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Method for performing headspace gas chromatographic detection on formic acid in aceclofenac bulk pharmaceutical chemicals

A headspace gas chromatography and aceclofenac technology, applied in the field of formic acid headspace gas chromatography detection, can solve problems such as human body and environmental hazards

Inactive Publication Date: 2013-01-30
JIANGSU JIBEIER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the level of residual solvent contained in the medicine is higher than the safe value, it will cause harm to the human body and the environment

Method used

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  • Method for performing headspace gas chromatographic detection on formic acid in aceclofenac bulk pharmaceutical chemicals
  • Method for performing headspace gas chromatographic detection on formic acid in aceclofenac bulk pharmaceutical chemicals
  • Method for performing headspace gas chromatographic detection on formic acid in aceclofenac bulk pharmaceutical chemicals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Get about 0.15g of aceclofenac crude drug, accurately weighed, add 10% (v / v) sulfuric acid-methanol solution 1ml, put into 40 ℃ water bath, after reacting for 20min, it will be used as the test solution; About 0.1mg, accurately weighed, add 1ml of 10% (v / v) sulfuric acid-methanol solution, put it in a water bath at 40°C, and react for 20min, then use it as the reference solution. The test solution and the reference solution were analyzed by headspace injection respectively, the chromatograms were recorded, and the content of formic acid in the test was calculated by the external standard method.

Embodiment 2

[0024] Take about 0.15g of aceclofenac raw material, weigh it accurately, add 0.5ml of anhydrous methanol to disperse and dissolve, then add 0.5ml of 20% (v / v) sulfuric acid-methanol solution, put it in a water bath at 40°C, and react for 20min , that is, as the test solution; take about 0.1mg of formic acid, accurately weighed, add 0.5ml of anhydrous methanol to disperse and dissolve, then add 0.5ml of 20% (v / v) sulfuric acid-methanol solution, and put it in a 40°C water bath , After 20min of reaction, it was used as the reference solution. The test solution and the reference solution were analyzed by headspace injection respectively, the chromatograms were recorded, and the content of formic acid in the test was calculated by the external standard method.

[0025] The chromatographic conditions of gas chromatography are:

[0026] Chromatographic column: HP-FFAP capillary column (50m×0.32mm×0.5μm); column temperature: 40°C; carrier gas: nitrogen; flow rate: 3ml / min; inlet te...

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Abstract

The invention discloses a method for performing headspace gas chromatographic detection on formic acid in aceclofenac bulk pharmaceutical chemicals. The analysis method comprises the following steps of: (1) performing an esterification reaction on the aceclofenac bulk pharmaceutical chemicals and superfluous methanol solution comprising 5-20 percent of strong acid by volume, or adding methanol first into the aceclofenac bulk pharmaceutical chemicals and then adding strong acid, wherein the strong acid accounts for 5-20 percent of the volume of the mixed strong acid-methanol solution; and (2) after the reaction is finished thoroughly, determining the obtained product which is generated when the formic acid is esterified by using the methanol. According to the method, after the formic acid is esterified by using the methanol, the product is subjected to gas chromatographic detection by using a headspace sampling method, so that a chromatographic response value and the analysis accuracy are greatly improved.

Description

Technical field: [0001] The invention relates to a headspace gas chromatographic detection method for organic acids in aceclofenac bulk medicine, in particular to a headspace gas chromatographic detection method for formic acid. Background technique: [0002] Aceclofenac (aceclofenac), chemical name is 2-(2,6-dichloroanilino) phenylacetoxyacetic acid, CAS registration number is 89796-99-6, developed by Spanish Almirall-Prodesfarma pharmaceutical company, 1992 It was listed for the first time in Spain in 1998, and it was included in the European and British Pharmacopoeia in 1998. The chemical structural formula is as follows: [0003] Molecular formula: C 16 h 13 C 12 NO 4 , 354.2 [0004] Aceclofenac is a powerful oral non-steroidal anti-inflammatory drug, suitable for the treatment of various rheumatoid arthritis, rheumatoid arthritis, and pain and fever caused by various diseases. Safe and reliable medicine for inflammation. [0005] Residual solvents in drugs re...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 李海岛陈进刘云峰王慧吴修艮
Owner JIANGSU JIBEIER PHARMA
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