,型号:UV-2600)测定溶液的吸光度,通过标准曲线换算出甲维盐含量。对样品的累积释放率,采用计算公式(1)来计算:
Q:累积释放率;
W:样品中甲维盐的总重量(mg);
V:每次取样的体积(100mL);
Ct:每次取样样品中甲维盐浓度(mg/mL)。
对实施例2制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品进行测试,普通3%的甲维盐乳油作为对照样,50%的甲醇水作为缓释溶剂,结果见图2和图3,图2为甲维盐-海藻酸钠纳米颗粒缓释农药制剂在25℃下的释放曲线图,图3为甲维盐-海藻酸钠纳米颗粒缓释农药制剂在45℃下的释放曲线图。
从图2中可以看到,在常温即25℃时,甲维盐-海藻酸钠纳米颗粒缓释农药制剂(EB-SA)具有很好的缓释效果。从图3中可以看出,当温度增加到45℃时,释放速度加快,说明该制剂的释放速率具有温度响应的特性。图4是甲维盐-海藻酸钠纳米颗粒缓释农药制剂(EB-SA)在T=25℃和T=45℃温度时的释放行为对比。从图中可以看到,在45℃时EB-SA中甲维盐具有较快的释放速率。45℃时,EB-SA纳米制剂释放20h时已经释放甲维盐约70%,而在25℃时释放20h时甲维盐释放率仅为30%,说明释放速率具有热效应特性,温度越高,释放速率越快。这是由于温度的升高,促进了海藻酸钠与甲维盐分子之间的解离,从而使释放速率大大加快。
三、甲维盐-海藻酸钠纳米颗粒缓释农药制剂抗紫外光分解试验
将实施例2制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品用去离子水稀释至2mg/mL,以相应的普通3%的甲维盐乳油悬浮剂作为对照。然后以每孔1mL的量加入到24孔培养板中,用透明塑料薄膜密封培养板,将培养板置于40W UV灯下以45cm的距离照射。在预先设计的时间间隔收集照射样品,在甲醇中稀释,并转移至10mL容量瓶中,定容至刻度。分别取样通过紫外可见光谱分析其中甲维盐的含量,计算不同时间节点甲维盐的分解率,并以此作出甲维盐分解率-时间的动力学曲线。
对实施例2制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品进行测试,普通3%的甲维盐乳油悬浮剂作为对照样,稀释浓度为2mg/mL,用紫外灯模拟太阳光照射做抗光解测试。结果见图5,图5为甲维盐-海藻酸钠纳米颗粒缓释农药制剂(EB-SA)抗紫外光分解曲线图。从图5可以看出,甲维盐-海藻酸钠纳米颗粒缓释农药制剂具有较好的抗光解能力,其光解半衰期T0.5比对照组普通甲维盐乳油悬浮剂提高一倍以上。
四、甲维盐-海藻酸钠纳米颗粒缓释农药制剂温室杀虫持效性测试
将适量土壤置于28×20cm塑料盆中,然后每个盆中种植玉米种子5颗,每2天浇水一次。植物在温室中生长15天后,在不同的时间间隔用刷子将实施例2制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品和对照样普通3%的甲维盐乳油均匀涂抹在叶子上,其中3盆作为空白对照而没有喷施药剂。最后,收集试验植物的叶子,剪切成5-6cm长的小叶片,进一步转移到培养盒中供试虫取食(每个培养皿放置2-3张小叶片),用具有小孔的塑料盖密封。培养盒置于害虫防治室中饲养(光/暗=16:8,温度=25±2℃,相对湿度=75±5%),48h后调查虫子的死亡率。计算公式如下:
采用实施例2的制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品进行测试,对照样是普通3%甲维盐乳油。以黏虫(三龄中末期)作为靶点害虫,施药浓度为20ppm,施药后在1,4,8,12,16和20天的时段分析药剂对黏虫的致死率,结果见图6,图6为甲维盐-海藻酸钠纳米颗粒缓释农药制剂对黏虫的杀虫持效性图。
从图6可以明显地看到,在施药第四天后,甲维盐-海藻酸钠纳米颗粒缓释农药制剂(EB-SA)对黏虫的致死率明显高于对照样3%甲维盐乳油(EB-EC),在20天时,该制剂还保持有80%以上的杀虫效果,而对照样的杀虫致死率却不到50%。因此可见,本发明的甲维盐-海藻酸钠纳米颗粒缓释农药制剂对靶点害虫具有较长的杀虫持效期。
五、甲维盐-海藻酸钠纳米颗粒缓释农药制剂内吸传导性测试
将玉米种植在28×20cm的塑料盆中,在温室中生长25天后开始实验。在不同时间间隔用刷子将实施例2制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品均匀涂抹在玉米叶片下方的根、茎部(不接触叶片),每个样品重复涂抹三盆。以普通3%的甲维盐乳油作为对照,设3盆作为空白对照,不施处理。最后采集试验植物的所有叶片,采用液相串联质谱法测定其中甲维盐的含量。
采用实施例2的制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品进行测试,施药浓度为100ppm,对照样是3%的普通甲维盐乳油。施药部位在玉米的根部位置,在施药后的不同时间节点(3、7、11、15天)收集玉米叶测定其中甲维盐含量,结果见图7,图7为甲维盐-海藻酸钠纳米颗粒缓释农药制剂在玉米中的内吸传导性图。
由图7中结果可以看到,甲维盐-海藻酸钠纳米颗粒缓释农药制剂(EB-SA)在玉米植株中具有很好的內吸传导性,在15天时,其含量达到0.2mg/Kg,大约为对照样(EB-EC)的3倍,说明甲维盐-海藻酸钠纳米颗粒缓释农药制剂使甲维盐的内吸传导性得到大大增强。
六、不同浓度甲维盐-海藻酸钠纳米颗粒缓释农药制剂在玉米中内吸性测定
测试方法参考中华人民共和国农业行业标准农药室内生物测定试验准则“内吸活性试验—连续浸液法”(NY/T 1154.4-2006)方法进行。首先,挖取生长期15天的玉米苗,将根部洗净备用。然后,用去离子水将实施例2的制备的3%甲维盐-海藻酸钠纳米颗粒缓释农药制剂样品分别稀释成为200、100、50、25和12.5ppm五个不同浓度,取不同浓度溶液各120mL置于聚乙烯塑料杯中,每个浓度设置3个平行样,同时以相应浓度的普通甲维盐乳油作为对照。接着,将玉米苗的根部浸入不同浓度的待测试液中(每个样品试液中放置3棵玉米苗,注意叶子不能接触溶液),去离子水作为空白对照。待玉米苗根部在试液中浸液24小时后,取出玉米苗,将未接触制剂的玉米叶剪断,然后给三龄期的玉米螟喂食,在养虫室培育48h后调查虫子的死亡情况,计算不同浓度下玉米螟的致死率。
图8为甲维盐-海藻酸钠纳米颗粒缓释农药制剂和普通甲维盐乳油在不同浓度稀释液浸泡玉米根24小时后玉米叶对玉米螟的致死率结果。可以看到,与对照样甲维盐乳油(EB-EC)比较,甲维盐-海藻酸钠纳米颗粒缓释农药制剂(EB-SA)具有非常好的内吸传导性。在50-200ppm的浸泡浓度范围内,EB-SA对玉米螟的杀虫致死率基本高于90%,而对照样EB-EC的致死率不到20%,说明EB-SA具有非常强的内吸传导性。特别是在12.5ppm的低浓度溶液中,对照EB-EC对玉米螟的杀虫致死率仅为4.7%,而纳米甲维盐制剂EB-SA的致死率为59%。甲维盐与海藻酸钠形成纳米制剂后,甲维盐(EB)的内吸传导性得到大大增强。对于对照EB-EC来说,在50ppm的浸泡浓度时,EB的内吸传导性最高,对玉米螟达到17.9%的杀虫致死率,由此可见甲维盐本身也具有一定的内吸传导性。但是,当与海藻酸钠结合形成纳米颗粒后,甲维盐的内吸传导性得到大大增强。
Claims (7)
1.一种甲维盐-海藻酸钠纳米颗粒缓释农药,其特征在于,包括如下重量份数的原料:甲维盐1-15份、固体成粒剂0.5-6份、表面活性剂1-10份、分散剂0.5-10份;其中,固体成粒剂为海藻酸钠。
2.根据权利要求1所述的甲维盐-海藻酸钠纳米颗粒缓释农药,其特征在于,所述表面活性剂为非离子表面活性剂吐温、司本、BY-125、卵磷脂、烷基酚聚氧乙烯醚、乳化剂603、高碳脂肪醇聚氧乙烯醚、脂肪酸聚氧乙烯酯、蓖麻油聚氧乙烯醚、聚氧乙烯烷基胺、失水山梨醇酯、蔗糖酯、聚氧乙烯烷基醇酰胺、苯乙烯基苯酚聚氧乙烯醚、聚醚中的任一种或几种。
3.根据权利要求1所述的甲维盐-海藻酸钠纳米颗粒缓释农药,其特征在于,所述表面活性剂为离子型表面活性剂聚丙烯酰胺、烷基苯磺酸钠、烷基硫酸酯盐、烷基磷酸酯盐中的任一种或几种。
4.根据权利要求1所述的甲维盐-海藻酸钠纳米颗粒缓释农药,其特征在于,所述分散剂为甲壳素、阿拉伯树胶、黄原胶、甲基纤维素、羧甲基纤维素钠、羟乙基纤维素、羟丙基淀粉醚、羟丙基二淀粉磷酸酯、乙酰化二淀粉磷酸酯、NS-500LQ、J-601、达润DSV、SP-SC29、明胶、大豆蛋白胶、聚丙烯酰胺、聚乙烯醇、聚乙烯吡咯烷酮、聚氧化乙烯、聚丙烯酸酯共聚乳液中的任一种或几种。
5.一种如权利要求1-4任一所述的甲维盐-海藻酸钠纳米颗粒缓释农药的制备方法,其特征在于,按照重量份数称取原料,并按照如下步骤制备:
(1)将固体成粒剂溶解于水中,搅拌至完全溶解,得到固体成粒剂溶液;
(2)将步骤(1)的固体成粒剂溶液加热至50-80℃,然后加入表面活性剂,经搅拌乳化10-60min后,得到固体成粒剂乳液;
(3)将甲维盐溶解于有机溶剂中,搅拌至完全溶解,得到甲维盐溶液;
(4)将步骤(3)的甲维盐溶液在高速搅拌下逐渐加入步骤(2)的固体成粒剂乳液中,继续搅拌10-120min,得到混合物;
(5)将步骤(4)得到的混合物低温超声分散10-120min,然后加入分散剂,经搅拌10-60min后,得到甲维盐-海藻酸钠纳米颗粒缓释农药。
6.根据权利要求5所述的甲维盐-海藻酸钠纳米颗粒缓释农药的制备方法,其特征在于,步骤(3)中,所述有机溶剂为二氯甲烷、乙酸乙酯、乙酸仲丁酯、乙酸异丁酯、乙酸正丁酯、环己酮、邻苯二甲酸苄丁酯、邻苯二甲酸二乙酯、邻苯二甲酸二甲酯、二乙二醇丁醚、二乙二醇乙醚、二乙二醇甲醚、四氢呋喃、正己烷、环己酮、乙腈、二甲苯、杜邦DBE、索尔维Green25、索尔维ADMA810、POLARCLEAN、RPDE、二甲亚砜、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、癸酰胺、叔丁基甲基醚、异丙醚、石蜡油、石脑油、溶剂油、植物油中的任一种或几种。
7.根据权利要求5所述的甲维盐-海藻酸钠纳米颗粒缓释农药的制备方法,其特征在于,步骤(5)中,所述低温超声分散为将混合物在0-5℃、650W的超声粉碎仪中进行分散。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210583915.4A CN114885953B (zh) | 2022-05-27 | 2022-05-27 | 一种甲维盐-海藻酸钠纳米颗粒缓释农药及其制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210583915.4A CN114885953B (zh) | 2022-05-27 | 2022-05-27 | 一种甲维盐-海藻酸钠纳米颗粒缓释农药及其制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN114885953A true CN114885953A (zh) | 2022-08-12 |
CN114885953B CN114885953B (zh) | 2024-08-23 |
Family
ID=82726461
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210583915.4A Active CN114885953B (zh) | 2022-05-27 | 2022-05-27 | 一种甲维盐-海藻酸钠纳米颗粒缓释农药及其制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114885953B (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115843794A (zh) * | 2022-12-13 | 2023-03-28 | 贵州大学 | 植物蛋白基包载药物分子的纳米体系及制备方法与应用 |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2006058478A1 (fr) * | 2004-12-03 | 2006-06-08 | Wuhan Green-Century Bioengineering Company Ltd. | Granules hydrodispersibles d’abamectine ou de ses dérivés, et méthodes de production desdits granules |
CN101455197A (zh) * | 2008-08-14 | 2009-06-17 | 迟德富 | 光降解纳米吡虫啉微胶囊制备方法 |
CN103444705A (zh) * | 2013-07-26 | 2013-12-18 | 青岛艾华隆生物科技有限公司 | 一种缓释高效生物杀虫剂及其制备方法 |
CN104872170A (zh) * | 2015-06-11 | 2015-09-02 | 福建农林大学 | 高效氯氟氰菊酯甲氨基阿维菌素苯甲酸盐微球水分散粒剂 |
CN108684690A (zh) * | 2018-07-27 | 2018-10-23 | 福建农林大学 | 一种可生物降解材料载农药微球悬浮剂及其制备方法 |
CN109006845A (zh) * | 2018-08-27 | 2018-12-18 | 广西田园生化股份有限公司 | 一种甲维盐纳米颗粒抗光解缓释农药及制备方法 |
CN114176072A (zh) * | 2021-11-10 | 2022-03-15 | 河北兴柏农业科技有限公司 | 一种甲维盐b2悬浮剂及制备方法 |
-
2022
- 2022-05-27 CN CN202210583915.4A patent/CN114885953B/zh active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2006058478A1 (fr) * | 2004-12-03 | 2006-06-08 | Wuhan Green-Century Bioengineering Company Ltd. | Granules hydrodispersibles d’abamectine ou de ses dérivés, et méthodes de production desdits granules |
CN101455197A (zh) * | 2008-08-14 | 2009-06-17 | 迟德富 | 光降解纳米吡虫啉微胶囊制备方法 |
CN103444705A (zh) * | 2013-07-26 | 2013-12-18 | 青岛艾华隆生物科技有限公司 | 一种缓释高效生物杀虫剂及其制备方法 |
CN104872170A (zh) * | 2015-06-11 | 2015-09-02 | 福建农林大学 | 高效氯氟氰菊酯甲氨基阿维菌素苯甲酸盐微球水分散粒剂 |
CN108684690A (zh) * | 2018-07-27 | 2018-10-23 | 福建农林大学 | 一种可生物降解材料载农药微球悬浮剂及其制备方法 |
CN109006845A (zh) * | 2018-08-27 | 2018-12-18 | 广西田园生化股份有限公司 | 一种甲维盐纳米颗粒抗光解缓释农药及制备方法 |
CN114176072A (zh) * | 2021-11-10 | 2022-03-15 | 河北兴柏农业科技有限公司 | 一种甲维盐b2悬浮剂及制备方法 |
Non-Patent Citations (1)
Title |
---|
卢晶;罗华超;张琼;方桂珍;任世学;: "木质素季铵盐-海藻酸钠聚合物负载阿维菌素粉体的制备及抗紫外光性能分析", 生物质化学工程, no. 03, pages 201 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115843794A (zh) * | 2022-12-13 | 2023-03-28 | 贵州大学 | 植物蛋白基包载药物分子的纳米体系及制备方法与应用 |
CN115843794B (zh) * | 2022-12-13 | 2024-03-01 | 贵州大学 | 植物蛋白基包载药物分子的纳米体系及制备方法与应用 |
Also Published As
Publication number | Publication date |
---|---|
CN114885953B (zh) | 2024-08-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Guo et al. | Preparation and characterization of enzyme-responsive emamectin benzoate microcapsules based on a copolymer matrix of silica–epichlorohydrin–carboxymethylcellulose | |
CN110946133B (zh) | 一种以木质素为包裹基质的纳米抗光解控释农药及其制备方法 | |
CN110622965B (zh) | 一种基于单宁酸修饰的叶面亲和型农药纳米微胶囊制备方法 | |
CN113575243B (zh) | 一种液体水果套袋材料、其制备方法及应用 | |
CN115039770B (zh) | 一种用于松材线虫防治的pH响应型自荧光纳米农药载体及制备方法、纳米农药和应用 | |
CN110663685A (zh) | 一种介孔二氧化硅负载ppte的纳米农药制剂 | |
CN102885060A (zh) | 一种阿维菌素纳米微乳剂及其制备方法 | |
CN112841218A (zh) | 一种采用纳米硅量子点防治玉米粘虫的方法 | |
CN107372524B (zh) | 一种含唑虫酰胺和甲氨基阿维菌素苯甲酸盐的农药悬浮剂及其应用 | |
CN102919221A (zh) | 纳米二氧化硅在农药控释中的应用 | |
CN114885953A (zh) | 一种甲维盐-海藻酸钠纳米颗粒缓释农药及其制备方法 | |
CN111165481A (zh) | 一种特定结构硅藻土-阿维菌素农药组合物及其应用 | |
CN113367130B (zh) | 一种用于金银花的杀虫剂复配载药微球及其制备方法 | |
CN104255808A (zh) | 一种蜡蚧菌油剂及其制备方法和在防治农业害虫中的作用 | |
CN110074143A (zh) | 一种引诱茶籽象甲成虫的组合物及其制备方法 | |
Wang et al. | Three-dimensional dendritic biosynthetic copper oxide nanoparticles: A novel approach for enhanced leaf deposition and retention to reduce environmental impact | |
CN116195589A (zh) | 一种云杉八齿小蠹成虫的驱避剂及其应用 | |
CN114208840A (zh) | 一种甲维盐·茚虫威悬浮剂及其制备方法 | |
CN111202083A (zh) | 一种特定结构硅藻土-阿维菌素水分散粒剂及其应用 | |
CN111328802A (zh) | 一种以聚乙烯蜡为包裹基质的纳米控释农药及其制备方法 | |
CN116897939B (zh) | Ro6889678-l-酒石酸在制备白蚁灭杀剂中的应用 | |
CN116602297B (zh) | 一种纳米化茉莉酸甲酯及其制备方法和应用 | |
CN115176808B (zh) | 一种环境敏感型氯虫苯甲酰胺缓释剂的制备方法及应用 | |
CN116831133B (zh) | 甲氨基阿维菌素苯甲酸盐水分散粒剂及其制备方法 | |
CN115530163B (zh) | 一种酶响应纳米农药及制备方法与应用 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |