CN110208424A - Analysis method containing impurity in a kind of pesticide flonicamid - Google Patents
Analysis method containing impurity in a kind of pesticide flonicamid Download PDFInfo
- Publication number
- CN110208424A CN110208424A CN201910580373.3A CN201910580373A CN110208424A CN 110208424 A CN110208424 A CN 110208424A CN 201910580373 A CN201910580373 A CN 201910580373A CN 110208424 A CN110208424 A CN 110208424A
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- CN
- China
- Prior art keywords
- reference material
- flonicamid
- material solution
- pesticide
- solution
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The present invention provides the analysis method containing impurity in a kind of pesticide flonicamid, and in particular to pesticide impurities detection field is settled to 25mL using pure water by configuring 1 group of impure reference material solution；6 groups of subject active compound solutions are configured, 208.7mg, 194.2mg, 194.6mg, 208.5mg, 209.6mg, 208.7mg raw medicine is weighed respectively, is then settled to 25mL respectively；The molecule of blank testing solution and reference material solution adds hydrogen peak and molecule that hydrogen is added to add acetonitrile peak value, by comparing the peak value of blank solution and reference material solution, that is, speculates the dopant species of impure reference material solution.The present invention can efficiently identify impurity component from flonicamid raw medicine, and by mass spectral analysis, confirm the compound information of impurity, provide technical support for the production, registration and instruction of the pesticide.
Description
Technical field
The invention belongs to pesticide impurities detection fields, and in particular to the analysis containing impurity in a kind of pesticide flonicamid
Method.
Background technique
Flonicamid is a kind of novel low-toxicity picolinamide class insect growth regulator, IGR insecticides, obtains me within 2007
State's Pesticidal products temporary registration certificate, preparation are 10% water dispersible granules；Flonicamid, which removes to have, tags and stomach poison function, also has
There are good never poison and quick antifeedant effect.Sucking pest feeding sucking has the water of flonicamid
Afterwards, it can be prevented to inhale juice by rapid, absolutely not excreta occurs within an hour, finally dead due to starvation；
The physicochemical property and content analysis of flonicamid, national standard and professional standard have had corresponding detection to mark
Quasi- and specification, but the analysis of possible by-product and impurity in pesticide actual production is not also difficult at present
Unified examination criteria is made, lacks unified effective analysis means especially for the physico-chemical analysis of raw medicine.
In view of the above deficiencies, the analysis method containing impurity in a kind of pesticide flonicamid is now needed, it can be efficiently
Impurity component is identified from flonicamid raw medicine, and by mass spectral analysis, the compound information of impurity is confirmed, for the pesticide
Production, registration and instruction provide technical support.
Summary of the invention
The object of the present invention is to provide the analysis method containing impurity in a kind of pesticide flonicamid, can efficiently from
Impurity component is identified in flonicamid raw medicine, and by mass spectral analysis, the compound information of impurity is confirmed, for the pesticide
Production, registration and instruction provide technical support.
The present invention provides the following technical solutions:
Analysis method containing impurity in a kind of pesticide flonicamid, specific as follows:
S1,1 group of impure reference material solution is configured first, with spare；
S2, it is reconfigured several groups blank solution, with spare；
S3, setting mass spectrometer parameters, design parameter are as follows:
S4, after instrument stabilizer, mass spectrograph successively sample introduction: advanced needle blank solvent and reference material solution, then according to
Blank solvent, the sequence of subject solution are measured；
The molecule of S5, blank testing solution and reference material solution add hydrogen peak and molecule that hydrogen is added to add acetonitrile peak value, pass through comparison
The peak value of blank solution and reference material solution speculates the dopant species of impure reference material solution.
Preferably, in S1 step, 1 group of impure reference material solution is configured, is settled to 25mL using pure water.
Preferably, in S2 step, 6 groups of subject active compound solutions is configured, are then settled to 25mL respectively using pure water.
Preferably, 1 group of impure reference material solution is configured, adopts and weighs flonicamid impurity 19.5mg in the balance, is used
Pure water is settled to 25mL；Configure 6 groups of subject active compound solutions, weigh respectively 208.7mg, 194.2mg, 194.6mg, 208.5mg,
209.6mg, 208.7mg raw medicine, be then settled to 25mL respectively.
Beneficial effects of the present invention:
The present invention can efficiently identify impurity component, and pass through by mass-spectrometric technique from flonicamid raw medicine
Mass spectral analysis confirms the compound information of impurity, provides technical support for the production, registration and instruction of the pesticide.
Specific embodiment
Instrument is as follows with reagent: Waters Alliance 2695/ZQ2000 LC-MS instrument, Waters, US；
MassLynx work station, version number 4.1, Waters, US；LE204E/02 electronic balance, Mei Tele-support benefit instrument
(Shanghai) Co., Ltd.；LD-DI-Micro-15 type ultrapure water machine, Shanghai Li Ding Water Management Equipment Ltd.；Volumetric flask,
25mL, Shanghai Shen Bo instrument company；N- cyanogen methyl -6- (trifluoromethyl) niacinamide (I reference material of flonicamid impurity), batch
Number: 20170223, content 99.40%, Jiangsu Pesticide Research Institute Co., Ltd；Flonicamid raw medicine, Wuxi City are sowed
Precious pharmaceutcal corporation, Ltd；Ultrapure water is prepared by ultrapure water machine；Acetonitrile (lot number: 16115072), chromatographically pure, U.S. Tidea public affairs
Department.
Mass spectrograph operating condition is as follows: chromatographic column: Agilent Eclipse XDB-C184.6 × 250mm, and 5 μm, sequence
Number USNH024434；Column temperature: 35 DEG C；Mobile phase: CH3CN:H2O=50:50 (contains 0.3%HAc)；Flow velocity: 0.3mL/min；Fortune
The row time: 15min；Sample volume: 5 μ L；
Mass spectrometry parameters setting is as follows:
Details as Follows for the preparation of determination step solution:
Under the operating conditions described above, after instrument stabilizer, advanced needle raw medicine solvent and reference material solution, then according to original
Medicine solvent, subject active compound solution sequence be measured；
According to the total ion current figure and mass spectrogram of I reference material of flonicamid impurity.Impurity I retention time about 11.5min,
According to its total ion current figure and its mass spectrogram.
I interpretation of mass spectra of flonicamid raw medicine impurity
According to reaction raw materials and reaction route, thus it is speculated that impurity I is N- cyanogen methyl -6- (trifluoromethyl) niacinamide, structural formula
It is as follows:
The present invention can efficiently identify impurity component, and pass through by mass-spectrometric technique from flonicamid raw medicine
Mass spectral analysis confirms the compound information of impurity, for the pesticide production, registration and instruction provide technical support with
On be merely a preferred embodiment of the present invention, be not intended to restrict the invention, although with reference to the foregoing embodiments to the present invention into
Having gone detailed description for those skilled in the art still can be to technology documented by foregoing embodiments
Scheme is modified or equivalent replacement of some of the technical features.All within the spirits and principles of the present invention, institute
Any modification, equivalent substitution, improvement and etc. of work, should all be included in the protection scope of the present invention.
Claims (4)
1. the analysis method containing impurity in a kind of pesticide flonicamid, it is characterised in that: it is specific as follows,
S1,1 group of impure reference material solution is configured first, with spare；
S2, it is reconfigured several groups blank solution, with spare；
S3, setting mass spectrometer parameters, design parameter are as follows:
S4, after instrument stabilizer, mass spectrograph successively sample introduction: advanced needle blank solvent and reference material solution, then according to blank
Solvent, subject solution sequence be measured；
The molecule of S5, blank testing solution and reference material solution add hydrogen peak and molecule that hydrogen is added to add acetonitrile peak value, by comparing blank
The peak value of solution and reference material solution speculates the dopant species of impure reference material solution.
2. the analysis method containing impurity in a kind of pesticide flonicamid according to claim 1, it is characterised in that: S1
In step, 1 group of impure reference material solution is configured, is settled to 25mL using pure water.
3. the analysis method containing impurity in a kind of pesticide flonicamid according to claim 2, it is characterised in that: S2
In step, 6 groups of subject active compound solutions are configured, are then settled to 25mL respectively using pure water.
4. the analysis method containing impurity in a kind of pesticide flonicamid according to claim 3, it is characterised in that: match
1 group of impure reference material solution is set, adopts and weighs flonicamid impurity 19.5mg in the balance, be settled to 25mL using pure water；Match
6 groups of subject active compound solutions are set, weigh 208.7mg, 194.2mg, 194.6mg, 208.5mg, 209.6mg, 208.7mg original respectively
Then medicine is settled to 25mL respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910580373.3A CN110208424A (en) | 2019-06-28 | 2019-06-28 | Analysis method containing impurity in a kind of pesticide flonicamid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910580373.3A CN110208424A (en) | 2019-06-28 | 2019-06-28 | Analysis method containing impurity in a kind of pesticide flonicamid |
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| Publication Number | Publication Date |
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| CN110208424A true CN110208424A (en) | 2019-09-06 |
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| CN201910580373.3A Pending CN110208424A (en) | 2019-06-28 | 2019-06-28 | Analysis method containing impurity in a kind of pesticide flonicamid |
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Citations (6)
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| US20040023955A1 (en) * | 2000-07-20 | 2004-02-05 | Rodgers James D. | Tricyclic-2-pyridone compounds useful as HIV reverse transcriptase inhibitors |
| US20110263602A1 (en) * | 2008-11-17 | 2011-10-27 | Eli Lilly And Company | Tetrasubstituted pyridazine hedgehog pathway antagonists |
| CN108623518A (en) * | 2018-07-09 | 2018-10-09 | 上海凯爱网络科技有限公司 | Amides compound containing trifluoromethyl pyridine and the preparation method and application thereof |
| CN109100443A (en) * | 2018-09-30 | 2018-12-28 | 浙江省检验检疫科学技术研究院 | The method of various new nicotinoids drug and its metabolite residue amount in royal jelly is measured simultaneously |
| CN109270190A (en) * | 2018-11-13 | 2019-01-25 | 山东农业大学 | A method of 101 kinds of persticide residues in measurement fructus lycii |
| CN109632981A (en) * | 2018-11-16 | 2019-04-16 | 常州合全药业有限公司 | A kind of method of LC-MS detection 2,2,6,6- tetramethyl piperidine nitrogen oxides |
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2019
- 2019-06-28 CN CN201910580373.3A patent/CN110208424A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040023955A1 (en) * | 2000-07-20 | 2004-02-05 | Rodgers James D. | Tricyclic-2-pyridone compounds useful as HIV reverse transcriptase inhibitors |
| US20110263602A1 (en) * | 2008-11-17 | 2011-10-27 | Eli Lilly And Company | Tetrasubstituted pyridazine hedgehog pathway antagonists |
| CN108623518A (en) * | 2018-07-09 | 2018-10-09 | 上海凯爱网络科技有限公司 | Amides compound containing trifluoromethyl pyridine and the preparation method and application thereof |
| CN109100443A (en) * | 2018-09-30 | 2018-12-28 | 浙江省检验检疫科学技术研究院 | The method of various new nicotinoids drug and its metabolite residue amount in royal jelly is measured simultaneously |
| CN109270190A (en) * | 2018-11-13 | 2019-01-25 | 山东农业大学 | A method of 101 kinds of persticide residues in measurement fructus lycii |
| CN109632981A (en) * | 2018-11-16 | 2019-04-16 | 常州合全药业有限公司 | A kind of method of LC-MS detection 2,2,6,6- tetramethyl piperidine nitrogen oxides |
Non-Patent Citations (6)
| Title |
|---|
| JUNG，DI 等: "Effects of light shading and climatic conditions on the metabolic behavior of flonicamid in red bell pepper", 《ENVIRONMENTAL MONITORING AND ASSESSMENT》 * |
| XINGANG LIU 等: "Dissipation and residue of flonicamid in cucumber, apple and soil under field conditions", 《 INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY》 * |
| 刘鹏飞 等: "氟啶虫酰胺合成方法述评", 《农药》 * |
| 周芸 等: "多氨基多苯基甲烷的LC-ESI/MS分析", 《聚氨酯工业》 * |
| 左爱华 等: "洋川芎内酯A和洋川芎内酯I的降解产物研究", 《中草药》 * |
| 董新蕊 等: "直接法合成氟啶虫酰胺杂质的确定及转化工艺", 《农药》 * |
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Application publication date: 20190906 |