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Method for detecting content of 2-chloronicotinamide by using ultra performance liquid chromatography

A technology of ultra-high performance liquid phase and chloronicotinamide, which is applied in the field of chemical analysis to achieve the effects of short retention time, simple method and high sensitivity

Active Publication Date: 2018-05-15
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, high-performance liquid chromatography is used more and more in the detection of drugs and their intermediates. Nicosulfuron technical mostly uses high-performance liquid chromatography for quantitative analysis, but the quantitative analysis of its intermediate 2-chloronicotinamide There are few reports on the method, but in the actual production process, the monitoring of the nicosulfuron intermediate 2-chloronicotinamide has important guiding significance

Method used

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  • Method for detecting content of 2-chloronicotinamide by using ultra performance liquid chromatography
  • Method for detecting content of 2-chloronicotinamide by using ultra performance liquid chromatography
  • Method for detecting content of 2-chloronicotinamide by using ultra performance liquid chromatography

Examples

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Effect test

Embodiment 1

[0037] There is a batch of 2-chloronicotinamide samples with unknown concentration, the content is about 95%, and it needs to be determined. Ultra-high performance liquid chromatography is used for detection and external standard method for quantitative analysis. The specific steps include:

[0038] (1) Preparation of 2-chloronicotinamide standard solution: Accurately weigh 15mg, 25mg, 35mg, 45mg, 55mg (accurate to 0.0002g) of 2-chloronicotinamide standard samples in a 100mL volumetric flask, and ultrasonically Dissolve for 10 minutes, and after cooling to room temperature, set the volume to the mark to obtain standard solutions I, II, III, IV, and V, whose concentrations are 150.0mg / L, 250.0mg / L, 350.0mg / L, and 450.0mg / L, respectively , 550.0mg / L;

[0039] (2) Preparation of 2-chloronicotinamide sample solution: Accurately weigh 3 parts of 2-chloronicotinamide sample 35mg (accurate to 0.0002g) into three 100mL volumetric flasks, ultrasonically dissolve with methanol-water mix...

Embodiment 2

[0042] There is a batch of 2-chloronicotinamide samples with unknown concentration, the content is about 95%, and it needs to be determined. Ultra-high performance liquid chromatography is used for detection and external standard method for quantitative analysis. The specific steps include:

[0043] (1) Preparation of 2-chloronicotinamide standard solution: Accurately weigh 15mg, 25mg, 35mg, 45mg, 55mg (accurate to 0.0002g) of 2-chloronicotinamide standard samples in a 100mL volumetric flask, and ultrasonically Dissolve for 10 minutes, and after cooling to room temperature, set the volume to the mark to obtain standard solutions I, II, III, IV, and V, whose concentrations are 150.0mg / L, 250.0mg / L, 350.0mg / L, and 450.0mg / L, respectively , 550.0mg / L;

[0044] (2) Preparation of 2-chloronicotinamide sample solution: Accurately weigh 3 parts of 2-chloronicotinamide sample 35mg (accurate to 0.0002g) into three 100mL volumetric flasks, ultrasonically dissolve with methanol-water mix...

Embodiment 3

[0047] There is a batch of 2-chloronicotinamide samples with unknown concentration, the content is about 95%, and it needs to be determined. Ultra-high performance liquid chromatography is used for detection and external standard method for quantitative analysis. The specific steps include:

[0048] (1) Preparation of 2-chloronicotinamide standard solution: Accurately weigh 15mg, 25mg, 35mg, 45mg, 55mg (accurate to 0.0002g) of 2-chloronicotinamide standard samples in a 100mL volumetric flask, and ultrasonically Dissolve for 10 minutes, and after cooling to room temperature, set the volume to the mark to obtain standard solutions I, II, III, IV, and V, whose concentrations are 150.0mg / L, 250.0mg / L, 350.0mg / L, and 450.0mg / L, respectively , 550.0mg / L;

[0049] (2) Preparation of 2-chloronicotinamide sample solution: Accurately weigh 3 parts of 2-chloronicotinamide sample 35mg (accurate to 0.0002g) into three 100mL volumetric flasks, ultrasonically dissolve with methanol-water mix...

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Abstract

The invention relates to the field of chemical analysis detection, and more specifically relates to a method for detecting content of 2-chloronicotinamide by using ultra performance liquid chromatography. An ultra performance liquid chromatograph and a UV-visible absorbance detector are used, a C18 chromatographic column of small particle size is used as a separation column, methanol and water areused as mobile phases, 2-chloronicotinamide is used as a standard sample, an external standard method is used for drafting a 2-chloronicotinamide concentration-peak area standard curve, in order to obtain an equation of linear regression; the content of 2-chloronicotinamide is obtained by calculation with the equation of linear regression. The method can be used for realizing effective separatingdetection of the nicosulfuron intermediate 2-chloronicotinamide with extremely short analysis time, simple and easy method, and convenience and reliability.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for determining the content of 2-chloronicotinamide by using ultra-high performance liquid chromatography. Background technique [0002] Nicosulfuron is a sulfonylurea herbicide in corn field, which has the advantages of good environmental compatibility, high efficiency and low toxicity. Its chemical name is 1-(4,6-dimethoxypyrimidin-2-yl )-3-(3-Dimethylaminomethylsulfonylpyridin-2-ylsulfonyl)urea. 2-Chloronicotinamide is an important intermediate in the synthesis process of nicosulfuron. It is very important to select the best detection method to quickly analyze its accurate content for the continuous production. [0003] At present, high-performance liquid chromatography is used more and more in the detection of drugs and their intermediates. Nicosulfuron technical mostly uses high-performance liquid chromatography for quantitative analysis, but the quantita...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 崔丽华马韵升王岳华吕印美刘清钊付鹿韩立霞董昭苹邢丽莉宋玉振
Owner CHAMBROAD CHEM IND RES INST CO LTD