Method for analyzing and determining relevant substances in pyrazinamide by employing liquid chromatography

Abstract

The invention discloses a method for analyzing and determining relevant substances in pyrazinamide by employing a liquid chromatography. The method comprises the following steps of (1) preparing a contrast solution; (2) preparing a system applicability solution; (3) preparing a test solution; (4) preparing a self-control solution; and (5) carrying out chromatographic analysis and determination, namely injecting taken diluent and prepared contrast solution, system applicability solution, test solution and appropriate self-control solution into a liquid chromatograph, recording a liquid chromatogram, and analyzing and determining the content of pyrazinoic acid, the content of 2-cyanopyrazine, the content of an unknown single impurity and the content of total impurities according to the liquid chromatogram. The method is higher in specificity and pertinence, and the 2-cyanopyrazine and the pyrazinoic acid existing in the pyrazinamide can be quantitatively tested accurately, thereby more effectively controlling the product quality and providing a certain basis for the study of the relevant substances.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for analyzing and determining related substances in pyrazinamide by liquid chromatography. Background technique [0002] Pyrazinamide has a good antibacterial effect on Mycobacterium tuberculosis, and patients are less likely to develop drug resistance to pyrazinamide. Pyrazinamide has the strongest bactericidal effect at pH 5-5.5, and it can be used in combination with streptomycin, ethambutol, isoniazid and rifampicin to treat tuberculosis. At present, pyrazinamide has been recommended by the WHO as an anti-tuberculosis essential drug, and has long been included in the national essential drug. At present, the preparation process of pyrazinamide mainly uses 2-cyanopyrazine as the starting raw material, which is hydrolyzed under alkaline conditions to obtain pyrazinamide; and pyrazinamide is easily hydrolyzed into pyrazinic acid. Therefore, pyrazinamide mainly con...

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Problems solved by technology

[0003] At present, although the detection method of pyrazinamide-related substances has relevant literature records, the detection method is relatively simple and has a wide limit. It can only control the total impurities to ≤0.2%, and cannot detect the specific impurity 2-cyano Quantitative detection of base pyrazine and pyrazinic acid, so there are hidden dangers in product quality control

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