CN114097813B - Suspending agent containing indoxacarb and methoxyfenozide and preparation method thereof - Google Patents
Suspending agent containing indoxacarb and methoxyfenozide and preparation method thereof Download PDFInfo
- Publication number
- CN114097813B CN114097813B CN202111519017.4A CN202111519017A CN114097813B CN 114097813 B CN114097813 B CN 114097813B CN 202111519017 A CN202111519017 A CN 202111519017A CN 114097813 B CN114097813 B CN 114097813B
- Authority
- CN
- China
- Prior art keywords
- agent
- methoxyfenozide
- indoxacarb
- dispersant
- percent
- 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.)
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Links
- 239000005907 Indoxacarb Substances 0.000 title claims abstract description 72
- VBCVPMMZEGZULK-NRFANRHFSA-N indoxacarb Chemical compound C([C@@]1(OC2)C(=O)OC)C3=CC(Cl)=CC=C3C1=NN2C(=O)N(C(=O)OC)C1=CC=C(OC(F)(F)F)C=C1 VBCVPMMZEGZULK-NRFANRHFSA-N 0.000 title claims abstract description 72
- 239000005917 Methoxyfenozide Substances 0.000 title claims abstract description 66
- QCAWEPFNJXQPAN-UHFFFAOYSA-N methoxyfenozide Chemical compound COC1=CC=CC(C(=O)NN(C(=O)C=2C=C(C)C=C(C)C=2)C(C)(C)C)=C1C QCAWEPFNJXQPAN-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000000375 suspending agent Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 52
- 239000000080 wetting agent Substances 0.000 claims abstract description 25
- 239000002562 thickening agent Substances 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000004480 active ingredient Substances 0.000 claims abstract description 21
- 239000003755 preservative agent Substances 0.000 claims abstract description 21
- 230000002335 preservative effect Effects 0.000 claims abstract description 21
- 239000012747 synergistic agent Substances 0.000 claims abstract description 13
- 239000002518 antifoaming agent Substances 0.000 claims description 19
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 19
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 19
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- TVFWYUWNQVRQRG-UHFFFAOYSA-N 2,3,4-tris(2-phenylethenyl)phenol Chemical compound C=1C=CC=CC=1C=CC1=C(C=CC=2C=CC=CC=2)C(O)=CC=C1C=CC1=CC=CC=C1 TVFWYUWNQVRQRG-UHFFFAOYSA-N 0.000 claims description 14
- 229910019142 PO4 Inorganic materials 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 8
- 239000010452 phosphate Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 6
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 6
- 239000004299 sodium benzoate Substances 0.000 claims description 6
- 235000010234 sodium benzoate Nutrition 0.000 claims description 6
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 claims description 6
- 239000000230 xanthan gum Substances 0.000 claims description 6
- 229920001285 xanthan gum Polymers 0.000 claims description 6
- 229940082509 xanthan gum Drugs 0.000 claims description 6
- 235000010493 xanthan gum Nutrition 0.000 claims description 6
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims description 5
- 229960000878 docusate sodium Drugs 0.000 claims description 5
- 229920001451 polypropylene glycol Polymers 0.000 claims description 5
- 159000000000 sodium salts Chemical class 0.000 claims description 5
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims 2
- 239000003814 drug Substances 0.000 abstract description 11
- 239000012752 auxiliary agent Substances 0.000 abstract description 7
- 239000013530 defoamer Substances 0.000 abstract description 7
- 239000000725 suspension Substances 0.000 abstract description 7
- 241000209094 Oryza Species 0.000 abstract description 5
- 229940079593 drug Drugs 0.000 abstract description 5
- 238000005338 heat storage Methods 0.000 abstract description 5
- 238000005457 optimization Methods 0.000 abstract description 4
- 238000012216 screening Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 12
- 241000607479 Yersinia pestis Species 0.000 description 11
- -1 alkylbenzene sulfonate Chemical class 0.000 description 11
- 239000000575 pesticide Substances 0.000 description 10
- 239000002253 acid Substances 0.000 description 8
- 150000002191 fatty alcohols Chemical class 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 231100000419 toxicity Toxicity 0.000 description 6
- 230000001988 toxicity Effects 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 241000098289 Cnaphalocrocis medinalis Species 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 150000003863 ammonium salts Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- NHFDKKSSQWCEES-UHFFFAOYSA-N dihydrogen phosphate;tris(2-hydroxyethyl)azanium Chemical compound OP(O)(O)=O.OCCN(CCO)CCO NHFDKKSSQWCEES-UHFFFAOYSA-N 0.000 description 3
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 description 3
- 229930182470 glycoside Natural products 0.000 description 3
- 229940073769 methyl oleate Drugs 0.000 description 3
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 235000012424 soybean oil Nutrition 0.000 description 3
- 239000003549 soybean oil Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 241000238631 Hexapoda Species 0.000 description 2
- 241000255777 Lepidoptera Species 0.000 description 2
- 229930040373 Paraformaldehyde Natural products 0.000 description 2
- 235000005205 Pinus Nutrition 0.000 description 2
- 241000218602 Pinus <genus> Species 0.000 description 2
- 241000500437 Plutella xylostella Species 0.000 description 2
- 108010052164 Sodium Channels Proteins 0.000 description 2
- 102000018674 Sodium Channels Human genes 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 229960000892 attapulgite Drugs 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 239000002552 dosage form Substances 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 230000037406 food intake Effects 0.000 description 2
- 229910021485 fumed silica Inorganic materials 0.000 description 2
- 230000000749 insecticidal effect Effects 0.000 description 2
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052625 palygorskite Inorganic materials 0.000 description 2
- 229920002866 paraformaldehyde Polymers 0.000 description 2
- 150000003904 phospholipids Chemical class 0.000 description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229940100555 2-methyl-4-isothiazolin-3-one Drugs 0.000 description 1
- 244000003416 Asparagus officinalis Species 0.000 description 1
- 235000005340 Asparagus officinalis Nutrition 0.000 description 1
- 241001517923 Douglasiidae Species 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- UPEZCKBFRMILAV-JNEQICEOSA-N Ecdysone Natural products O=C1[C@H]2[C@@](C)([C@@H]3C([C@@]4(O)[C@@](C)([C@H]([C@H]([C@@H](O)CCC(O)(C)C)C)CC4)CC3)=C1)C[C@H](O)[C@H](O)C2 UPEZCKBFRMILAV-JNEQICEOSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000255967 Helicoverpa zea Species 0.000 description 1
- 240000001307 Myosotis scorpioides Species 0.000 description 1
- 241001477931 Mythimna unipuncta Species 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- 206010035673 Pneumonia chlamydial Diseases 0.000 description 1
- 241000985245 Spodoptera litura Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- UPEZCKBFRMILAV-UHFFFAOYSA-N alpha-Ecdysone Natural products C1C(O)C(O)CC2(C)C(CCC3(C(C(C(O)CCC(C)(C)O)C)CCC33O)C)C3=CC(=O)C21 UPEZCKBFRMILAV-UHFFFAOYSA-N 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 238000010296 bead milling Methods 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- UPEZCKBFRMILAV-JMZLNJERSA-N ecdysone Chemical compound C1[C@@H](O)[C@@H](O)C[C@]2(C)[C@@H](CC[C@@]3([C@@H]([C@@H]([C@H](O)CCC(C)(C)O)C)CC[C@]33O)C)C3=CC(=O)[C@@H]21 UPEZCKBFRMILAV-JMZLNJERSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229940042795 hydrazides for tuberculosis treatment Drugs 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229940126181 ion channel inhibitor Drugs 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- BEGLCMHJXHIJLR-UHFFFAOYSA-N methylisothiazolinone Chemical compound CN1SC=CC1=O BEGLCMHJXHIJLR-UHFFFAOYSA-N 0.000 description 1
- 210000002569 neuron Anatomy 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 231100000820 toxicity test Toxicity 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 230000001018 virulence Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- 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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
- A01N37/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a suspending agent containing indoxacarb and methoxyfenozide, which comprises the following components: active ingredient, dispersant, wetting agent, thickener, antifreezing agent, defoamer, preservative and synergist; the active ingredients are indoxacarb and methoxyfenozide; the mass ratio of the indoxacarb to the methoxyfenozide is (5-30): (5-40). The invention performs scheme optimization aiming at different raw medicines through a large number of auxiliary agent screening, finally obtains a system with the optimal matching degree among the components, particularly the combination of wetting agent, dispersing agent and synergistic agent, greatly improves the stability and tolerance of the product, has the advantages of good dispersibility, high suspension rate, meeting different water qualities, lower surface tension and the like, and effectively solves the problems of heat storage Oryza curing, caking and the like of the sample.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to a suspending agent containing indoxacarb and methoxyfenozide and a preparation method thereof.
Background
Indoxacarb is used as a brand-new pesticide, and has the action mechanism of a sodium ion channel inhibitor, and is mainly used for blocking sodium channels in nerve cells of pests, so that target pests are paralyzed and finally die. Has effects of killing and regulating stomach toxin. The pesticide enters the insect body through contact killing and ingestion, and the behavior of pests is changed rapidly, so that the pests terminate ingestion rapidly, and the target crops are protected well. Can be used for vegetables, fruit trees, ornamental plants and the like, and can prevent and control leaf miner, plutella xylostella, cnaphalocrocis medinalis and other pests.
Methoxyfenozide is a novel specific phenylhydrazide low-toxicity pesticide, has high selective insecticidal activity on lepidoptera pests, mainly has touch-killing effect, and has a certain systemic effect. The medicine belongs to bionic ecdysone, and after pests take the medicine, ecdysis reaction is generated to start ecdysis, and larvae are dehydrated and starved to die because the ecdysis can not be completely performed. Can be used for controlling various pests in lepidoptera such as armyworms, plutella xylostella, asparagus caterpillar, prodenia litura, cotton bollworms and the like.
The active ingredients with different action mechanisms are compounded, the synergistic effect generated by mixing the two active ingredients can be utilized, the insecticidal spectrum is enlarged, the control effect is improved, the generation of drug resistance of pests is delayed, the environmental pollution is reduced, and the compound pesticide is an important means for comprehensively controlling the pests.
At present, the combined use of indoxacarb and methoxyfenozide for killing insects is reported, and the indoxacarb is difficult to disperse when being used as a water suspending agent due to low melting point and strong lipophilicity, so that the problem of Oryza curing or caking of the product is easy to occur when the product is stored under heat. Because the indoxacarb raw medicines are uneven in quality, different processes exist (S: R is 3:1 or 9:1), the two raw medicines can be used, and the difficulty of meeting different water qualities is high. Therefore, how to develop a suspending agent, and through the selection and compatibility of auxiliary agents, it is very necessary to improve the stability of the product.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide the suspending agent containing indoxacarb and methoxyfenozide, and the stability of the product is improved through the selection of the auxiliary agent.
The invention provides a suspending agent containing indoxacarb and methoxyfenozide, which comprises the following components:
active ingredient, dispersant, wetting agent, thickener, antifreezing agent, defoamer, preservative and synergist;
the active ingredients are indoxacarb and methoxyfenozide; the mass ratio of the indoxacarb to the methoxyfenozide is (5-30): (5-40).
Optionally, the method comprises the following steps in percentage by mass:
10% -70% of active ingredients;
1-10% of dispersing agent;
1-10% of wetting agent;
0.1 to 1 percent of thickening agent;
1-10% of antifreezing agent;
0.1% -1% of defoaming agent;
0.1 to 1 percent of preservative;
1% -15% of synergistic agent;
the balance of water;
the active ingredients comprise indoxacarb and methoxyfenozide; the mass ratio of the indoxacarb to the methoxyfenozide is (5-30): (5-40).
Optionally, the method comprises the following steps in percentage by mass:
10 to 60 percent of medicinal active ingredients, 1 to 10 percent of dispersing agent, 1 to 10 percent of wetting agent, 0.1 to 1 percent of thickening agent, 1 to 10 percent of antifreezing agent, 0.1 to 1 percent of defoaming agent, 1 to 15 percent of synergistic agent, 0.1 to 0.8 percent of preservative and the balance of water.
Optionally, the dispersing agent is one or more of sodium salt of polycarboxylic acid, ammonium salt of polycarboxylic acid, potassium salt of polycarboxylic acid, tristyrylphenol polyoxyethylene ether phosphate, nonionic high molecular polymer, tristyrylphenol polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, alkylbenzene sulfonate or alkyl naphthalene sulfonate formaldehyde condensate.
Optionally, the dispersant comprises a first dispersant and a second dispersant; the first dispersing agent comprises polycarboxylate sodium salt, polycarboxylate ammonium salt or nonionic high molecular polymer; the second dispersant comprises one or more of tristyrylphenol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether phosphate or alkyl naphthalene sulfonate formaldehyde condensate.
Optionally, the mass ratio of the first dispersant to the second dispersant is 1: (1-5).
Optionally, the mass ratio of the first dispersant to the second dispersant is 1: (1-3).
Optionally, the wetting agent is one or more of tristyrylphenol polyoxyethylene ether, polyethylene oxide polypropylene oxide monobutyl ether, fatty alcohol polyoxyethylene ether and polyoxyethylene-polyoxypropylene block copolymer.
The thickener is one or more of gas-phase white carbon black, magnesium aluminum silicate, attapulgite and xanthan gum;
the antifreezing agent is one or more of ethylene glycol, propylene glycol, urea or glycerol;
the defoaming agent is organic siloxane, high-carbon alcohol fatty acid ester compound, organic silicon defoaming agent or C 8-10 One or more of the fatty alcohols of (a);
the preservative is one of paraformaldehyde, isothiazolinone, pinone, sodium benzoate or 2-methyl-4-isothiazolin-3-one;
the synergistic agent is one or more of docusate sodium, methyl oleate, soybean oil, alkyl glycoside or soft phospholipids.
Optionally, the wetting agent is polyethylene oxide polypropylene oxide monobutyl ether;
the synergistic agent is docusate sodium;
the antifreezing agent is glycerol;
the thickener is xanthan gum;
the defoaming agent is an organosilicon defoaming agent;
the preservative is sodium benzoate.
The invention provides a preparation method of the suspending agent containing indoxacarb and methoxyfenozide, which comprises the following steps:
mixing a wetting agent, a dispersing agent, a defoaming agent, a preservative, a synergist and water, adding indoxacarb and methoxyfenozide in a high-speed dispersion state, dispersing, grinding, and adding an antifreezing agent and a thickening agent for shearing to obtain the suspending agent containing indoxacarb and methoxyfenozide.
Compared with the prior art, the invention provides a suspending agent containing indoxacarb and methoxyfenozide, which comprises the following components: active ingredient, dispersant, wetting agent, thickener, antifreezing agent, defoamer, preservative and synergist; the active ingredients are indoxacarb and methoxyfenozide; the mass ratio of the indoxacarb to the methoxyfenozide is (5-30): (5-40). The invention performs scheme optimization aiming at different raw medicines through a large number of auxiliary agent screening, finally obtains a system with the optimal matching degree among the components, particularly the combination of wetting agent, dispersing agent and synergistic agent, greatly improves the stability and tolerance of the product, has the advantages of good dispersibility, high suspension rate, meeting different water qualities, lower surface tension and the like, and effectively solves the problems of heat storage Oryza curing, caking and the like of the sample.
Detailed Description
The invention provides a suspending agent containing indoxacarb and methoxyfenozide, which comprises the following components:
active ingredient, dispersant, wetting agent, thickener, antifreezing agent, defoamer, preservative and synergist;
the active ingredients are indoxacarb and methoxyfenozide; the mass ratio of the indoxacarb to the methoxyfenozide is (5-30): (5-40).
The invention discloses a suspending agent containing indoxacarb and methoxyfenozide, which comprises the following components in percentage by mass:
10% -70% of active ingredients;
1-10% of dispersing agent;
1-10% of wetting agent;
0.1 to 1 percent of thickening agent;
1-10% of antifreezing agent;
0.1% -1% of defoaming agent;
0.1 to 1 percent of preservative;
1% -15% of synergistic agent;
the balance of water;
the active ingredients comprise indoxacarb and methoxyfenozide; the mass ratio of the indoxacarb to the methoxyfenozide is (5-30): (5-40).
Indoxacarb: (S/R isomer) melting point 88.1 ℃, 139-141 ℃; kowlogp=4.65 (25 ℃), vapor pressure: 1.010-5Pa (20-25 ℃), density: 1.53 (20 ℃ C.) solubility in water (20 ℃ C.). Less than 0.5mg/L; solubility in other solvents (g/L): methanol 0.39, acetonitrile 76, acetone 140. Aqueous stability DT50 > 30 days (ph=5); 30 days (ph=7), about 2 days (ph=9).
Methoxyfenozide: the pure product is white powder with melting point of 202-205 deg.C and vapor pressure of less than 5.3X10 -5 Pa (25 ℃ C.), the solubility in an organic solvent is: 11g/100g dimethyl sulfoxide, 9.9g/100g cyclohexanone and 9g/100g acetone, and has a solubility of less than 1mg/L in water and is stable in storage at 25 ℃.
Wherein, the indoxacarb has low melting point and strong lipophilicity, so that the indoxacarb is difficult to disperse when being used as an aqueous suspending agent, and the problem of Oryza curing or caking easily occurs when the indoxacarb is thermally stored. The inventor creatively discovers a system with the best matching degree among the auxiliary agents of the components, particularly the combination of the dispersing agent, the wetting agent and the synergist, greatly improves the stability and the tolerance of the product, has the advantages of good dispersibility, high suspension rate, different water quality meeting, lower surface tension and the like, and effectively solves the problems of heat storage Ornithose curing, caking and the like of samples.
The suspending agent containing indoxacarb and methoxyfenozide provided by the invention comprises 10-70% of active ingredients by mass percent; preferably 10% -60%; more preferably 20% to 50%.
The active ingredients of the invention comprise indoxacarb and methoxyfenozide; the mass ratio of the indoxacarb to the methoxyfenozide is (5-30): (5-40); preferably (5 to 25): (5-35). More preferably (10 to 20): (15-35). Most preferably, the composition comprises 15.2% of indoxacarb and 29.5% of methoxyfenozide.
The suspending agent containing indoxacarb and methoxyfenozide provided by the invention comprises 1-10% of dispersing agent by mass percent; preferably comprising 3% -8%; more preferably 3% to 6%; most preferably 4%.
The dispersing agent is preferably one or more of sodium salt of polycarboxylic acid, ammonium salt of polycarboxylic acid, potassium salt of polycarboxylic acid, tristyrylphenol polyoxyethylene ether phosphate, nonionic high molecular polymer, tristyrylphenol polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine, alkylbenzene sulfonate or alkyl naphthalene sulfonate formaldehyde condensate. More preferably, the dispersant comprises a first dispersant and a second dispersant; the first dispersing agent comprises one of polycarboxylic acid sodium salt, polycarboxylic acid ammonium salt or nonionic high molecular polymer; the second dispersant comprises one of tristyrylphenol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine, tristyrylphenol polyoxyethylene ether sulfate, alkylbenzene sulfonate or alkyl naphthalene sulfonate formaldehyde condensate.
In some embodiments of the present invention, the mass ratio of the first dispersant to the second dispersant is 1: (1-5).
In some embodiments of the present invention, the mass ratio of the first dispersant to the second dispersant is 1: (1-3).
In some embodiments of the present invention, the mass ratio of the first dispersant to the second dispersant is 1:1, a step of;
in some embodiments of the present invention, the mass ratio of the first dispersant to the second dispersant is 1:2.
in some embodiments of the present invention, the mass ratio of the first dispersant to the second dispersant is 1:3.
the suspending agent containing indoxacarb and methoxyfenozide provided by the invention comprises 1-10% of wetting agent by mass percent; preferably comprising 2% -4%; specifically, the ratio of the components can be 2%, 3% and 4%; or a point value between any two of the above, most preferably 2%.
The wetting agent is preferably one or more of tristyrylphenol polyoxyethylene ether, polyethylene oxide polypropylene oxide monobutyl ether, fatty alcohol polyoxyethylene ether and polyoxyethylene-polyoxypropylene segmented copolymer; most preferred is polyethylene oxide polypropylene oxide monobutyl ether.
The suspending agent containing indoxacarb and methoxyfenozide provided by the invention comprises 0.1% -1% of thickening agent by mass percent; more preferably, the thickener is included in the range of 0.1% to 0.5%; most preferably from 0.1 to 0.25%; particularly preferably 0.12%.
The thickener is preferably one or more of fumed silica, magnesium aluminum silicate, attapulgite or xanthan gum; more preferably, the thickener is one or more of fumed silica, magnesium aluminum silicate or xanthan gum; most preferably, the thickener is xanthan gum.
The suspending agent containing indoxacarb and methoxyfenozide provided by the invention comprises 1-10% of antifreezing agent by mass percent; preferably comprising 3% -8%; more preferably from 4% to 6%; most preferably 5%.
The antifreezing agent is preferably one or more of ethylene glycol, propylene glycol, urea and glycerol; more preferably urea or glycerol; most preferred is glycerol.
The suspending agent containing indoxacarb and methoxyfenozide provided by the invention comprises 0.1% -1% of defoamer in percentage by mass; preferably comprises 0.1 to 0.5 percent of defoaming agent; most preferably 0.2% defoamer is included.
The defoamer is preferably one or more of organic siloxane, higher alcohol fatty acid ester complex, organic silicone and C8-10 fatty alcohol; more preferably one or more of silicone-based, C8-10 fatty alcohols; most preferred are silicone defoamers.
The suspending agent containing indoxacarb and methoxyfenozide provided by the invention comprises 0.1% -1% of preservative by mass percent; preferably 0.1% -0.5%; most preferably 0.1%.
The preservative is preferably any one of paraformaldehyde, isothiazolinone, pinus, sodium benzoate and 2-methyl-4-isothiazolin-3-ketone; more preferably, it is pinus or sodium benzoate; most preferred is sodium benzoate.
The suspending agent containing indoxacarb and methoxyfenozide provided by the invention comprises 1-15% of a synergist by mass percent; preferably comprises 3 to 10 percent of synergistic agent; more preferably 3% to 5%; most preferably 3%.
The synergistic agent is preferably one or more of docusate sodium, methyl oleate, soybean oil, alkyl glycoside and soft phospholipids; more preferably sodium docusate, methyl oleate, soybean oil or alkyl glycoside; most preferred is docusate sodium.
The synergist can effectively improve the wetting spreading and permeability of a target, and accelerate the absorption and the efficacy of the drug.
In a part of preferred embodiments of the present invention, the suspending agent containing indoxacarb and methoxyfenozide comprises, by mass:
10-60% of a pharmaceutical active ingredient, 1-10% of a dispersing agent, 1-10% of a wetting agent, 0.1-1% of a thickening agent, 1-10% of an antifreezing agent, 0.1-1% of a defoaming agent, 1-15% of a synergistic agent and 0.1-1% of a preservative; the balance of water.
In a part of preferred embodiments of the present invention, the suspending agent containing indoxacarb and methoxyfenozide comprises, by mass:
20 to 50 percent of medicinal active ingredients, 3 to 8 percent of dispersing agent, 2 to 4 percent of wetting agent, 0.1 to 0.5 percent of thickening agent, 3 to 8 percent of antifreezing agent, 0.1 to 0.5 percent of defoaming agent, 3 to 10 percent of synergistic agent and 0.1 to 1 percent of preservative; the balance of water.
In a part of preferred embodiments of the present invention, the suspending agent containing indoxacarb and methoxyfenozide comprises, by mass:
15.2% of indoxacarb, 29.5% of methoxyfenozide, 4% of dispersing agent, 2% of wetting agent, 0.12% of thickening agent, 0.2% of defoaming agent, 3% of synergistic agent, 0.1% of preservative, 5% of antifreezing agent and the balance of water.
The inventor selects the auxiliary agents to ensure that the water suspending agent has the advantages of good dispersion stability, high suspension rate, different water quality resistance, good heat storage stability and the like, and when the auxiliary agents are optimized, the optimization of the dosage form performance and the efficacy exertion of the effective components are more facilitated, and particularly, the optimization of the wetting agent, the dispersing agent and the synergist has better promotion effect on the performance and the efficacy exertion of the dosage form. If not used, problems such as Oryza ripening, reduction in suspension rate, delamination and the like often occur in the storage of heat storage.
The invention provides a preparation method of the suspending agent containing indoxacarb and methoxyfenozide, which comprises the following steps:
mixing a wetting agent, a dispersing agent, a defoaming agent, a preservative, a synergist and water, adding indoxacarb and methoxyfenozide in a high-speed dispersion state, dispersing, grinding, and adding an antifreezing agent and a thickening agent for shearing to obtain the suspending agent containing indoxacarb and methoxyfenozide.
The present invention has been described in detail with reference to the above components and proportions, and will not be described in detail herein.
Firstly, mixing a wetting agent, a dispersing agent, a defoaming agent, a preservative, a synergist and water; preferably, the mixture is uniformly mixed in a reaction kettle.
Adding indoxacarb and methoxyfenozide in a high-speed dispersion state, and dispersing at a high speed for 20-40 min; grinding; the grinding is carried out by using a sand mill until the particle diameter D90 of the mixture is 2-4 mu m.
And adding an antifreezing agent and a thickening agent for shearing to obtain the suspending agent containing indoxacarb and methoxyfenozide. The shearing time is 30-50 min.
In the present invention, the milling may be performed using any of the milling methods disclosed in the prior art, for example, milling may be performed under zirconia bead milling media. After grinding, the particles were measured by a laser particle size distribution analyzer until the particle diameter D90 was 2 to 4. Mu.m.
In order to further illustrate the present invention, the suspending agent containing indoxacarb and methoxyfenozide provided by the present invention and the preparation method thereof are described in detail below with reference to examples.
Examples 1 to 8
The suspending agent was prepared according to the proportions of table 1, the preparation method being as follows:
mixing a wetting agent, a dispersing agent, a defoaming agent, a preservative, a synergist and water; preferably, the mixture is uniformly mixed in a reaction kettle. Adding indoxacarb and methoxyfenozide in a high-speed dispersion state, and dispersing at a high speed for 20-40 min; grinding; the grinding is carried out by using a sand mill until the particle diameter D90 of the mixture is 2-4 mu m. Adding antifreezing agent and thickener for shearing to obtain suspending agent containing indoxacarb and methoxyfenozide
Comparative example 1
The suspending agent was prepared according to the proportions of table 1, the preparation method being as follows:
TABLE 1 summary of the amounts of the raw materials used in the examples and comparative examples of the present invention
The properties of the aqueous suspensions prepared in the above examples and comparative examples were examined, and the results are shown in the following table. The suspension rate is detected according to a GB/T14825-2006 pesticide suspension rate measuring method, the pourability is detected according to a GB/T31737-2015 pesticide pourability measuring method, the spontaneous dispersibility in water is detected according to a CIPAC MT160 method, and the foamability is detected according to a GB/T28137-2011 persistent foamability method.
TABLE 2 Properties of suspending agent product prepared by compounding indoxacarb and methoxyfenozide
Field test
Toxicity experiment
The embodiment of the invention discloses a method for measuring indoor toxicity. According to the sun cloud Peel method, indoor toxicity measurement is carried out, so that the co-toxicity coefficient (CTC) of the two medicaments compounded according to a certain proportion is clear, CTC is smaller than 80 and is antagonistic, CTC is smaller than or equal to 80 and smaller than or equal to 120 and is additive, and CTC is larger than 120 and is synergistic.
Indoxacarb and methoxyfenozide are compounded to measure the indoor toxicity of cnaphalocrocis medinalis.
The test agents are all provided by Shandong Weifang Runfeng chemical industry Co., ltd.
And (3) test design: after the effective inhibition concentration range of each medicament is determined through pre-test, each medicament is respectively provided with a series of concentration treatments according to the content of the effective components, and clear water is used for comparison. The method is carried out by referring to pesticide of biological assay test rule in pesticide room, the concentration in killing after pesticide and mixed use is measured by adopting a pest dipping method, and the co-toxicity coefficient is calculated by a method for calculating combined toxicity proposed by Sunyanpei et al (1960).
The calculation formula is as follows (taking indoxacarb as a standard medicament, and the toxicity index is 100)
Theoretical virulence index (TTI) =indoxacarb ti×p for M Indoxacarb +methoxyfenozide TI x P Methoxyfenozide
Wherein: m is a mixture of indoxacarb and methoxyfenozide in different proportions;
P indoxacarb The indoxacarb accounts for the proportion of the compound composition;
P methoxyfenozide The methoxyfenozide accounts for the proportion of the compound composition.
The test results are shown in table 1:
TABLE 1 toxicity determination results of indoxacarb and methoxyfenozide on cnaphalocrocis medinalis according to different ratios
From the hydrazides Table 1, it is clear that indoxacarb and methoxyfenozide provide LC for cnaphalocrocis medinalis 50 6.16mg/L and 8.25mg/L, respectively. Indoxacarb and methoxyfenozide in a mass ratio of 1:10 to 1: 5. 1:3. 1:1, 3: 1. 5: 1. 10: the co-toxicity coefficients of 1 are respectively 132.28, 138.94, 142.15, 140.51, 142.04, 143.56 and 151.53 which are all more than 120, and the synergistic effect is shown.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (2)
1. A suspending agent containing indoxacarb and methoxyfenozide, which comprises:
the anti-freezing agent comprises an active ingredient, a dispersing agent, a wetting agent, a thickening agent, an anti-freezing agent, a defoaming agent, a preservative and a synergistic agent;
the suspending agent containing indoxacarb and methoxyfenozide,
comprises the following components in percentage by mass:
the active ingredient is 15.2 percent of indoxacarb and 29.5 percent of methoxyfenozide;
the dispersant comprises a first dispersant and a second dispersant; the first dispersant is 2% polycarboxylate sodium salt; the second dispersant is 2% tristyrylphenol polyoxyethylene ether phosphate; the wetting agent is 2% polyethylene oxide polypropylene oxide monobutyl ether;
the thickener is 0.1% xanthan gum;
the antifreezing agent is 5% glycerol;
the defoaming agent is 0.2 percent of organic silicon defoaming agent;
the preservative is 0.1% sodium benzoate;
the synergist is 3% docusate sodium;
the balance of water.
2. The preparation method of the suspending agent containing indoxacarb and methoxyfenozide as claimed in claim 1, which comprises the following steps:
mixing a wetting agent, a dispersing agent, a defoaming agent, a preservative, a synergist and water, adding indoxacarb and methoxyfenozide in a high-speed dispersion state, dispersing, grinding, and adding an antifreezing agent and a thickening agent for shearing to obtain the suspending agent containing indoxacarb and methoxyfenozide.
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| CN103518765A (en) * | 2013-11-06 | 2014-01-22 | 南京南农农药科技发展有限公司 | Indoxacarb and methoxyfenozide compound insecticide combination |
| CN106376589A (en) * | 2016-08-25 | 2017-02-08 | 安徽美兰农业发展股份有限公司 | Methoxyfenozide and indoxacarb compound suspending agent and preparation method thereof |
| CN109673659A (en) * | 2018-08-31 | 2019-04-26 | 中国农业科学院植物保护研究所 | A method of prevention and treatment resistance lepidoptera pest |
| CN113040165A (en) * | 2021-04-02 | 2021-06-29 | 蚌埠格润生物科技有限公司 | Suspending agent containing indoxacarb and methoxyfenozide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103518765A (en) * | 2013-11-06 | 2014-01-22 | 南京南农农药科技发展有限公司 | Indoxacarb and methoxyfenozide compound insecticide combination |
| CN106376589A (en) * | 2016-08-25 | 2017-02-08 | 安徽美兰农业发展股份有限公司 | Methoxyfenozide and indoxacarb compound suspending agent and preparation method thereof |
| CN109673659A (en) * | 2018-08-31 | 2019-04-26 | 中国农业科学院植物保护研究所 | A method of prevention and treatment resistance lepidoptera pest |
| CN113040165A (en) * | 2021-04-02 | 2021-06-29 | 蚌埠格润生物科技有限公司 | Suspending agent containing indoxacarb and methoxyfenozide and preparation method thereof |
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