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Method for analyzing content of imidacloprid synthetic intermediate through liquid chromatography-mass spectrometry

A technology of imidacloprid and combined use, applied in the field of analysis

Active Publication Date: 2019-06-21
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the use of such ion-pairing reagents and LC / MS analysis methods for the content analysis of imidacloprid synthesis intermediates

Method used

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  • Method for analyzing content of imidacloprid synthetic intermediate through liquid chromatography-mass spectrometry
  • Method for analyzing content of imidacloprid synthetic intermediate through liquid chromatography-mass spectrometry
  • Method for analyzing content of imidacloprid synthetic intermediate through liquid chromatography-mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Experimental instruments and reagents

[0022] (1) Experimental equipment: The instrument used is a Thermo Fisher ultra-high performance liquid chromatography-ion trap mass spectrometer, and the chromatographic column is an Agilent Eclipse PluC18 liquid chromatographic column (4.6×100mm, 3.5μm); a syringe-type microporous organic filter membrane (0.22μm);

[0023] (2) Experimental reagents: methanol, Watsons distilled water, ammonium acetate, perfluorovaleric acid, guanidine nitrate, nitroguanidine, imidazolidine, 2-chloro-5-chloromethylpyridine and imidacloprid standard substances;

[0024] (2) Chromatography and mass spectrometry conditions

[0025] (3) Liquid phase conditions: mobile phase A is methanol; mobile phase B is 0.02mol / L ammonium acetate aqueous solution (containing 0.04 / % perfluorovaleric acid); flow rate is 0.3mL / min, gradient elution program: 0-5min : A: 15%, the remaining components are B; 5.1-15min: A: 75%, the remaining components are B; 20.1-2...

Embodiment 2

[0034] (1) Experimental instruments and reagents

[0035](1) Experimental equipment: The instrument used is a Thermo Fisher ultra-high performance liquid chromatography-ion trap mass spectrometer, and the chromatographic column is an Agilent Eclipse PluC18 liquid chromatographic column (4.6×100mm, 3.5μm); a syringe-type microporous organic filter membrane (0.22μm);

[0036] (2) Experimental reagents: methanol, Watsons distilled water, ammonium acetate, perfluoroheptanoic acid, guanidine nitrate, nitroguanidine, imidazolidine, 2-chloro-5-chloromethylpyridine and imidacloprid standard substances;

[0037] (2) Chromatography and mass spectrometry conditions

[0038] (3) Liquid phase conditions: mobile phase A is methanol; mobile phase B is 0.01mol / L ammonium acetate aqueous solution (containing 0.06 / % perfluoroheptanoic acid); flow rate is 0.5mL / min, gradient elution program: 0-5min : A: 10%, the remaining components are B; 5.1-15min: A: 80%, the remaining components are B; 20....

Embodiment 3

[0048] (1) Experimental instruments and reagents

[0049] (1) Experimental equipment: The instrument used is a Thermo Fisher ultra-high performance liquid chromatography-ion trap mass spectrometer, and the chromatographic column is an Agilent Eclipse PluC18 liquid chromatographic column (4.6×100mm, 3.5μm); a syringe-type microporous organic filter membrane (0.22μm);

[0050] (2) Experimental reagents: methanol, Watsons distilled water, ammonium acetate, perfluorooctanoic acid, guanidine nitrate, nitroguanidine, imidazolidine, 2-chloro-5-chloromethylpyridine and imidacloprid standard

[0051] (2) Chromatography and mass spectrometry conditions

[0052] (3) Liquid phase conditions: mobile phase A is methanol; mobile phase B is 0.015mol / L ammonium acetate aqueous solution (containing 0.1 / % perfluorooctanoic acid); flow rate is 0.3mL / min, gradient elution program: 0-5min: A: 25%, the remaining components are B; 5.1-15min: A: 70%, the remaining components are B; 20.1-25min: A: 25...

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Abstract

The invention relates to the analysis technology field and especially relates to a method for analyzing a content of an imidacloprid synthetic intermediate through liquid chromatography-mass spectrometry. In the invention, a perfluorinated organic acid is taken as an ion-pairing agent. Under an ion-pairing chromatography condition, all the above intermediates can reach baseline separation and realize quantitative detection. Simultaneously, the ion-pairing agent is compatible with a mass spectrometry system and can be used for completing efficient separation and qualitative and quantitative detection in a liquid chromatography-mass spectrometry (LC / MS) system.

Description

technical field [0001] The invention relates to the technical field of analysis, in particular to a method for analyzing the content of imidacloprid synthesis intermediates by liquid chromatography-mass spectrometry. Background technique [0002] Imidacloprid is a new type of ultra-efficient systemic broad-spectrum neonicotinoid insecticide, which has the characteristics of high efficiency, high selectivity, low toxicity and low pollution, and has broad application prospects in the field of sanitary pest control. The molecular formula of imidacloprid is C 9 h 10 ClN 5 o 2 , the chemical name is 1-(6-chloro-3-pyridylmethyl)-N-nitroimidazole-2-imine, and the structural formula is: [0003] [0004] Imidacloprid is produced by the condensation reaction of imidazolidine and 2-chloro-5-chloromethylpyridine, and impurities in imidazolidine, 2-chloro-5-chloromethylpyridine and imidazolidine may exist or remain in the reaction liquid and finished products. guanidine and guan...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 陶文波孟颖王彬丁克鸿徐林王根林李杰赵洁徐业庆
Owner JIANGSU YANGNONG CHEM GROUP
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