CN116806838A - Liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine and preparation method and application thereof - Google Patents
Liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine and preparation method and application thereof Download PDFInfo
- Publication number
- CN116806838A CN116806838A CN202310743489.0A CN202310743489A CN116806838A CN 116806838 A CN116806838 A CN 116806838A CN 202310743489 A CN202310743489 A CN 202310743489A CN 116806838 A CN116806838 A CN 116806838A
- Authority
- CN
- China
- Prior art keywords
- liquid preparation
- mass fraction
- methoxyphenyl
- fluoro
- compound
- 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.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 383
- 239000007788 liquid Substances 0.000 title claims abstract description 347
- KJBRXNXZODWCMC-UHFFFAOYSA-N anisiflupurin Chemical compound COC1=CC=CC(NC=2C=3NC=NC=3N=C(F)N=2)=C1 KJBRXNXZODWCMC-UHFFFAOYSA-N 0.000 title claims abstract description 202
- 239000006184 cosolvent Substances 0.000 claims abstract description 143
- 150000001875 compounds Chemical class 0.000 claims abstract description 92
- 239000003381 stabilizer Substances 0.000 claims description 148
- REZQBEBOWJAQKS-UHFFFAOYSA-N triacontan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCO REZQBEBOWJAQKS-UHFFFAOYSA-N 0.000 claims description 140
- 239000003995 emulsifying agent Substances 0.000 claims description 126
- 239000002904 solvent Substances 0.000 claims description 118
- 239000012669 liquid formulation Substances 0.000 claims description 86
- IXORZMNAPKEEDV-UHFFFAOYSA-N gibberellic acid GA3 Natural products OC(=O)C1C2(C3)CC(=C)C3(O)CCC2C2(C=CC3O)C1C3(C)C(=O)O2 IXORZMNAPKEEDV-UHFFFAOYSA-N 0.000 claims description 69
- IXORZMNAPKEEDV-OBDJNFEBSA-N gibberellin A3 Chemical compound C([C@@]1(O)C(=C)C[C@@]2(C1)[C@H]1C(O)=O)C[C@H]2[C@]2(C=C[C@@H]3O)[C@H]1[C@]3(C)C(=O)O2 IXORZMNAPKEEDV-OBDJNFEBSA-N 0.000 claims description 69
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 66
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 66
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 63
- 239000004480 active ingredient Substances 0.000 claims description 53
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 46
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 46
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 44
- 239000005980 Gibberellic acid Substances 0.000 claims description 42
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 40
- IXVMHGVQKLDRKH-KNBKMWSGSA-N brassinolide Chemical compound C1OC(=O)[C@H]2C[C@H](O)[C@H](O)C[C@]2(C)[C@H]2CC[C@]3(C)[C@@H]([C@H](C)[C@@H](O)[C@H](O)[C@@H](C)C(C)C)CC[C@H]3[C@@H]21 IXVMHGVQKLDRKH-KNBKMWSGSA-N 0.000 claims description 39
- IXVMHGVQKLDRKH-VRESXRICSA-N Brassinolide Natural products O=C1OC[C@@H]2[C@@H]3[C@@](C)([C@H]([C@@H]([C@@H](O)[C@H](O)[C@H](C(C)C)C)C)CC3)CC[C@@H]2[C@]2(C)[C@@H]1C[C@H](O)[C@H](O)C2 IXVMHGVQKLDRKH-VRESXRICSA-N 0.000 claims description 37
- OORIKNJWZHTXDC-UHFFFAOYSA-N CCCC(CC)C(CC)(C(=O)OCC)N Chemical compound CCCC(CC)C(CC)(C(=O)OCC)N OORIKNJWZHTXDC-UHFFFAOYSA-N 0.000 claims description 31
- UDPGUMQDCGORJQ-UHFFFAOYSA-N (2-chloroethyl)phosphonic acid Chemical compound OP(O)(=O)CCCl UDPGUMQDCGORJQ-UHFFFAOYSA-N 0.000 claims description 28
- 239000005976 Ethephon Substances 0.000 claims description 28
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 28
- 150000002596 lactones Chemical class 0.000 claims description 28
- IXVMHGVQKLDRKH-QHBHMFGVSA-N 24-Epibrassinolide Natural products C1OC(=O)[C@H]2C[C@H](O)[C@H](O)C[C@]2(C)[C@H]2CC[C@]3(C)[C@@H]([C@H](C)[C@@H](O)[C@H](O)[C@H](C)C(C)C)CC[C@H]3[C@@H]21 IXVMHGVQKLDRKH-QHBHMFGVSA-N 0.000 claims description 27
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 23
- 235000019253 formic acid Nutrition 0.000 claims description 23
- 239000004310 lactic acid Substances 0.000 claims description 20
- 235000014655 lactic acid Nutrition 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 19
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 19
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 14
- 229920000053 polysorbate 80 Polymers 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 235000011054 acetic acid Nutrition 0.000 claims description 12
- 150000002191 fatty alcohols Chemical class 0.000 claims description 12
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 11
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 10
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 claims description 10
- 229920000570 polyether Polymers 0.000 claims description 10
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 9
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- 239000005648 plant growth regulator Substances 0.000 claims description 8
- 239000004250 tert-Butylhydroquinone Substances 0.000 claims description 7
- 235000019281 tert-butylhydroquinone Nutrition 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 4
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical group [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims 2
- 239000012895 dilution Substances 0.000 abstract description 71
- 238000010790 dilution Methods 0.000 abstract description 71
- 235000013399 edible fruits Nutrition 0.000 abstract description 45
- 230000000694 effects Effects 0.000 abstract description 44
- 238000005338 heat storage Methods 0.000 abstract description 22
- 229930002875 chlorophyll Natural products 0.000 abstract description 18
- 235000019804 chlorophyll Nutrition 0.000 abstract description 18
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 abstract description 18
- 230000002045 lasting effect Effects 0.000 abstract description 9
- 102000004169 proteins and genes Human genes 0.000 abstract description 5
- 229930192334 Auxin Natural products 0.000 abstract description 4
- 239000002363 auxin Substances 0.000 abstract description 4
- SEOVTRFCIGRIMH-UHFFFAOYSA-N indole-3-acetic acid Chemical compound C1=CC=C2C(CC(=O)O)=CNC2=C1 SEOVTRFCIGRIMH-UHFFFAOYSA-N 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 239000003905 agrochemical Substances 0.000 abstract description 2
- 150000001413 amino acids Chemical class 0.000 abstract description 2
- 230000035784 germination Effects 0.000 abstract description 2
- 238000003306 harvesting Methods 0.000 abstract description 2
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 2
- 108091005461 Nucleic proteins Proteins 0.000 abstract 1
- 230000032683 aging Effects 0.000 abstract 1
- 239000003337 fertilizer Substances 0.000 abstract 1
- 102000039446 nucleic acids Human genes 0.000 abstract 1
- 108020004707 nucleic acids Proteins 0.000 abstract 1
- 150000007523 nucleic acids Chemical class 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 131
- 238000012360 testing method Methods 0.000 description 101
- 239000000047 product Substances 0.000 description 86
- 238000003756 stirring Methods 0.000 description 81
- 239000003153 chemical reaction reagent Substances 0.000 description 40
- 238000004090 dissolution Methods 0.000 description 34
- 230000012010 growth Effects 0.000 description 32
- 244000105624 Arachis hypogaea Species 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 30
- 239000003795 chemical substances by application Substances 0.000 description 22
- 229960004063 propylene glycol Drugs 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 16
- 241000220225 Malus Species 0.000 description 15
- 229930186179 lupulin Natural products 0.000 description 15
- 235000020232 peanut Nutrition 0.000 description 14
- 241000196324 Embryophyta Species 0.000 description 13
- 230000001965 increasing effect Effects 0.000 description 13
- 238000001556 precipitation Methods 0.000 description 13
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 12
- 229960000583 acetic acid Drugs 0.000 description 12
- 230000005923 long-lasting effect Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 240000007228 Mangifera indica Species 0.000 description 11
- 235000014826 Mangifera indica Nutrition 0.000 description 11
- 238000009472 formulation Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 238000005070 sampling Methods 0.000 description 9
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 8
- 238000011056 performance test Methods 0.000 description 8
- 238000005086 pumping Methods 0.000 description 8
- 235000004936 Bromus mango Nutrition 0.000 description 7
- 235000009184 Spondias indica Nutrition 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- 230000001737 promoting effect Effects 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 235000017060 Arachis glabrata Nutrition 0.000 description 6
- 235000010777 Arachis hypogaea Nutrition 0.000 description 6
- 235000018262 Arachis monticola Nutrition 0.000 description 6
- 244000075850 Avena orientalis Species 0.000 description 6
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 6
- 229930003268 Vitamin C Natural products 0.000 description 6
- 235000021016 apples Nutrition 0.000 description 6
- 239000003085 diluting agent Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000013112 stability test Methods 0.000 description 6
- 235000019154 vitamin C Nutrition 0.000 description 6
- 239000011718 vitamin C Substances 0.000 description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 5
- 238000005187 foaming Methods 0.000 description 5
- 230000008635 plant growth Effects 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 4
- 229960004463 (s)- propylene glycol Drugs 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
- 239000012362 glacial acetic acid Substances 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 235000016709 nutrition Nutrition 0.000 description 4
- 235000019260 propionic acid Nutrition 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 4
- QFMDFTQOJHFVNR-UHFFFAOYSA-N 1-[2,2-dichloro-1-(4-ethylphenyl)ethyl]-4-ethylbenzene Chemical compound C1=CC(CC)=CC=C1C(C(Cl)Cl)C1=CC=C(CC)C=C1 QFMDFTQOJHFVNR-UHFFFAOYSA-N 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- MJWPFSQVORELDX-UHFFFAOYSA-K aluminium formate Chemical compound [Al+3].[O-]C=O.[O-]C=O.[O-]C=O MJWPFSQVORELDX-UHFFFAOYSA-K 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000012258 culturing Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 235000021022 fresh fruits Nutrition 0.000 description 3
- GMDNUWQNDQDBNQ-UHFFFAOYSA-L magnesium;diformate Chemical compound [Mg+2].[O-]C=O.[O-]C=O GMDNUWQNDQDBNQ-UHFFFAOYSA-L 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 2
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- FAIXYKHYOGVFKA-UHFFFAOYSA-N Kinetin Natural products N=1C=NC=2N=CNC=2C=1N(C)C1=CC=CO1 FAIXYKHYOGVFKA-UHFFFAOYSA-N 0.000 description 2
- 231100000674 Phytotoxicity Toxicity 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 2
- 239000003708 ampul Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 108010088245 cytokinin oxidase Proteins 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 210000002950 fibroblast Anatomy 0.000 description 2
- 239000008233 hard water Substances 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- QANMHLXAZMSUEX-UHFFFAOYSA-N kinetin Chemical compound N=1C=NC=2N=CNC=2C=1NCC1=CC=CO1 QANMHLXAZMSUEX-UHFFFAOYSA-N 0.000 description 2
- 229960001669 kinetin Drugs 0.000 description 2
- 239000001630 malic acid Substances 0.000 description 2
- 235000011090 malic acid Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WCZNSRQVTJYMRQ-UHFFFAOYSA-N n-phenyl-7h-purin-6-amine Chemical class N=1C=NC=2N=CNC=2C=1NC1=CC=CC=C1 WCZNSRQVTJYMRQ-UHFFFAOYSA-N 0.000 description 2
- 230000002085 persistent effect Effects 0.000 description 2
- -1 polyoxyethylene Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- 240000001592 Amaranthus caudatus Species 0.000 description 1
- 235000009328 Amaranthus caudatus Nutrition 0.000 description 1
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 206010020649 Hyperkeratosis Diseases 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 244000098338 Triticum aestivum Species 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 230000036579 abiotic stress Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 239000004178 amaranth Substances 0.000 description 1
- 235000012735 amaranth Nutrition 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- 239000004410 anthocyanin Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000004062 cytokinin Substances 0.000 description 1
- UQHKFADEQIVWID-UHFFFAOYSA-N cytokinin Natural products C1=NC=2C(NCC=C(CO)C)=NC=NC=2N1C1CC(O)C(CO)O1 UQHKFADEQIVWID-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019439 ethyl acetate Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001976 improved effect Effects 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 201000008968 osteosarcoma Diseases 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000007981 phosphate-citrate buffer Substances 0.000 description 1
- 230000000243 photosynthetic effect Effects 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 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
- 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
- A01N25/02—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
-
- 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
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
- A01N31/02—Acyclic 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
- 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
- A01N37/12—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 the group, wherein Cn means a carbon skeleton not containing a 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/06—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings
- A01N43/12—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings condensed with a carbocyclic ring
-
- 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
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/22—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom rings with more than six members
-
- 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
- A01N45/00—Biocides, pest repellants or attractants, or plant growth regulators, containing compounds having three or more carbocyclic rings condensed among themselves, at least one ring not being a six-membered ring
-
- 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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
- A01N57/20—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P21/00—Plant growth regulators
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- General Health & Medical Sciences (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Engineering & Computer Science (AREA)
- Agronomy & Crop Science (AREA)
- Dentistry (AREA)
- Toxicology (AREA)
- Botany (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine, and a preparation method and application thereof, belonging to the technical field of agricultural chemicals. The 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine-containing liquid preparation provided by the invention is prepared by compounding the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine with different compounds, and simultaneously selecting a specific cosolvent, so that the liquid preparation has good lasting foamability, dilution stability, low-temperature stability and heat storage stability. The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine has the functions of inhibiting decomposition of plant chlorophyll, nucleic acid and protein and protecting green and resisting aging; the fertilizer has various effects of transporting amino acid, auxin, inorganic salt and the like, and can be widely used for various stages from germination to harvest of agricultural, fruit tree and horticultural crops.
Description
Technical Field
The invention relates to a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine, and a preparation method and application thereof, belonging to the technical field of agricultural chemicals.
Background
According to the report of the Chinese pesticide industry association, 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine (Anisiflupurin) is a fluorine-containing purine cytokinin newly published by ISO, and the accession number of chemical abstract is 1089014-47-0; international generic name anisiflupurin (P); the Chinese culture name is 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine; molecular formula C 12 H 10 FN 5 O; the relative molecular mass is 259.239; the melting point is 195 ℃; is a 6-anilinopurine derivative; the chemical structure is as follows:
the aniifluprin raw medicine is white crystal powder, is insoluble in water and slightly soluble in ethanol, and is stable in acid and alkali. Aniif luprin is a 6-anilinopurine derivative; in agriculture, the plant has the effects of stimulating the growth of tobacco callus, maintaining the chlorophyll content in isolated wheat leaves, inducing the synthesis of beta-anthocyanin in amaranth cotyledon, and inhibiting cytokinin oxidase/dehydrogenase induced by abiotic stress. In-vitro test results show that anirifluprin has lower toxicity, and has better anti-aging performance on human fibroblasts than kinetin after 80 passages, and the toxicity on cells such as mammalian osteosarcoma cell line HOS, breast cancer cell line MCF-7, mouse cell line fibroblast NIH-3T3 and the like is equivalent to that of kinetin. Therefore, the anirifluprin has the advantages of low toxicity and good use safety.
At present, the single use of a plurality of plant growth regulators often cannot achieve ideal effects, and the defects of single use are that the biological activity is single, the growth regulating effect is relatively low, the use concentration is large, and the growth regulating effect can only be exerted in a certain growth period of crops. Therefore, it is necessary to properly and reasonably select and mix different plant growth regulators in order to overcome or avoid side effects, so as to achieve the expected application effects, i.e., synergistic, additive or inductive effects, and avoid antagonism. However, at present, preparations prepared by compounding aniriflupulin with other compounds in China have not been reported and registered yet.
Therefore, there is a need to develop a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine with good stability, thereby better improving the bioactivity and growth regulating effect of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine.
Disclosure of Invention
The invention aims to provide a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine, which can solve the problems of single activity and poor plant growth regulation effect when the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine is singly used at present.
The second object of the present invention is to provide a method for producing a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine, which can solve the problems that the activity is single and the plant growth regulating effect is poor when 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine is used alone as a liquid preparation at present.
The third object of the present invention is to provide a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine as a plant growth regulator, which can solve the problems of single activity and poor plant growth regulating effect when 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine is used alone as a plant growth regulator.
In order to achieve the above object, the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the present invention adopts the following technical scheme:
a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine mainly comprises active ingredient, emulsifying agent, solvent and cosolvent; the active ingredient consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and a compound; the compound is gibberellic acid GA3, gibberellic acid GA4+7, 24-epibrassinolide, 28-Gao Yuntai lactone, diethyl aminoethyl hexanoate, ethephon or triacontanol; the cosolvent is dimethyl sulfoxide, N-dimethylformamide, N-methylpyrrolidone and lactic acid; the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine in the liquid preparation is not more than 10%; the mass fraction of the compound in the liquid preparation is not more than 30%.
The 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine-containing liquid preparation provided by the invention is prepared by compounding the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine with different compounds, and simultaneously selecting a specific cosolvent, so that the liquid preparation has good lasting foamability, dilution stability, low-temperature stability and heat storage stability. The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine has the efficacy of transferring amino acid, auxin, inorganic salt and the like to growth parts, and can be widely used in various stages from germination to harvest of agricultural, fruit tree and horticultural crops.
Preferably, the compound is gibberellic acid GA3, gibberellic acid GA4+7, 24-epibrassinolide, 28-Gao Yuntai lactone, diethyl aminoethyl hexanoate or triacontanol, and the liquid preparation further comprises a stabilizer which is formic acid, acetic acid, lactic acid, 2, 6-di-tert-butyl-p-cresol or tert-butyl hydroquinone. The stabilizer has the following functions: ensuring that the preparation keeps the diluent uniform in the process of diluting with water and has no precipitate; the utility model is convenient for farmers to use, and avoids blocking the atomizing nozzle of the pesticide apparatus.
Preferably, the compound is gibberellic acid GA3, and the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and gibberellic acid GA3 in the liquid preparation is not more than 0.9% independently;
Or the compound is gibberellic acid GA4+7, and the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and gibberellic acid GA4+7 in the liquid preparation is not more than 1.8% independently;
or the compound is 24-epibrassinolide, the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.99%, and the mass fraction of 24-epibrassinolide is not more than 0.01%;
or the compound is 28-Gao Yuntai lactone, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 4.995%, and the mass fraction of the 28-Gao Yuntai lactone is not more than 0.005%;
or the compound is diethyl aminoethyl hexanoate, wherein the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 2%, and the mass fraction of the diethyl aminoethyl hexanoate is not more than 8%;
or the compound is ethephon, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 0.5%, and the mass fraction of the ethephon is not more than 29.5%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 9.8%, and the mass fraction of the triacontanol is not more than 0.2%. In different liquid preparations, the excessive content of active ingredients can cause the phenomena of precipitation, crystallization, layering and the like during normal-temperature storage.
Preferably, the compound is gibberellic acid GA3, and the stabilizer is formic acid and/or lactic acid; the mass fraction of the stabilizer in the liquid preparation is 0.5-2%;
or the compound is gibberellic acid GA4+7, and the stabilizer is formic acid and/or lactic acid; the mass fraction of the stabilizer in the liquid preparation is 10-20%;
or the compound is 24-epibrassinolide, and the stabilizer is formic acid and/or acetic acid; the mass fraction of the stabilizer in the liquid preparation is 3-6%;
or the compound is 28-Gao Yuntai lactone, and the stabilizer is formic acid and/or acetic acid; the mass fraction of the stabilizer in the liquid preparation is 0.3-0.6%;
or the compound is diethyl aminoethyl hexanoate, and the stabilizer is 2, 6-di-tert-butyl-p-cresol or tert-butyl hydroquinone; the mass fraction of the stabilizer in the liquid preparation is 1-3%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, the mass fraction of the triacontanol in the liquid preparation is not more than 0.1%, and the stabilizer in the liquid preparation is acetic acid; the mass fraction of the stabilizer in the liquid preparation is 1-3%;
Or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the stabilizer in the liquid preparation is formic acid; the mass fraction of the stabilizer in the liquid preparation is 6-10%. The type and amount of the stabilizer have an important influence on the physical stability of the liquid preparation, and for different formulations, the corresponding stabilizer and the corresponding stabilizer amount are required to be used, and if the type and amount of the stabilizer are changed, the performance of the liquid preparation cannot reach the standard. When the stabilizer is used in an excessive amount, the pH value of the preparation is too low, so that the problems of decomposition of active ingredients and the like are caused; when the stabilizer is used in an excessively small amount, precipitation of the aqueous dilution of the preparation occurs, and the dilution stability is not acceptable.
Preferably, the compound is gibberellic acid GA3, and the emulsifier in the liquid preparation is octyl phenol polyoxyethylene ether and/or fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the liquid preparation is 1-4%;
or the compound is gibberellic acid GA4+7, and the emulsifier in the liquid preparation is octyl phenol polyoxyethylene ether and/or fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the liquid preparation is 2-4%;
Or the compound is 24-epibrassinolide, and the emulsifier in the liquid preparation is Tween 80; the mass fraction of the emulsifier in the liquid preparation is 3-7%;
or the compound is 28-Gao Yuntai lactone, and the emulsifying agent in the liquid preparation is polyethylene glycol 400; the mass fraction of the emulsifier in the liquid preparation is 4-8%;
or the compound is diethyl aminoethyl hexanoate, and the emulsifier in the liquid preparation is polyether; the mass fraction of the emulsifier in the liquid preparation is 0.5-2%;
or the compound is ethephon, and the emulsifier in the liquid preparation is polyethylene glycol 400; the mass fraction of the emulsifier in the liquid preparation is 3-6%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, and the emulsifier in the liquid preparation is fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the liquid preparation is 2-6%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the emulsifier in the liquid preparation is Tween 80; the mass fraction of the emulsifier in the liquid preparation is 3-7%. The function of the emulsifier is: the interfacial tension of the components in the mixed system is reduced, a stronger film is formed on the surface of the droplets or an electric double layer is formed on the surface of the droplets by the charges given by the emulsifier, and the droplets are prevented from accumulating with each other, so that a uniform state is maintained. For different formulations, the corresponding emulsifier and the corresponding amount of emulsifier need to be used, and when the amount of emulsifier is too large, the problem is that: the viscosity of the preparation system is too high, which is not beneficial to filling and metering in actual production; meanwhile, the turbidity phenomenon of the preparation is easy to occur at low temperature; excessive dosage and high permeability of the preparation can cause phytotoxicity to crops. When the amount of the emulsifier is too small, it may cause: the droplets of the active ingredients of the preparation aggregate and flocculate, thereby generating unqualified phenomena of crystal precipitation and precipitation.
Preferably, the compound is gibberellic acid GA3, and the cosolvent in the liquid preparation is dimethyl sulfoxide; the mass fraction of the cosolvent in the liquid preparation is 15-25%;
or the compound is gibberellic acid GA4+7, and the cosolvent in the liquid preparation is N, N-dimethylformamide; the mass fraction of the cosolvent in the liquid preparation is 30-40%;
or the compound is 24-epibrassinolide, and the cosolvent in the liquid preparation is N-methylpyrrolidone and/or dimethyl sulfoxide; the mass fraction of the cosolvent in the liquid preparation is 10-20%;
or the compound is 28-Gao Yuntai lactone, and the cosolvent in the liquid preparation is N-methylpyrrolidone and/or dimethyl sulfoxide; the mass fraction of the cosolvent in the liquid preparation is 20-40%;
or the compound is diethyl aminoethyl hexanoate, and the cosolvent in the liquid preparation is N-methyl pyrrolidone; the mass fraction of the cosolvent in the liquid preparation is 20-30%;
or the compound is ethephon, and the cosolvent in the liquid preparation is lactic acid; the mass fraction of the cosolvent in the liquid preparation is 30-40%;
Or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, the mass fraction of the triacontanol in the liquid preparation is not more than 0.1%, and the cosolvent in the liquid preparation is dimethyl sulfoxide; the mass fraction of the cosolvent in the liquid preparation is 10-20%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the cosolvent in the liquid preparation is N-methylpyrrolidone; the mass fraction of the cosolvent in the liquid preparation is 30-40%. The cosolvent acts to dissolve the active ingredient in the liquid formulation and may form complexes, associations, double salts, or the like with poorly soluble substances to increase the solubility of the drug in the solvent. The cosolvent can also increase the stability of the preparation, improve physical properties, correct odor and taste, relieve irritation, improve absorption and increase pharmacological action. The use amount of the cosolvent is too small, so that the active ingredients of the preparation are not completely dissolved, and unstable phenomena such as crystal precipitation and precipitation are easy to occur.
Preferably, the compound is gibberellic acid GA3, the solvent in the liquid preparation is an alcohol solvent, and the alcohol solvent is ethylene glycol and/or propylene glycol;
or the compound is gibberellic acid GA4+7, the solvent in the liquid preparation is an alcohol solvent, and the alcohol solvent is ethylene glycol and/or propylene glycol;
or the compound is 24-epibrassinolide, and the solvent in the liquid preparation is propylene glycol;
or the compound is 28-Gao Yuntai lactone, and the solvent in the liquid preparation is N, N-dimethylformamide;
or the compound is diethyl aminoethyl hexanoate, and the solvent in the liquid preparation is N, N-dimethylformamide;
or the compound is ethephon, and the solvent in the liquid preparation is selected from one or any combination of water, ethylene glycol and propylene glycol;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, the mass fraction of the triacontanol in the liquid preparation is not more than 0.1%, and the solvent in the liquid preparation is propylene glycol;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the solvent in the liquid preparation is N, N-dimethylformamide. The solvents in the liquid formulation have the following effects: (1) dilution effect: the solvent may dilute the concentrated material, making it easier to handle or handle. (2) Dissolution: can dissolve the water-insoluble substance to become a soluble substance. (3) Stabilization: the solvent may stabilize certain substances against oxidation or decomposition. (4) Changing physical properties of a substance: solvents can alter physical properties of a substance, such as viscosity, surface tension, etc., making it easier to handle or process. Too little solvent can cause: the solubility of the active ingredients of the preparation is low, the dissolution is incomplete, and then crystals are separated out.
Preferably, the liquid formulation is a composition a, B, C, D, E, F or G;
the composition A mainly comprises an active ingredient, a stabilizer, an emulsifier, a solvent and a cosolvent; the active ingredients in the A composition consist of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and gibberellic acid GA 3; the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and gibberellic acid GA3 in the a composition is independently no more than 0.9%; the stabilizer in the composition A is formic acid and/or lactic acid; the mass fraction of the stabilizer in the composition A is 0.5-2%; the emulsifier in the composition A is octyl phenol polyoxyethylene ether and/or fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the composition A is 1-4%; the solvent in the composition A is an alcohol solvent; the solvent in the composition A is ethylene glycol and/or propylene glycol; the cosolvent in the A composition is dimethyl sulfoxide; the mass fraction of the cosolvent in the composition A is 15-25%;
the composition B mainly comprises an active ingredient, a stabilizer, an emulsifier, a solvent and a cosolvent; the active ingredients in the composition B consist of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and gibberellic acid GA 4+7; the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and gibberellic acid GA4+7 in the B composition is independently not more than 1.8%; the stabilizer in the composition B is formic acid and/or lactic acid; the mass fraction of the stabilizer in the composition B is 10-20%; the emulsifier in the composition B is octyl phenol polyoxyethylene ether and/or fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the composition B is 2-4%; the solvent in the composition B is an alcohol solvent; the solvent in the composition B is ethylene glycol and/or propylene glycol; the cosolvent in the composition B is N, N-dimethylformamide; the mass fraction of the cosolvent in the composition B is 30-40%;
The composition C mainly comprises an active ingredient, a stabilizer, an emulsifier, a solvent and a cosolvent; the active ingredients in the composition C consist of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and 24-epibrassinolide; the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine in the composition C is not more than 1.99%, and the mass fraction of 24-epibrassinolide is not more than 0.01%; the stabilizer in the composition C is formic acid and/or acetic acid; the mass fraction of the stabilizer in the composition C is 3-6%; the emulsifier in the composition C is Tween 80; the mass fraction of the emulsifier in the composition C is 3-7%; the solvent in the composition C is propylene glycol; the cosolvent in the composition C is N-methyl pyrrolidone and/or dimethyl sulfoxide; the mass fraction of the cosolvent in the composition C is 10-20%;
the composition D mainly comprises an active ingredient, a stabilizer, an emulsifier, a solvent and a cosolvent; the active ingredients in the D composition consist of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and 28-Gao Yuntai lactone; the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine in the D composition is not more than 4.995%, and the mass fraction of 28-Gao Yuntai lactone is not more than 0.005%; the stabilizer in the composition D is formic acid and/or acetic acid; the mass fraction of the stabilizer in the composition D is 0.3-0.6%; the emulsifier in the composition D is polyethylene glycol 400; the mass fraction of the emulsifier in the composition D is 4-8%; the solvent in the composition D is N, N-dimethylformamide; the cosolvent in the composition D is N-methyl pyrrolidone and/or dimethyl sulfoxide; the mass fraction of the cosolvent in the composition D is 20-40%;
The E composition mainly comprises an active ingredient, a stabilizer, an emulsifier, a solvent and a cosolvent; the active ingredients in the E composition consist of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and diethyl aminoethyl hexanoate; the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine in the E composition is not more than 2%; the mass fraction of the diethyl aminoethyl hexanoate in the E composition is not more than 8%; the stabilizer in the E composition is 2, 6-di-tert-butyl-p-cresol and/or tert-butyl hydroquinone; the mass fraction of the stabilizer in the E composition is 1-3%; the emulsifier in the E composition is polyether; the mass fraction of the emulsifier in the E composition is 0.5-2%; the solvent in the E composition is N, N-dimethylformamide; the cosolvent in the E composition is N-methyl pyrrolidone; the mass fraction of the cosolvent in the E composition is 20-30%; the polyether is EO/PO block polyether;
the composition F mainly comprises an active ingredient, an emulsifying agent, a solvent and a cosolvent; the active ingredients in the F composition consist of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and ethephon; the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine in the F composition is not more than 0.5%; the mass fraction of ethephon in the F composition is not more than 29.5%; the emulsifier in the F composition is polyethylene glycol 400; the mass fraction of the emulsifier in the F composition is 3-6%; the solvent in the F composition is selected from one or any combination of water, ethylene glycol and propylene glycol; the cosolvent in the F composition is lactic acid; the mass fraction of the cosolvent in the F composition is 30-40%;
The composition G mainly comprises an active ingredient, a stabilizer, an emulsifier, a solvent and a cosolvent; the active ingredients in the G composition consist of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and triacontanol;
the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the G composition is not more than 1.9%, the mass fraction of triacontanol in the G composition is not more than 0.1%, and the stabilizer in the G composition is acetic acid; the mass fraction of the stabilizer in the G composition is 1-3%; the emulsifier in the composition G is fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the G composition is 2-6%; the solvent in the composition G is propylene glycol; the cosolvent in the G composition is dimethyl sulfoxide; the mass fraction of the cosolvent in the G composition is 10-20%;
or the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the G composition is more than 1.9% and less than or equal to 9.8%, the mass fraction of triacontanol in the G composition is more than 0.1% and less than or equal to 0.2%, and the stabilizer in the G composition is formic acid; the mass fraction of the stabilizer in the G composition is 6-10%; the emulsifier in the composition G is Tween 80; the mass fraction of the emulsifier in the G composition is 3-7%; the solvent in the G composition is N, N-dimethylformamide; the cosolvent in the G composition is N-methyl pyrrolidone; the mass fraction of the cosolvent in the G composition is 30-40%.
The emulsifier in the E composition can be a commercial product, for example, a product with the model of Ethylan NS-500LQ manufactured by Nanjing Jie Runchi technology Co., ltd, is a nonionic hydroxyl polyethylene oxide segmented copolymer, has the molar ratio of EO/PO of 1:1.71 and the pH of 6.5-7.5, and has good emulsifying, wetting and dispersing functions.
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine adopts the following technical scheme:
a process for the preparation of a liquid formulation comprising 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine as described above, comprising the steps of: the components with the formula amount are uniformly mixed to obtain the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine.
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine is simple to operate, and the prepared liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine has good lasting foamability, dilution stability, low-temperature stability and heat storage stability.
Preferably, the method for uniformly mixing comprises the following steps: the active ingredients in each composition are dissolved in the cosolvent, and then the other components are added and mixed uniformly.
The application of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine as a plant growth regulator adopts the following technical scheme:
use of a liquid formulation comprising 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine as described above as a plant growth regulator.
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine can be used as a plant growth regulator, so that plant growth can be effectively promoted.
Use of a liquid formulation comprising 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine as described above for promoting plant growth.
Preferably, the liquid formulation is a composition a and/or a composition B, which has the effect of promoting coleoptile growth. Further preferably, the liquid formulation is a composition a and/or a composition B, which has the effect of promoting oat coleoptile growth.
Preferably, the liquid preparation is composition C and/or composition D, and has the effect of increasing plant height and/or increasing the content of nutritional ingredients in plant leaves, wherein the nutritional ingredients are selected from one or any combination of chlorophyll, protein and fat. Further preferably, the liquid formulation is a composition C and/or a composition D, the liquid formulation having the effect of increasing plant height and/or increasing the content of a nutritional ingredient in plant leaves, the nutritional ingredient being selected from one or any combination of chlorophyll, protein and fat. Preferably, the liquid formulation is a composition C and/or a composition D and the food is peanut.
Preferably, the liquid formulation is an E composition and/or an F composition, which has the effect of increasing the fruit setting rate of plants and/or increasing the quality of the fruits of plants, which are overweight per fruit and/or vitamin C content in the fruits. Further preferably, the liquid formulation is an E composition and/or an F composition, which has the effect of increasing the fruit setting rate of apples and/or increasing the quality of apples fruits, which are overweight per fruit and/or vitamin C content in the fruits.
Preferably, the liquid formulation is a G composition, which has the effect of increasing the volume and/or weight of the plant fruit. Preferably, the liquid formulation is a G composition, which has the effect of increasing the diameter of the plant fruit. Further preferably, the liquid preparation is a G composition, and the liquid preparation has the effect of improving the longitudinal diameter and/or transverse diameter of mango fruits.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
The liquid formulations of examples 1-8 were tested for pH as specified in standard GB/T1601;
the persistent foamability is tested according to the specification in the standard GB/T28137, the foam volume at 1min is recorded during the test, when the foam volume is not more than 40mL, the persistent foamability test result is qualified, otherwise, the foam volume is unqualified;
The test method of dilution stability is as follows: sucking 5mL of a sample (liquid preparation) by a pipette, placing the sample into a 100mL measuring cylinder, diluting the sample to 100mL by standard hard water, shaking the sample uniformly, placing the measuring cylinder into a constant-temperature water bath with the temperature of 30+/-2 ℃, standing the sample for 1h, observing the appearance of the diluent in the measuring cylinder, if solid particles are precipitated in the diluent, determining that the diluent stability test result is unqualified, and if no solid particles are precipitated in the diluent, determining that the diluent stability test result is qualified; standard hard water is prepared according to the specification in the standard GB/T14825;
the low temperature stability was tested according to the method of "emulsion and homogeneous liquid formulation" in standard GB/T19137, the specific method is as follows: placing 100mL of the liquid preparation into a beaker, then cold-storing the beaker at 0+/-2 ℃ for 7 days, taking out the beaker, recovering to room temperature, observing whether oily matters are precipitated in the beaker, and determining the volume of the oily matters precipitated, wherein if no oily matters are precipitated or the volume of the oily matters precipitated is not more than 0.3mL, the low-temperature stability test result is qualified, and if the volume of the oily matters precipitated is more than 0.3mL, the low-temperature stability test result is unqualified;
the test method of heat storage stability is as follows: 30mL of the sample (liquid formulation) was measured and tested according to the method "liquid formulation" in Standard GB/T19136, the specific method is as follows: injecting the sample into a clean ampoule bottle by using a syringe, sealing by using high-temperature flame, placing the sealed ampoule bottle in a constant temperature box at 54+/-2 ℃ for 14 days, taking out, recovering to room temperature, measuring the mass of the sample, measuring the mass fraction of the effective components in the sample, the pH value and the dilution stability of the sample within 24 hours if the mass of the sample is unchanged, and determining that the test result of the pH value and the dilution stability of the sample after heat storage is qualified if the mass fraction of the effective components is not less than 95% before heat storage.
The mass fraction of the effective components is tested by adopting a liquid chromatograph-ultraviolet detector, wherein the liquid chromatograph is an Agilent 1260 high performance liquid chromatograph, and the ultraviolet detector is an adjustable ultraviolet wavelength detector; 150mm x 4.6mm (id) column, C18.mu.m packing; 25 mu L of microsyringe; chromatographic conditions: the mobile phase was methanol+water+acetic acid=40+60+0.1 (V/V), degassed by ultrasound and filtered; the flow rate is 1.0mL/min; the column temperature is 25+/-2 ℃; the detection wavelength is 210nm; the sample volume was 5. Mu.L.
Example 1
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this example consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine (aniriflupulin), gibberellic acid, stabilizer, emulsifier, solvent and cosolvent; the types of gibberellic acid, stabilizer, emulsifier, solvent and cosolvent and mass fractions of the components are shown in table 1.
TABLE 1 types of gibberellic acid, stabilizers, emulsifiers, solvents and cosolvents in the liquid formulation of example 1, mass fractions of the respective components
| Type of material | Composition of the composition | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 0.9 |
| Active ingredient | Gibberellic acid GA3 | 0.9 |
| Cosolvent | Dimethyl sulfoxide | 20 |
| Stabilizing agent | Formic acid | 1 |
| Emulsifying agent | Octyl phenol polyoxyethylene ether | 2 |
| Solvent(s) | Ethylene glycol | 75.2 |
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment specifically comprises the following steps: pumping the cosolvent into a reaction kettle by using a diaphragm pump, starting stirring, wherein the stirring speed is 80 revolutions per minute, adding aniif lupulin and gibberellic acid while stirring, and stirring for 30 minutes after the adding is finished, wherein no solute particles are visible in the reaction kettle, so that the complete dissolution is achieved; sequentially adding a stabilizer and an emulsifier, continuously stirring for 60min, finally adding a solvent, and continuously stirring for 30min to obtain a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine.
In other embodiments, the stirring speed is controlled to be 40-80 rpm when preparing the liquid preparation; after the addition of the aniif lupulin and the gibberellic acid is finished, controlling the stirring time to be 30-60min; adding stabilizer and emulsifier, and stirring for 30-60min; after the solvent is added, the stirring time is controlled to be 30-60min.
The liquid formulations of this example were tested for the content of aniriflutuprin, gibberellic acid, pH, long-lasting foamability, dilution stability, low-temperature stability and heat storage stability, and the results are shown in table 2.
TABLE 2 results of Performance test of liquid formulations of example 1
In order to examine the influence of different cosolvents on the liquid preparation, 20g of cosolvent is added into a mixing device, 0.9g of aniiflupulin and 0.9g of gibberellic acid GA3 are accurately weighed, stirred and dissolved for 30min under the condition of rotating speed of 80 revolutions per minute, and the dissolution conditions of aniiflupulin and gibberellic acid GA3 are observed, and the results are shown in table 3.
TABLE 3 dissolution of different cosolvents on Anisiflupurin, gibberellic acid GA3
As is clear from Table 3, when the raw materials were dissolved in the same mass of absolute ethyl alcohol, cyclohexanone, propylene glycol methyl ether acetate, N-dimethylformamide and dimethyl sulfoxide, the dissolution effect of N, N-dimethylformamide and dimethyl sulfoxide on aniriflupulin and gibberellic acid GA3 was the best.
To examine the effect of the stabilizer on the liquid formulation, liquid formulations containing different stabilizers were prepared according to the preparation method of the liquid formulation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 1, and the types of the stabilizers and the dilution stability of each of the prepared liquid formulations are shown in table 4.
TABLE 4 types of stabilizers and dilution stability of the respective liquid formulations produced
As can be seen from table 4, when formic acid was used as the stabilizer, the dilution stability of the formulation was acceptable; when aluminum formate, magnesium formate and citric acid are selected as stabilizers, precipitation appears at the bottom of the liquid preparation during the test of dilution stability, and the liquid preparation is unqualified.
When the cosolvent in Table 4 is replaced by N, N-dimethylformamide or the emulsifier is replaced by octyl phenol polyoxyethylene ether and Tween 80, the test results of dilution stability are all disqualified.
Finally, the influence of the dosage of each component on the liquid preparation is examined, and the specific method is as follows: the liquid preparation was prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 1, except that the mass fraction of each component was changed, and the results showed that when the mass fraction of aniflupurin was less than or equal to 0.9%, the mass fraction of gibberellic acid GA3 was less than or equal to 0.9%, the mass fraction of the cosolvent was 15-25%, the mass fraction of the stabilizer was 0.5-2%, the mass fraction of the emulsifier was 1-4%, and the balance was the solvent, the prepared liquid preparation was clear and transparent liquid, and the pH value was 2-5, and the test results of long-lasting foamability, dilution stability, low-temperature stability and heat storage stability were all acceptable. When the mass fraction of a certain component constituting the liquid preparation is not within the above-mentioned numerical range, one or more of the performance indexes of the liquid preparation produced are not satisfied.
Example 2
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this example consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine (aniriflupulin), gibberellic acid, stabilizer, emulsifier, solvent and cosolvent; the types of gibberellic acid, stabilizer, emulsifier, solvent and cosolvent and mass fractions of the components are shown in table 5.
TABLE 5 types of gibberellic acid, stabilizers, emulsifiers, solvents and cosolvents in the liquid formulation of example 2, mass fractions of the respective components
| Type of material | Composition of the composition | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 1.8 |
| Active ingredient | Gibberellic acid GA4+7 | 1.8 |
| Cosolvent | N, N-dimethylformamide | 35 |
| Stabilizing agent | Lactic acid | 15 |
| Emulsifying agent | Fatty alcohol polyoxyethylene ether | 3 |
| Solvent(s) | Propylene glycol | 43.4 |
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment specifically comprises the following steps: pumping the cosolvent into a reaction kettle by using a diaphragm pump, starting stirring at a stirring speed of 40 revolutions per minute, adding aniif lupulin and gibberellic acid while stirring, and stirring for 60 minutes after the addition is finished, wherein no solute particles are visible in the reaction kettle, so that the complete dissolution is achieved; sequentially adding a stabilizer and an emulsifier, continuously stirring for 30min, finally adding a solvent, and continuously stirring for 60min to obtain a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine.
In other embodiments, the stirring speed is controlled to be 40-80 rpm when preparing the liquid preparation; after the addition of the aniif lupulin and the gibberellic acid is finished, controlling the stirring time to be 30-60min; adding stabilizer and emulsifier, and stirring for 30-60min; after the solvent is added, the stirring time is controlled to be 30-60min.
The liquid formulations of this example were tested for the content of aniriflutuprin, gibberellic acid, pH, long-lasting foamability, dilution stability, low-temperature stability and heat storage stability, and the results are shown in table 6.
TABLE 6 results of Performance test of liquid formulations of example 2
| Project | Index (I) | Detection result | Result determination |
| Mass fraction of aniriflupulin% | 1.8±0.27 | 1.87 | Qualified product |
| Gibberellic acid GA4+7 mass percent% | 1.8±0.27 | 1.82 | Qualified product |
| pH value of | 2-5 | 3.91 | Qualified product |
| Lasting foamability (after 1 min), mL < | 40 | 20 | Qualified product |
| Dilution stability | Qualified product | Qualified product | Qualified product |
| Low temperature stability | Qualified product | Qualified product | Qualified product |
| Thermal storage stability | Qualified product | Qualified product | Qualified product |
In order to examine the influence of different cosolvents on the liquid preparation, 35g of cosolvent is added into a mixing device, 1.8g of aniiflupulin and 1.8g of gibberellic acid GA4+7 are accurately weighed, stirred and dissolved for 60min under the condition of 40 revolutions per minute, and the dissolution conditions of aniiflupulin and gibberellic acid GA4+7 are observed, and the results are shown in Table 7.
TABLE 7 dissolution of different cosolvents on aniriflutuprin, gibberellic acid GA4+7
As is clear from Table 7, when trimethyl phosphate, monoethanolamine, methyl isobutyl ketone, N-methylpyrrolidone and N, N-dimethylformamide of the same mass were used as the raw materials, only N-methylpyrrolidone and N, N-dimethylformamide gave the best dissolution effect on aniriflutorin and gibberellic acid GA 4+7.
To examine the effect of the stabilizer on the liquid formulation, liquid formulations containing different stabilizers were prepared according to the preparation method of the liquid formulation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 2, and the types of the stabilizers and the dilution stability of each of the prepared liquid formulations are shown in table 8.
TABLE 8 types of stabilizers and dilution stability of the respective liquid formulations produced
As can be seen from table 8, when lactic acid was used as the stabilizer, the dilution stability of the preparation was acceptable; when aluminum sulfate, ferric sulfate and malic acid are used as stabilizers, precipitation appears at the bottom of the liquid preparation during the test of dilution stability, and the liquid preparation is unqualified.
When the cosolvent in Table 8 was replaced with N, N-dimethylformamide or the emulsifier was replaced with Tween 80, the test results of dilution stability were all failed.
Finally, the influence of the dosage of each component on the liquid preparation is examined, and the specific method is as follows: the liquid preparation was prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 2, except that the mass fraction of each component was changed, and the results showed that when the mass fraction of aniflupurin was not more than 1.8%, the mass fraction of gibberellic acid GA4+7 was not more than 1.8%, the mass fraction of the cosolvent was 30-40%, the mass fraction of the stabilizer was 10-20%, the mass fraction of the emulsifier was 2-4%, and the balance was the solvent, the prepared liquid preparation was clear and transparent liquid, and the pH was 2-5, and the test results of long-lasting foaming, dilution stability, low-temperature stability and heat storage stability were all acceptable. When the mass fraction of a certain component constituting the liquid preparation is not within the above-mentioned numerical range, one or more of the performance indexes of the liquid preparation produced are not satisfied.
Example 3
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this example consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine (aniriflutorin), brassinolide, stabilizer, emulsifier, solvent and cosolvent; the types of brassinolide, stabilizer, emulsifier, solvent and co-solvent and the mass fractions of the components are shown in table 9.
TABLE 9 types of brassinolide, stabilizers, emulsifiers, solvents and cosolvents in liquid formulations of example 3, mass fractions of each component
| Type of material | Composition of the composition | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 1.99 |
| Active ingredient | 24-epibrassinolide | 0.01 |
| Cosolvent | N-methylpyrrolidone | 15 |
| Stabilizing agent | Glacial acetic acid | 5 |
| Emulsifying agent | Tween 80 | 5 |
| Solvent(s) | Propylene glycol | 73 |
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment specifically comprises the following steps: pumping the cosolvent into a reaction kettle by using a diaphragm pump, starting stirring, wherein the stirring speed is 80 revolutions per minute, adding the aniif lupulin and brassin lactone while stirring, and stirring for 30 minutes after the addition is finished, wherein no solute particles are visible in the reaction kettle, so that the complete dissolution is achieved; sequentially adding a stabilizer and an emulsifier, continuously stirring for 60min, finally adding a solvent, and continuously stirring for 30min to obtain a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine.
In other embodiments, the stirring speed is controlled to be 40-80 rpm when preparing the liquid preparation; after the addition of the aniriflutuprin and the brassinolide is finished, the stirring time is controlled to be 30-60min; adding stabilizer and emulsifier, and stirring for 30-60min; after the solvent is added, the stirring time is controlled to be 30-60min.
The liquid formulations of this example were tested for the content of aniriflutuprin, brassinolide, pH, long-lasting foaming, dilution stability, low temperature stability and heat storage stability and the results are shown in table 10.
Table 10 results of performance test of the liquid formulation of example 3
| Project | Index (I) | Detection result | Result determination |
| Mass fraction of aniriflupulin% | 1.99±0.2985 | 2.01 | Qualified product |
| Mass fraction of 24-epibrassinolide,% | 0.01±0.0015 | 0.0101 | Qualified product |
| pH value of | 2-5 | 4.37 | Qualified product |
| Lasting foamability (after 1 min), mL < | 40 | 16 | Qualified product |
| Dilution stability | Qualified product | Qualified product | Qualified product |
| Low temperature stability | Qualified product | Qualified product | Qualified product |
| Thermal storage stability | Qualified product | Qualified product | Qualified product |
In order to examine the influence of different cosolvents on a liquid preparation, 15g of a cosolvent is added into a mixing device, 1.99g of aniriflutuprin and 0.01g of 24-epibrassinolide are accurately weighed, stirred and dissolved for 30min under the condition of 80 revolutions per minute, and the dissolution conditions of the aniriflutuprin and the 24-epibrassinolide are observed, and the results are shown in table 11.
TABLE 11 dissolution of Anisiflupurin, 24-Epiposide by different cosolvents
As is clear from Table 11, when the raw materials were dissolved using triethanolamine, N-butyl ether, ethyl acetate, ethylene glycol and N-methylpyrrolidone of the same mass, only ethylene glycol and N-methylpyrrolidone had the best effect of dissolving the aniif lupulin and 24-epibrassinolide.
To examine the effect of the stabilizer on the liquid formulation, liquid formulations containing different stabilizers were prepared according to the preparation method of the liquid formulation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 3, and the types of the stabilizers and the dilution stability of each of the prepared liquid formulations are shown in table 12.
TABLE 12 types of stabilizers and dilution stability of the liquid formulations prepared
As can be seen from table 12, when glacial acetic acid was used as the stabilizer, the dilution stability of the preparation was acceptable; when ammonia water, 0.1mol/L NaOH aqueous solution and tartaric acid are used as stabilizers, precipitation appears at the bottom of the liquid preparation during the dilution stability test, and the liquid preparation is unqualified.
When the cosolvent in Table 12 was replaced with ethylene glycol from N-methylpyrrolidone or span 60 from Tween 80, the dilution stability test results were all failed.
Finally, the influence of the dosage of each component on the liquid preparation is examined, and the specific method is as follows: the liquid preparation was prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 3, except that the mass fraction of each component was changed, and the results showed that when the mass fraction of aniflupurin was less than or equal to 1.99%, the mass fraction of 24-Gao Yuntai lactone was less than or equal to 0.01%, the mass fraction of the cosolvent was 10-20%, the mass fraction of the stabilizer was 3-6%, the mass fraction of the emulsifier was 3-7%, and the balance was the solvent, the prepared liquid preparation was clear and transparent liquid, and the pH value was 2-5, and the test results of long-lasting foamability, dilution stability, low-temperature stability and heat storage stability were all acceptable. When the mass fraction of a certain component constituting the liquid preparation is not within the above-mentioned numerical range, one or more of the performance indexes of the liquid preparation produced are not satisfied.
Example 4
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this example consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine (aniriflutorin), brassinolide, stabilizer, emulsifier, solvent and cosolvent; the types of brassinolide, stabilizer, emulsifier, solvent and co-solvent and mass fractions of each component are shown in table 13.
TABLE 13 types of brassinolide, stabilizers, emulsifiers, solvents and cosolvents in liquid formulations of example 4, mass fractions of each component
| Type of material | Composition of the composition | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 4.995 |
| Active ingredient | 28-Gao Yuntai lactone | 0.005 |
| Cosolvent | Dimethyl sulfoxide | 30 |
| Stabilizing agent | Formic acid | 0.5 |
| Emulsifying agent | Polyethylene glycol 400 | 6 |
| Solvent(s) | N, N-dimethylformamide | 58.5 |
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment specifically comprises the following steps: pumping the cosolvent into a reaction kettle by using a diaphragm pump, starting stirring at a stirring speed of 40 revolutions per minute, adding the aniif lupulin and brassin lactone while stirring, and stirring for 60 minutes again after the addition is finished, wherein no solute particles are visible in the reaction kettle, so that the complete dissolution is achieved; sequentially adding a stabilizer and an emulsifier, continuously stirring for 30min, finally adding a solvent, and continuously stirring for 60min to obtain a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine.
In other embodiments, the stirring speed is controlled to be 40-80 rpm when preparing the liquid preparation; after the addition of the aniriflutuprin and the brassinolide is finished, the stirring time is controlled to be 30-60min; adding stabilizer and emulsifier, and stirring for 30-60min; after the solvent is added, the stirring time is controlled to be 30-60min.
The liquid formulations of this example were tested for the content of aniriflutuprin, brassinolide, pH, long-lasting foaming, dilution stability, low temperature stability and heat storage stability and the results are shown in table 14.
Table 14 results of performance test of the liquid formulation of example 4
| Project | Index (I) | Detection result | Result determination |
| Mass fraction of aniriflupulin% | 4.995±0.4995 | 4.990 | Qualified product |
| 28-Gao Yuntai mass percent of lactone,% | 0.005±0.00075 | 0.0049 | Qualified product |
| pH value of | 2-5 | 3.91 | Qualified product |
| Lasting foamability (after 1 min), mL < | 40 | 13 | Qualified product |
| Dilution stability | Qualified product | Qualified product | Qualified product |
| Low temperature stability | Qualified product | Qualified product | Qualified product |
| Thermal storage stability | Qualified product | Qualified product | Qualified product |
In order to examine the influence of different cosolvents on the liquid preparation, 30g of cosolvent is added into a mixing device, 4.995g of aniflupurin and 0.005g of 28-Gao Yuntai lactone are accurately weighed, stirring and dissolving are carried out for 60min under the condition of 40 revolutions per minute, and the dissolution conditions of the aniflupurin and the 28-Gao Yuntai lactone are observed, wherein the results are shown in Table 15.
TABLE 15 dissolution of Anisiflupurin, 28-Gao Yuntai lactone by different cosolvents
As is clear from Table 15, when the raw materials were dissolved in the same mass of absolute ethyl alcohol, n-butanol, ethyl acetate, propylene glycol and dimethyl sulfoxide, only propylene glycol and dimethyl sulfoxide gave the best results for dissolving the aniifluprin and the 28-Gao Yuntai lactone.
To examine the effect of the stabilizer on the liquid formulation, liquid formulations containing different stabilizers were prepared according to the preparation method of the liquid formulation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 4, and the types of the stabilizers and the dilution stability of each of the prepared liquid formulations are shown in table 16.
TABLE 16 type of stabilizer and dilution stability of each liquid formulation produced
As can be seen from table 16, when formic acid was used as the stabilizer, the dilution stability of the formulation was acceptable; when aluminum formate, magnesium formate and propionic acid are selected as stabilizers, precipitation appears at the bottom of the liquid preparation during the test of dilution stability, and the liquid preparation is unqualified.
The test results of dilution stability were all failed when the co-solvent in table 16 was replaced with propylene glycol from dimethyl sulfoxide or span 80 from polyethylene glycol 400.
Finally, the influence of the dosage of each component on the liquid preparation is examined, and the specific method is as follows: the liquid preparation was prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 4, except that the mass fraction of each component was changed, and the results showed that when the mass fraction of aniflupurin was not more than 4.995%, the mass fraction of 28-Gao Yuntai lactone was not more than 0.005%, the mass fraction of cosolvent was 20-40%, the mass fraction of stabilizer was 0.3-0.6%, the mass fraction of emulsifier was 4-8%, and the balance was solvent, the prepared liquid preparation was clear and transparent liquid, and the pH value was 2-5, and the test results of long-lasting foamability, dilution stability, low-temperature stability and heat storage stability were all acceptable. When the mass fraction of a certain component constituting the liquid preparation is not within the above-mentioned numerical range, one or more of the performance indexes of the liquid preparation produced are not satisfied.
Example 5
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this example consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine (aniriflutorin), diethyl aminoethyl hexanoate, a stabilizer, an emulsifier, a solvent and a cosolvent; the types of stabilizers, emulsifiers, solvents and co-solvents and mass fractions of the components are shown in table 17. The EO/PO block polyethers in Table 17 were manufactured by Nanje Jie Runner technology Co., ltd, and had a product model of Ethylan NS-500LQ, and the molar ratio of EO/PO in the EO/PO block polyethers was 1:1.71.
TABLE 17 types of stabilizers, emulsifiers, solvents and cosolvents in liquid formulations of example 5, mass fractions of the respective components
| Type of material | Composition of the composition | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 2 |
| Active ingredient | Diethyl aminoethyl hexanoate | 8 |
| Cosolvent | N-methylpyrrolidone | 15 |
| Stabilizing agent | BHT (2, 6-Di-tert-butyl-p-cresol) | 2 |
| Emulsifying agent | EO/PO block polyether | 1 |
| Solvent(s) | N, N-dimethylformamide | 72 |
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment specifically comprises the following steps: pumping the cosolvent into a reaction kettle by using a diaphragm pump, starting stirring, wherein the stirring speed is 80 revolutions per minute, adding the aniif lupulin and the diethyl aminoethyl hexanoate while stirring, and stirring for 30 minutes after the adding is finished, wherein no solute particles are visible in the reaction kettle, so that the complete dissolution is achieved; sequentially adding a stabilizer and an emulsifier, continuously stirring for 60min, finally adding a solvent, and continuously stirring for 30min to obtain a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine.
In other embodiments, the stirring speed is controlled to be 40-80 rpm when preparing the liquid preparation; after the addition of the aniiflupulin and the diethyl aminoethyl hexanoate is finished, the stirring time is controlled to be 30-60min; adding stabilizer and emulsifier, and stirring for 30-60min; after the solvent is added, the stirring time is controlled to be 30-60min.
The liquid formulations of this example were tested for aniriflutuprin, diethyl aminoethyl hexanoate content, pH, long-lasting foamability, dilution stability, low temperature stability, and heat storage stability, and the results are shown in table 18.
Table 18 results of performance test of the liquid formulation of example 5
| Project | Index (I) | Detection result | Result determination |
| Mass fraction of aniriflupulin% | 2.0±0.3 | 2.1 | Qualified product |
| Fresh amineMass fraction of esters,% | 8±0.8 | 7.9 | Qualified product |
| pH value of | 5.0-8.0 | 7.52 | Qualified product |
| Lasting foamability (after 1 min), mL < | 40 | 18 | Qualified product |
| Dilution stability | Qualified product | Qualified product | Qualified product |
| Low temperature stability | Qualified product | Qualified product | Qualified product |
| Thermal storage stability | Qualified product | Qualified product | Qualified product |
In order to examine the influence of different cosolvents on the liquid preparation, 15g of cosolvent is added into a mixing device, 2.00g of aniiflupulin and 8.00g of diethyl aminoethyl hexanoate are accurately weighed, stirred and dissolved for 30min under the condition of rotating speed of 80 r/min, and the dissolution conditions of the aniiflupulin and diethyl aminoethyl hexanoate are observed, and the results are shown in table 19.
TABLE 19 dissolution of different cosolvents on aniriflutuprin, diethyl aminoethyl hexanoate
As is clear from Table 19, when trimethyl phosphate, monoethanolamine, methyl isobutyl ketone, ethylene glycol and N-methylpyrrolidone of the same mass were used as the dissolution materials, only ethylene glycol and N-methylpyrrolidone had the best dissolution effects on aniif lupulin and diethyl aminoethyl hexanoate.
To examine the effect of the stabilizer on the liquid formulation, liquid formulations containing different stabilizers were prepared according to the preparation method of the liquid formulation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 5, and the types of the stabilizers and the dilution stability of each of the prepared liquid formulations are shown in table 20. BHT in Table 20 represents 2, 6-di-tert-butyl-p-cresol, TBHQ represents tert-butylhydroquinone, and the manufacturer of EO/PO block polyether is Nanjie Jie Runner technology Co., ltd, and the product model is Ethylan NS-500LQ.
TABLE 20 types of stabilizers and dilution stability of the respective liquid formulations prepared
As can be seen from table 20, when BHT or TBHQ was used as the stabilizer, the dilution stability of the preparation was acceptable; when iron sulfate, ammonia water and tea polyphenol are selected as stabilizers, precipitation appears at the bottom of the liquid preparation during the test of dilution stability, and the liquid preparation is unqualified.
The test results for dilution stability were all unacceptable when the co-solvent in table 20 was replaced with ethylene glycol from N-methylpyrrolidone or tween 80 from EO/PO block polyether.
Finally, the influence of the dosage of each component on the liquid preparation is examined, and the specific method is as follows: the liquid preparation was prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 5, except that the mass fraction of each component was changed, and the results show that when the mass fraction of aniflupurin was less than or equal to 2%, the mass fraction of diethyl aminoethyl hexanoate was less than or equal to 8%, the mass fraction of cosolvent was 20-30%, the mass fraction of stabilizer was 1-3%, the mass fraction of emulsifier was 0.5-2%, and the balance was solvent, the prepared liquid preparation was clear and transparent liquid, and the pH value was 2-5, and the test results of durable foamability, dilution stability, low temperature stability and heat storage stability were all qualified. When the mass fraction of a certain component constituting the liquid preparation is not within the above-mentioned numerical range, one or more of the performance indexes of the liquid preparation produced are not satisfied.
Example 6
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment consists of the following components in percentage by mass: consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine (aniriflupulin), ethephon, an emulsifying agent, a solvent and a cosolvent; the types of emulsifier, solvent and co-solvent and mass fractions of the components are shown in table 21.
TABLE 21 types of emulsifiers, solvents and cosolvents in liquid formulation of example 6, mass fractions of each component
| Type of material | Composition of the composition | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 0.5 |
| Active ingredient | Ethephon | 29.5 |
| Cosolvent | Lactic acid | 35 |
| Emulsifying agent | Polyethylene glycol 400 | 5 |
| Solvent(s) | Deionized water | 30 |
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment specifically comprises the following steps: pumping the cosolvent into a reaction kettle by using a diaphragm pump, starting stirring, wherein the stirring speed is 80 revolutions per minute, adding aniif lupulin and ethephon while stirring, and stirring for 30 minutes after the adding is finished, wherein no solute particles are visible in the reaction kettle, so that the complete dissolution is achieved; sequentially adding the emulsifying agent, continuously stirring for 60min, finally adding the solvent, and continuously stirring for 30min to obtain the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine.
In other embodiments, the stirring speed is controlled to be 40-80 rpm when preparing the liquid preparation; after the addition of the aniiflupulin and the ethephon are finished, the stirring time is controlled to be 30-60min; after adding the emulsifying agent, controlling the stirring time to be 30-60min; after the solvent is added, the stirring time is controlled to be 30-60min.
The liquid formulations of this example were tested for aniriflutuprin, ethephon content, pH, long-lasting foamability, dilution stability, low temperature stability and heat storage stability, and the results are shown in table 22.
Table 22 results of performance test of the liquid formulation of example 6
| Project | Index (I) | Detection result | Result determination |
| Mass fraction of aniriflupulin% | 0.5±0.075 | 0.506 | Qualified product |
| Mass fraction of ethephon,% | 29.5±1.475 | 29.8 | Qualified product |
| pH value of | 2.0-5.0 | 2.38 | Qualified product |
| Lasting foamability (after 1 min), mL < | 40 | 10 | Qualified product |
| Dilution stability | Qualified product | Qualified product | Qualified product |
| Low temperature stability | Qualified product | Qualified product | Qualified product |
| Thermal storage stability | Qualified product | Qualified product | Qualified product |
In order to examine the influence of different cosolvents on the liquid preparation, 35g of cosolvent is added into a mixing device, 0.5g of aniflupurin and 29.5g of ethephon are accurately weighed, stirred and dissolved for 30min under the condition of rotating speed of 80 revolutions per minute, and the dissolution conditions of the aniflupurin and the ethephon are observed, and the results are shown in table 23.
TABLE 23 dissolution of different cosolvents on anirifluprin and ethephon
As is clear from Table 23, when the raw materials were dissolved in the same mass of absolute ethyl alcohol, n-butanol, ethyl acetate, propionic acid and lactic acid, only propionic acid and lactic acid had the best dissolution effect on aniifluprin and ethephon.
To examine the effect of the solvent on the liquid preparation, liquid preparations containing different solvents, the types of solvents and the dilution stability of each of the prepared liquid preparations are shown in Table 24, were prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 6.
TABLE 24 types of solvents and dilution stability of the resulting liquid formulations
| Type of material | Composition of the composition | Mass fraction (%) | Mass fraction (%) | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 0.5 | 0.5 | 0.5 |
| Active ingredient | Ethephon | 29.5 | 29.5 | 29.5 |
| Cosolvent | Lactic acid | 35 | 35 | 35 |
| Emulsifying agent | Polyethylene glycol 400 | 5 | 5 | 5 |
| Solvent(s) | Ethylene glycol | 30 | - | - |
| Solvent(s) | Propylene glycol | - | 30 | - |
| Solvent(s) | Deionized water | - | - | 30 |
| Dilution stability | - | Qualified product | Qualified product | Qualified product |
As can be seen from Table 24, when ethylene glycol, propylene glycol and deionized water are selected as solvents, the dilution stability of the preparation is qualified; but the cost of deionized water is lower.
The test results for dilution stability were all failed when the co-solvent in table 24 was replaced with propionic acid or the emulsifier was replaced with tween 80 from polyethylene glycol 400.
Finally, the influence of the dosage of each component on the liquid preparation is examined, and the specific method is as follows: the liquid preparation was prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 6, except that the mass fraction of each component was changed, and the results showed that when the mass fraction of aniflupurin was not more than 0.5%, the mass fraction of ethephon was not more than 29.5%, the mass fraction of cosolvent was 30-40%, the mass fraction of emulsifier was 3-6%, and the balance was solvent, the prepared liquid preparation was clear and transparent liquid, and the pH was 2-5, and the test results of durable foamability, dilution stability, low temperature stability and heat storage stability were all acceptable. When the mass fraction of a certain component constituting the liquid preparation is not within the above-mentioned numerical range, one or more of the performance indexes of the liquid preparation produced are not satisfied.
Example 7
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this example consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine (anirifluprin), triacontanol, a stabilizer, an emulsifier, a solvent and a cosolvent; the types of stabilizers, emulsifiers, solvents and co-solvents and mass fractions of the components are shown in table 25.
TABLE 25 types of stabilizers, emulsifiers, solvents and cosolvents in liquid formulations of example 7, mass fractions of the components
| Type of material | Composition of the composition | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 1.9 |
| Active ingredient | Triacontanol | 0.1 |
| Cosolvent | Dimethyl sulfoxide | 15 |
| Stabilizing agent | Glacial acetic acid | 2 |
| Emulsifying agent | Fatty alcohol polyoxyethylene ether | 4 |
| Solvent(s) | Propylene glycol | 77 |
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment specifically comprises the following steps: pumping the cosolvent into a reaction kettle by using a diaphragm pump, starting stirring, wherein the stirring speed is 80 revolutions per minute, adding the aniif lupulin and the triacontanol while stirring, and stirring for 30 minutes after the adding is finished, wherein no solute particles are visible in the reaction kettle, so that the complete dissolution is achieved; sequentially adding a stabilizer and an emulsifier, continuously stirring for 60min, finally adding a solvent, and continuously stirring for 30min to obtain a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine.
In other embodiments, the stirring speed is controlled to be 40-80 rpm when preparing the liquid preparation; after the addition of the aniif lupulin and the triacontanol is finished, controlling the stirring time to be 30-60min; adding stabilizer and emulsifier, and stirring for 30-60min; after the solvent is added, the stirring time is controlled to be 30-60min.
The liquid formulations of this example were tested for the content of aniriflutuprin, triacontanol, pH, long-lasting foamability, dilution stability, low temperature stability and heat storage stability, and the results are shown in table 26.
Table 26 results of performance test of the liquid formulation of example 7
| Project | Index (I) | Detection result | Result determination |
| Mass fraction of aniriflupulin% | 1.9±0.285 | 1.931 | Qualified product |
| Triacontanol mass fraction% | 0.1±0.015 | 0.105 | Qualified product |
| pH value of | 2.0-5.0 | 3.68 | Qualified product |
| Lasting foamability (after 1 min), mL < | 40 | 24 | Qualified product |
| Dilution stability | Qualified product | Qualified product | Qualified product |
| Low temperature stability | Qualified product | Qualified product | Qualified product |
| Thermal storage stability | Qualified product | Qualified product | Qualified product |
In order to examine the influence of different cosolvents on the liquid preparation, 15g of cosolvent is added into a mixing device, 1.9g of aniflupurin and 0.1g of triacontanol are accurately weighed, stirred and dissolved for 30min under the condition of rotating speed of 80 revolutions per minute, and the dissolution conditions of the aniflupurin and the triacontanol are observed, and the results are shown in table 27.
TABLE 27 dissolution of different cosolvents on aniriflutuprin, triacontanol
As is clear from Table 27, when trimethyl phosphate, monoethanolamine, methyl isobutyl ketone, ethylene glycol and dimethyl sulfoxide having the same mass were used to dissolve the raw materials, only ethylene glycol and dimethyl sulfoxide had the best dissolution effect on aniifluprin and triacontanol.
To examine the effect of the stabilizer on the liquid preparation, liquid preparations containing different stabilizers were prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 7, and the types of the stabilizers and the dilution stability of each of the prepared liquid preparations are shown in table 28.
Table 28 type of stabilizer and dilution stability of each liquid formulation produced
As can be seen from table 28, when glacial acetic acid was used as the stabilizer, the dilution stability of the formulations was acceptable; when ferric sulfate, ammonia water and lactic acid are used as stabilizers, precipitation appears at the bottom of the liquid preparation during the test of dilution stability, and the liquid preparation is unqualified.
When the cosolvent in Table 28 was replaced with ethylene glycol or the emulsifier was replaced with polyoxyethylene fatty alcohol ether, the test results of dilution stability were all failed.
Finally, the influence of the dosage of each component on the liquid preparation is examined, and the specific method is as follows: the liquid preparation was prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 7, except that the mass fraction of each component was changed, and the results showed that when the mass fraction of aniflupurin was 1.9% or less, the mass fraction of triacontanol was 0.1% or less, the mass fraction of the cosolvent was 10 to 20%, the mass fraction of the stabilizer was 1 to 3%, the mass fraction of the emulsifier was 2 to 6%, and the balance was the solvent, the prepared liquid preparation was clear and transparent liquid, and the pH was 2 to 5, and the test results of the permanent foaming property, the dilution stability, the low temperature stability and the heat storage stability were all qualified. When the mass fraction of a certain component constituting the liquid preparation is not within the above-mentioned numerical range, one or more of the performance indexes of the liquid preparation produced are not satisfied.
Example 8
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment consists of the following components in percentage by mass: consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine (aniriflupulin), triacontanol, a stabilizer, an emulsifier, a solvent and a cosolvent; the types of stabilizers, emulsifiers, solvents and co-solvents and mass fractions of the components are shown in table 29.
TABLE 29 types of stabilizers, emulsifiers, solvents and cosolvents in liquid formulations of example 8, mass fractions of the respective components
| Type of material | Composition of the composition | Mass fraction (%) |
| Active ingredient | Anisiflupurin | 9.8 |
| Active ingredient | Triacontanol | 0.2 |
| Cosolvent | N-methylpyrrolidone | 35 |
| Stabilizing agent | Formic acid | 8 |
| Emulsifying agent | Tween 80 | 5 |
| Solvent(s) | N, N-dimethylformamide | 42 |
The preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of the embodiment specifically comprises the following steps: pumping the cosolvent into a reaction kettle by using a diaphragm pump, starting stirring at a stirring speed of 40 revolutions per minute, adding aniif lupulin and triacontanol while stirring, and stirring for 60 minutes again after the addition is finished, wherein no solute particles are visible in the reaction kettle, so that the complete dissolution is achieved; sequentially adding a stabilizer and an emulsifier, continuously stirring for 30min, finally adding a solvent, and continuously stirring for 60min to obtain a liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine.
In other embodiments, the stirring speed is controlled to be 40-80 rpm when preparing the liquid preparation; after the addition of the aniif lupulin and the triacontanol is finished, controlling the stirring time to be 30-60min; adding stabilizer and emulsifier, and stirring for 30-60min; after the solvent is added, the stirring time is controlled to be 30-60min.
The liquid formulations of this example were tested for the content of aniriflutuprin, triacontanol, pH, long-lasting foamability, dilution stability, low temperature stability and heat storage stability, and the results are shown in table 30.
Table 30 results of performance test of the liquid formulation of example 8
In order to examine the influence of different cosolvents on the liquid preparation, 35g of cosolvent is added into a mixing device, 9.8g of aniflupurin and 0.2g of triacontanol are accurately weighed, and are stirred and dissolved for 60min under the condition of 40 revolutions per minute, and the dissolution conditions of the aniflupurin and the triacontanol are observed, and the results are shown in table 31.
TABLE 31 dissolution of different cosolvents on aniriflutuprin, triacontanol
As is clear from Table 31, when N-butanol, triethanolamine, propylene carbonate, propylene glycol and N-methylpyrrolidone of the same mass were used as the dissolution materials, only propylene glycol and N-methylpyrrolidone had the best dissolution effect on aniif lupulin and triacontanol.
To examine the effect of the stabilizer on the liquid preparation, liquid preparations containing different stabilizers were prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 8, and the types of the stabilizers and the dilution stability of each of the prepared liquid preparations are shown in table 32.
TABLE 32 types of stabilizers and dilution stability of the respective liquid formulations prepared
As can be seen from table 32, when formic acid was used as the stabilizer, the dilution stability of the formulation was acceptable; when aluminum formate, magnesium formate and malic acid are selected as stabilizers, precipitation appears at the bottom of the liquid preparation during the test of dilution stability, and the liquid preparation is unqualified.
When the cosolvent in table 32 was replaced with propylene glycol from N-methylpyrrolidone or the emulsifier with span 80 from tween 80, the test results of dilution stability were all failed.
Finally, the influence of the dosage of each component on the liquid preparation is examined, and the specific method is as follows: the liquid preparation was prepared according to the preparation method of the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 8, except that the mass fraction of each component was changed, and the results showed that when the mass fraction of aniflupurin was > 1.9% and was not more than 9.8%, the mass fraction of triacontanol was > 0.1% and was not more than 0.2%, the mass fraction of cosolvent was 30 to 40%, the mass fraction of stabilizer was 6 to 10%, the mass fraction of emulsifier was 3 to 7%, and the balance was solvent, the prepared liquid preparation was clear and transparent liquid, and the pH was 2 to 5, and the test results of permanent foaming, dilution stability, low temperature stability and heat storage stability were all acceptable. When the mass fraction of a certain component constituting the liquid preparation is not within the above-mentioned numerical range, one or more of the performance indexes of the liquid preparation produced are not satisfied.
Comparative example 1
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 1 only in that the mass fraction of gibberellic acid GA3 in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 2
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 2 only in that the mass fraction of gibberellic acid GA4+7 in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 3
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 3 only in that the mass fraction of 24-epibrassinolide in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 4
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 4 only in that the mass fraction of 28-Gao Yuntai lactone in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 5
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 5 only in that the mass fraction of diethyl aminoether in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 6
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 6 only in that the mass fraction of ethephon in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 7
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 5 only in that the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 8
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 6 only in that the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 9
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 7 only in that the mass fraction of triacontanol in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Comparative example 10
The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was different from the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of example 8 only in that the mass fraction of triacontanol in the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of this comparative example was 0.
Experimental example 1
To evaluate the effect of the 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine-containing liquid formulations of examples 1 and 2 on oat coleoptile growth, a commercially available 4% gibberellic acid soluble solution (produced by zheng chemical company, inc.) was used as a control agent, while clear water was used as a blank, and then the different formulations were diluted with clear water to obtain test agents. The effect of each test agent on oat coleoptile growth was then tested as follows: culturing oat under dark condition, cutting bud sheath from oat seedling when oat seedling grows to about 5cm, cutting off top end of bud sheath (length of 6 mm), removing bud sheath, and cutting 1cm section by quantitative shearing knife at the top end of bud sheath. The bud sheath sections were then immersed in a phosphate-citrate buffer (ph=5.0) containing 2% (mass fraction) sucrose for 3 hours, and endogenous auxin was washed away. Then taking washed and dried culture dishes, placing 10 bud sheath segments for washing endogenous auxin into each culture dish, adding the same test reagent (the volume is 20 mL) into each culture dish, soaking the bud sheath segments in the culture dish in the test reagent, setting 5 parallel experiments for each test reagent (namely, the number of the culture dishes added corresponding to each test reagent is 5), placing the culture dishes added with the test reagent and the bud sheath segments in a shaking table, culturing for 24 hours or 48 hours in dark condition, testing the growth amount of each bud sheath segment in each culture dish after culturing is finished, calculating the average value of the growth amounts of all bud sheath segments in 5 culture dishes corresponding to each test reagent, taking the calculated average value as the test result of the growth amounts of the bud sheath segments corresponding to the corresponding test reagent, defining the test result of the bud sheath segments corresponding to the test reagent as M, and calculating the growth rate of the bud sheath corresponding to each test reagent according to the formula: coleoptile growth rate (%) = (test result of growth amount of coleoptile section-M)/mx100. The numbers of the test reagents, the concentrations of the active ingredients (2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine, gibberellic acid GA3 and gibberellic acid GA 4+7) in the test reagents, and the corresponding coleoptile growth rates of the test reagents at different culture times are shown in Table 33.
TABLE 33 number of each test reagent, concentration of active ingredient in each test reagent, and coleoptile growth rate corresponding to each test reagent at different incubation times
As is clear from Table 33, the liquid formulations containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of examples 1-2 all had the effect of promoting coleoptile growth and were superior to the effect of gibberellic acid, a control agent (conventional plant conditioner), on coleoptile growth.
Experimental example 2
To evaluate the effect of the 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine-containing liquid formulations of examples 3 and 4 on crop growth, a commercially available 0.01% 24-epibrassinolide soluble (produced by zheng Zhengzhou chemical company) and a commercially available 0.01% 28-Gao Yuntai-lactone soluble (produced by zheng Zhengzhou chemical company) were used as the control agent 1 and the control agent 2, respectively, with clear water as a blank, and then the different formulations were diluted with clear water to obtain test agents. Then, the influence of each test reagent on peanut growth is tested, and the test method is as follows: selecting a peanut field with consistent growth vigor (peanuts in the peanut field are in a seedling stage), randomly dividing regions, covering three rows of peanuts in each region, setting one row of peanuts with width between different regions as a protection row, and dividing the regions into three rows of peanut rows, wherein the three rows of peanut rows are respectively arranged in the protection rows The areas of the subareas are all 30m 2 The identification plate is manufactured in different subareas, then different test reagents are uniformly sprayed on peanut plants in different subareas in a spraying mode by using an electric sprayer, the number of subareas corresponding to each test reagent is 1, the quality of liquid preparations sprayed on peanuts in each subarea is the same, and the spraying method is the same. And finally testing the height, chlorophyll content, protein content and fat content of peanut plants 7d after spraying. The testing method of the peanut plant height, chlorophyll content, protein content and fat content comprises the following steps:
(1) Plant height: and each subarea randomly selects 10 peanut plants at different positions as sampling points, marks the positions, uniformly measures the height of the main stems of the peanuts in order to ensure the accuracy and the representativeness of data, adopts a steel tape measure to measure the distance from the root to the stem tip growth point, the measured distance is the height of the main stems of the peanut plants, and the average value of the heights of the main stems of 10 peanut plants randomly selected in each subarea is used as the test result of the height of the main stems of the peanut plants in the subarea.
(2) Chlorophyll content: and randomly selecting peanut plants at 5 different positions from each partition as sampling points and registering and marking. Chlorophyll content, protein content and fat content of 2 leaves out of all leaves except the new leaf in the upper layer of peanut plants at each sampling point were randomly determined. Taking the average value of chlorophyll content of 2 leaves corresponding to each sampling point as the representative value of chlorophyll level of peanut plants at the sampling points, wherein a chlorophyll content testing instrument is a KonicaMinoltaSPAD502 handheld chlorophyll meter; taking the average value of the protein content of 2 leaves corresponding to each sampling point as the protein level representative value of the peanut plants at the sampling points, and measuring the protein content by adopting a full-automatic Kjeldahl nitrogen analyzer; the average value of the fat content of 2 leaves corresponding to each sampling point is taken as the representative value of the fat level of the peanut plants at the sampling point, and the fat content is measured by a fat meter. And finally, calculating the average value of chlorophyll level representative values, the average value of protein level representative values and the average value of fat level representative values of peanut plants at 5 different positions in each partition, and taking the calculated average values as a test result of chlorophyll content, a test result of protein content and a test result of fat content of the peanut plants in the partition respectively.
The numbers of the test reagents, the concentrations of the active ingredients (2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine, 24-epibrassinolide and 28-Gao Yuntai-lactone) in the test reagents, and the test results of the plant height, chlorophyll content, protein content and fat content of peanuts after the use of the test reagents are shown in table 34.
TABLE 34 numbering of each test agent, concentration of active ingredient in each test agent, and results of testing plant height, chlorophyll content, protein content and fat content of peanuts after use of each test agent
As can be seen from Table 34, the liquid formulations of examples 3-4 containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine all have the effect of promoting the growth of peanut plants, and compared with the blank control group (clear water), the liquid formulations of examples 3-4 can obviously improve the chlorophyll content, protein content and fat content in the leaves of peanut plants, can obviously promote the growth of peanuts, and can improve the accumulation of chlorophyll, thereby being beneficial to the accumulation of photosynthetic products, promoting the full fruit, increasing the yield and improving the quality.
Experimental example 3
To evaluate the effect of the 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine-containing liquid formulations of examples 5 and 6 on crop growth, the test agent was obtained by using 30% of commercially available diethyl aminoethyl hexanoate ethylene Li Shuiji (produced by zheng chemical industry products limited company) as a control agent, and using clear water as a blank, and then diluting the different formulations with clear water. And then the method in the standard GB/T17980.145-2004 pesticide field efficacy test criterion (II) is implemented by taking Fuji apples with the same growth vigor as an experimental object. The method comprises the steps of uniformly spraying test reagents on stems and leaves of apple plants in a fruit setting period and a fruit swelling period, wherein the area of each apple plant sprayed by each test reagent is 1 mu, the quality of each test reagent sprayed on each apple plant is the same, after each test reagent is sprayed, the existence of phytotoxicity is investigated in 3d, meanwhile, the data of fruit setting rate, single fruit weight, quality and the like are investigated, the content of vitamin C in fresh fruits and the hardness of apple fruits are tested, 5 apple plants sprayed by each test reagent are randomly selected as test samples in the test, and the average value of the test results of 5 apple plants is used as the test result of the fruit setting rate, the single fruit weight of apples after the corresponding test reagent is used, the content of vitamin C in fresh fruits and the hardness of apple fruits.
The numbers of the respective test agents, the concentrations of the active ingredients (2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine, diethyl aminoethyl hexanoate and ethephon) in the respective test agents, and the results of the tests of the fruit setting rate, the weight of single fruit, the vitamin C content in fresh fruit and the hardness of apple fruit after using the respective test agents are shown in table 35.
Table 35 number of each test reagent, concentration of active ingredient in each test reagent, and coleoptile growth rate corresponding to each test reagent at different incubation times
As is clear from Table 35, the liquid formulations of examples 5 to 6 containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine showed an increase in apple fruit setting rate, an increase in weight of individual apples, and an increase in vitamin C content in the fruits after spraying the apples.
Experimental example 4
To evaluate the effect of the 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine-containing liquid formulations of examples 7 and 8 on crop growth, the test agent was obtained by using a commercially available 0.1% triacontanol soluble (manufactured by the company of the pharmaceutical industry, inc.) as a control agent, and clear water as a blank, and then diluting the different formulations with clear water. And then taking mango of a first variety of Tainong as a test object, wherein 5 mango trees are used for applying the same test reagent, each mango tree is only applied with one test reagent, before the application of the test reagent, each mango tree is marked with 3 flower-shaped battles according to five directions of east, south, west and north, each direction is marked (the diameters of young fruits on the flower-shaped battles are 0.8-1 cm, the total amount of the young fruits on the flower-shaped battles is consistent), then the marked flower-shaped battles are immersed in the test reagent, so that the test reagent is used for immersing the young fruits, the test reagent is shared for 2 times in a test period, the application interval of the two times is 7 days, the time of each flower-shaped battle immersing the test reagent is the same, the aspect diameter of the fruit is investigated on the day before the first application, then the second application is carried out on the day 7 after the first application while the aspect diameter of the fruit is investigated, and the aspect diameter of the fruit on the day 7 after the second application is calculated, and the aspect diameter of the fruit on the day 7 after the first application is increased compared with the aspect diameter of the fruit on the day before the first application and the aspect diameter of the fruit on the day 7 application is increased after the day 7 application. Finally, the average value of the increase in the longitudinal and transverse diameters of all marked fruits on 5 mango trees applied with each test agent at the 7 th day after the first application and the average value of the increase in the longitudinal and transverse diameters of the fruits at the 7 th day after the second application are calculated.
The numbers of the test reagents, the concentrations of the active ingredients (2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and triacontanol) in the test reagents, the increase in the longitudinal and transverse diameters of the fruits at day 7 after the first administration and the increase in the longitudinal and transverse diameters of the fruits at day 7 after the second administration of the test reagents are shown in table 36.
TABLE 36 number of each test agent, concentration of active ingredient in each test agent, and increase in longitudinal and transverse diameters of mango young fruit by each test agent
As is clear from Table 36, the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine of examples 7 to 8 was used to promote the growth of the longitudinal and transverse diameters of the young mango fruits after the young mango fruits were immersed in the liquid preparation, and the promotion effect was remarkably improved with the increase of the concentration of the active ingredient. In addition, when the concentrations of the active ingredients were the same, the increase in the longitudinal and transverse diameters of mango fruits was significantly greater on day 7 after the second administration of the 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine-containing liquid preparation of examples 7-8, compared with the control agent, indicating that the 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine-containing liquid preparation of examples 7-8 has a better promoting effect on the growth of young mango fruits.
Claims (10)
1. A liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine is characterized by mainly comprising an active ingredient, an emulsifying agent, a solvent and a cosolvent; the active ingredient consists of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and a compound; the compound is gibberellic acid GA3, gibberellic acid GA4+7, 24-epibrassinolide, 28-Gao Yuntai lactone, diethyl aminoethyl hexanoate, ethephon or triacontanol; the cosolvent is dimethyl sulfoxide, N-dimethylformamide, N-methylpyrrolidone and lactic acid; the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine in the liquid preparation is not more than 10%; the mass fraction of the compound in the liquid preparation is not more than 30%.
2. The liquid formulation comprising 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to claim 1, wherein the complex is gibberellic acid GA3, and wherein the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and gibberellic acid GA3 in the liquid formulation is independently not more than 0.9%;
or the compound is gibberellic acid GA4+7, and the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine and gibberellic acid GA4+7 in the liquid preparation is not more than 1.8% independently;
Or the compound is 24-epibrassinolide, the mass fraction of 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.99%, and the mass fraction of 24-epibrassinolide is not more than 0.01%;
or the compound is 28-Gao Yuntai lactone, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 4.995%, and the mass fraction of the 28-Gao Yuntai lactone is not more than 0.005%;
or the compound is diethyl aminoethyl hexanoate, wherein the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 2%, and the mass fraction of the diethyl aminoethyl hexanoate is not more than 8%;
or the compound is ethephon, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 0.5%, and the mass fraction of the ethephon is not more than 29.5%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 9.8%, and the mass fraction of the triacontanol is not more than 0.2%.
3. The liquid formulation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to claim 1 or 2, wherein the compound is gibberellic acid GA3, gibberellic acid GA4+7, 24-epibrassinolide, 28-Gao Yuntai lactone, diethyl aminoethyl hexanoate or triacontanol, and the liquid formulation further comprises a stabilizer which is formic acid, acetic acid, lactic acid, 2, 6-di-t-butyl-p-cresol, t-butyl hydroquinone.
4. A liquid formulation comprising 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to claim 3, wherein the complex is gibberellic acid GA3 and the stabilizing agent is formic acid and/or lactic acid;
or the compound is gibberellic acid GA4+7, and the stabilizer is formic acid and/or lactic acid;
or the compound is 24-epibrassinolide, and the stabilizer is formic acid and/or acetic acid;
or the compound is 28-Gao Yuntai lactone, and the stabilizer is formic acid and/or acetic acid;
or the compound is diethyl aminoethyl hexanoate, and the stabilizer is 2, 6-di-tert-butyl-p-cresol or tert-butyl hydroquinone;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, the mass fraction of the triacontanol in the liquid preparation is not more than 0.1%, and the stabilizer in the liquid preparation is acetic acid;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the stabilizer in the liquid preparation is formic acid.
5. The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to claim 4, wherein the compound is gibberellic acid GA3, and the mass fraction of the stabilizer in the liquid preparation is 0.5-2%;
or the compound is gibberellic acid GA4+7, and the mass fraction of the stabilizer in the liquid preparation is 10-20%;
or the compound is 24-epibrassinolide, and the mass fraction of the stabilizer in the liquid preparation is 3-6%;
or the compound is 28-Gao Yuntai lactone, and the mass fraction of the stabilizer in the liquid preparation is 0.3-0.6%;
or the compound is diethyl aminoethyl hexanoate, and the mass fraction of the stabilizer in the liquid preparation is 1-3%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, the mass fraction of the triacontanol in the liquid preparation is not more than 0.1%, and the mass fraction of the stabilizer in the liquid preparation is 1-3%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the mass fraction of the stabilizer in the liquid preparation is 6-10%.
6. The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to claim 1 or 2, wherein the compound is gibberellic acid GA3, and the emulsifier in the liquid preparation is octyl phenol polyoxyethylene ether and/or fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the liquid preparation is 1-4%;
or the compound is gibberellic acid GA4+7, and the emulsifier in the liquid preparation is octyl phenol polyoxyethylene ether and/or fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the liquid preparation is 2-4%;
or the compound is 24-epibrassinolide, and the emulsifier in the liquid preparation is Tween 80; the mass fraction of the emulsifier in the liquid preparation is 3-7%;
or the compound is 28-Gao Yuntai lactone, and the emulsifying agent in the liquid preparation is polyethylene glycol 400; the mass fraction of the emulsifier in the liquid preparation is 4-8%;
or the compound is diethyl aminoethyl hexanoate, and the emulsifier in the liquid preparation is polyether; the mass fraction of the emulsifier in the liquid preparation is 0.5-2%;
or the compound is ethephon, and the emulsifier in the liquid preparation is polyethylene glycol 400; the mass fraction of the emulsifier in the liquid preparation is 3-6%;
Or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, and the emulsifier in the liquid preparation is fatty alcohol polyoxyethylene ether; the mass fraction of the emulsifier in the liquid preparation is 2-6%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the emulsifier in the liquid preparation is Tween 80; the mass fraction of the emulsifier in the liquid preparation is 3-7%.
7. The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to claim 1 or 2, wherein the compound is gibberellic acid GA3, and the cosolvent in the liquid preparation is dimethyl sulfoxide; the mass fraction of the cosolvent in the liquid preparation is 15-25%;
or the compound is gibberellic acid GA4+7, and the cosolvent in the liquid preparation is N, N-dimethylformamide; the mass fraction of the cosolvent in the liquid preparation is 30-40%;
Or the compound is 24-epibrassinolide, and the cosolvent in the liquid preparation is N-methylpyrrolidone and/or dimethyl sulfoxide; the mass fraction of the cosolvent in the liquid preparation is 10-20%;
or the compound is 28-Gao Yuntai lactone, and the cosolvent in the liquid preparation is N-methylpyrrolidone and/or dimethyl sulfoxide; the mass fraction of the cosolvent in the liquid preparation is 20-40%;
or the compound is diethyl aminoethyl hexanoate, and the cosolvent in the liquid preparation is N-methyl pyrrolidone; the mass fraction of the cosolvent in the liquid preparation is 20-30%;
or the compound is ethephon, and the cosolvent in the liquid preparation is lactic acid; the mass fraction of the cosolvent in the liquid preparation is 30-40%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, the mass fraction of the triacontanol in the liquid preparation is not more than 0.1%, and the cosolvent in the liquid preparation is dimethyl sulfoxide; the mass fraction of the cosolvent in the liquid preparation is 10-20%;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the cosolvent in the liquid preparation is N-methylpyrrolidone; the mass fraction of the cosolvent in the liquid preparation is 30-40%.
8. The liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to claim 1 or 2, wherein the compound is gibberellic acid GA3, the solvent in the liquid preparation is an alcoholic solvent, and the alcoholic solvent is ethylene glycol and/or propylene glycol;
or the compound is gibberellic acid GA4+7, the solvent in the liquid preparation is an alcohol solvent, and the alcohol solvent is ethylene glycol and/or propylene glycol;
or the compound is 24-epibrassinolide, and the solvent in the liquid preparation is propylene glycol;
or the compound is 28-Gao Yuntai lactone, and the solvent in the liquid preparation is N, N-dimethylformamide;
or the compound is diethyl aminoethyl hexanoate, and the solvent in the liquid preparation is N, N-dimethylformamide;
or the compound is ethephon, and the solvent in the liquid preparation is selected from one or any combination of water, ethylene glycol and propylene glycol;
or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is not more than 1.9%, the mass fraction of the triacontanol in the liquid preparation is not more than 0.1%, and the solvent in the liquid preparation is propylene glycol;
Or the compound is triacontanol, the mass fraction of the 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine in the liquid preparation is more than 1.9% and less than or equal to 9.8%, the mass fraction of the triacontanol in the liquid preparation is more than 0.1% and less than or equal to 0.2%, and the solvent in the liquid preparation is N, N-dimethylformamide.
9. A process for the preparation of a liquid formulation comprising 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to any one of claims 1 to 8, comprising the steps of: the components with the formula amount are uniformly mixed to obtain the liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine.
10. Use of a liquid formulation comprising 2-fluoro-N- (3-methoxyphenyl) -7H-purin-6-amine according to any one of claims 1 to 8 as a plant growth regulator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310743489.0A CN116806838A (en) | 2023-06-21 | 2023-06-21 | Liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310743489.0A CN116806838A (en) | 2023-06-21 | 2023-06-21 | Liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116806838A true CN116806838A (en) | 2023-09-29 |
Family
ID=88113983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310743489.0A Pending CN116806838A (en) | 2023-06-21 | 2023-06-21 | Liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116806838A (en) |
-
2023
- 2023-06-21 CN CN202310743489.0A patent/CN116806838A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105557716A (en) | Pinoxaden and clodinafop-propargyl compound emulsifiable oil and preparation method thereof | |
| US20200236933A1 (en) | Use of a non-ionic surfactant which is a polyol derivative as a plant growth stimulating agent or as an adjuvant | |
| CN115968255A (en) | Solvent composition for promoting plant growth | |
| CN116806838A (en) | Liquid preparation containing 2-fluoro-N- (3-methoxyphenyl) -7H-purine-6-amine and preparation method and application thereof | |
| CN113396915A (en) | Compound plant growth regulator containing brassinolide and DA-7 or DA-8 | |
| CN116349678A (en) | Stress-resistant yield-increasing plant growth regulator and application thereof | |
| CN108863580B (en) | Leaf fertilizer containing L-pyroglutamic acid and use method thereof | |
| CN110771618A (en) | Plant growth regulator for mangoes | |
| CN114514930B (en) | Bactericidal composition for preventing and treating crop bacterial diseases | |
| CN105994276A (en) | Method for improving fruit setting rate of tomatoes | |
| CN105557712A (en) | Penoxsulam and fluroxypr-mepthyl compound dispersible oil suspending agent and preparation method thereof | |
| CN107212005A (en) | A kind of cyhalofop-butyl and bispyribac-sodium compound dispersible oil-suspending agent and preparation method thereof | |
| CN110352977B (en) | Pesticide composition containing forchlorfenuron, strigolactone and gamma-aminobutyric acid | |
| CN113180039A (en) | Special auxiliary agent for unmanned aerial vehicle plant protection and flying prevention and preparation method and application thereof | |
| CN105994272A (en) | Method for improving fruit setting rate of tomatoes in summer and autumn | |
| CN106070330A (en) | Wheat conditioner for preventing premature senility | |
| KR101091494B1 (en) | Method of reducing the sponginess and/or softness of oriental pears and composition thereof | |
| CN115850106B (en) | Compound with plant growth regulator action effect and application thereof | |
| CN114557350B (en) | Stable and high-control-efficiency herbicide and application thereof | |
| CN109907063A (en) | Plant growth regulator composition containing Thidiazuron | |
| CN107094772A (en) | A kind of 15% fenoxaprop and cyhalofop-butyl complex microemulsion and preparation method thereof | |
| CN115281195B (en) | Plant growth regulating composition for regulating tobacco growth | |
| CN115119844B (en) | Seedling antifreeze fluid and preparation method thereof | |
| CN106035350A (en) | Cyhalofop-butyl, metamifop and bentazone compounded dispersible oil suspended agent and preparation method thereof | |
| CN105475308A (en) | Compound dispersible oil suspension agent containing pyribenzoxim, penoxsulam and cyhalofop-butyl as well as preparation method thereof |
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 |