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Detection method of 4-chlorobutyric acid

A detection method and chlorobutyric acid technology, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as the inability to achieve the limit control of 4-chlorobutyric acid, and the lack of maturity, reliability and stability of 4-chlorobutyric acid.

Pending Publication Date: 2021-06-22
NKD PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no mature, reliable and stable method for the detection of 4-chlorobutyric acid, and it is impossible to achieve the limit control of 4-chlorobutyric acid residues in raw materials and formulate corresponding quality testing standards

Method used

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  • Detection method of 4-chlorobutyric acid
  • Detection method of 4-chlorobutyric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Taking the detection of 4-chlorobutyric acid derived from methanol as an example, a specific experiment was carried out.

[0060] (1) 4-Chlorobutyric acid derivatization conditions and preliminary detection instrument conditions

[0061] Solvent: Methanol

[0062] 4-Chlorobutyric acid stock solution: Take about 24mg of 4-chlorobutyric acid, weigh it accurately, put it in a 100ml measuring bottle, add methanol to dissolve and dilute to the mark, shake well to get 0.24mg / ml stock solution.

[0063] 6μg / ml 4-chlorobutyric acid solution: Accurately measure 5ml of 0.24mg / ml 4-chlorobutyric acid stock solution, put it in a 200ml measuring bottle, dilute with methanol to the mark, and shake well. Take 5ml and place it in a 20ml headspace bottle, add 50μl sulfuric acid dropwise, seal the cap, and inject the sample for analysis.

[0064] The detection method is as follows: arrange methanol and 6 μg / ml 4-chlorobutyric acid solution in the sample tray in turn, refer to the instr...

Embodiment 2

[0071] Example 2 Determination of 4-chlorobutyric acid derivative detection instrument conditions and methodological verification

[0072] On the basis of Example 1, the quantitative ion is determined to be 74, and the adjusted instrument parameters are as follows in Table 2:

[0073] Table 2 4-Chlorobutyric acid detection instrument parameter settings

[0074]

[0075]

[0076] Linear solution preparation: Take 3ml, 1.0ml, 0.5ml, and 0.1ml of 4-chlorobutyric acid stock solution with a concentration of 6μg / ml in sequence, place them in 10ml volumetric flasks, dilute to the mark with methanol, and shake well to obtain a linear standard curve with solution. Accurately measure 5ml of the solution for each linear standard curve, put it in a 20ml headspace bottle, add 50μl of sulfuric acid dropwise, seal the cap, inject the sample for analysis, record the chromatogram and peak area, take the concentration as the abscissa, and the peak area as the ordinate , draw a graph to ...

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Abstract

The invention relates to a detection method of 4-chlorobutyric acid, in particular to a detection method of a 4-chlorobutyric acid substance in bulk drugs. A gas chromatography-mass spectrometry method is adopted for detection, and the method comprises the following steps: deriving 4-chlorobutyric acid in a sample to be detected into 4-chlorobutyrate, wherein the conditions of the gas chromatography detection are as follows: a 5% phenyl-95%-dimethyl polysiloxane copolymer stationary liquid chromatographic column is selected as a chromatographic column. The detection method of 4-chlorobutyric acid provided by the invention is simple, stable and reliable, and can be used for detecting 4-chlorobutyric acid residues in bulk drugs.

Description

technical field [0001] The invention relates to a detection method for 4-chlorobutyric acid, in particular to a detection method for 4-chlorobutyric acid in raw materials. Background technique [0002] 4-Chlorobutyric acid is a colorless transparent liquid, and it is one of the most commonly used pharmaceutical intermediates in the synthesis of raw materials. In recent years, the requirements for research on genotoxic impurities in raw materials have been improved, making substances such as 4-chlorobutyric acid identified as genotoxic impurities, which have become necessary research contents in the detection of raw materials. Genotoxic impurities originate from the starting materials, intermediates, reagents, and reaction by-products during the synthesis of APIs, and may also be produced by the degradation of drugs during synthesis, storage, or preparation. Its characteristic is that it can cause damage to the genetic material of the human body at a low concentration, which...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/04G01N30/72G01N30/06G01N30/30G01N30/86G01N30/88
CPCG01N30/02G01N30/04G01N30/72G01N30/06G01N30/30G01N30/8634G01N30/88G01N2030/047G01N2030/067G01N2030/884
Inventor 温永青韩建平贺永桓
Owner NKD PHARMA CO LTD
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