Method for detecting valsartan and content of N-nitrosodimethylamine in preparation thereof

Abstract

The invention belongs to the field of analytical chemistry detection, and relates to a method for detecting valsartan and content of N-nitrosodimethylamine in the preparation thereof. The detecting method comprises the steps of: grinding an object under test and weighing fine powder; adding a polar organic solvent in the powder and filtering by a filter membrane to prepare a solution under test; preparing a standard curve solution; acquiring a standard chromatogram map and a regression equation; detecting the solution under test by a gas chromatography-thermal energy analyzer to acquire a chromatogram map of the solution under test; if a chromatographic peak corresponding to the chromatographic peak in a standard curve chromatogram map exists in the chromatogram map of the solution under test, showing that the solution under test contains the N-nitrosodimethylamine; and calculating to acquire the concentration of the N-nitrosodimethylamine according to the area of the chromatographic peak in the chromatogram map of the solution under test. The principle of the method is reliable; the experimental operation is simple; the measuring precision and accuracy are ensured by using the high-separation efficiency of the capillary gas chromatography and the high-selectivity and the high-sensitivity of the thermal energy analyzer; and thus, the analysis time and test cost are greatly saved.

Description

technical field [0001] The invention belongs to the field of analytical chemistry detection, and relates to a method for detecting the content of N-dimethylnitrosamine in valsartan and its preparations. Background technique [0002] N-nitrosodimethylamine (NDMA), also known as N-nitrosodimethylamine, has strong liver toxicity, and the World Health Organization classifies it as a 2A carcinogen. Recently, an excessive amount of NDMA was detected in valsartan, a mainstream antihypertensive drug in the global market, which seriously threatened the life and health of patients, and led to the emergency recall of valsartan raw materials and preparations in more than 20 countries and regions around the world, which has become a global concern. Valsartan incident". There is no applicable N-dimethylnitrosamine detection method in the drug quality standards, and the inability to effectively monitor product quality is one of the main reasons for this incident. [0003] At present, the...

AI Technical Summary

Problems solved by technology

The pretreatment methods in the current NDMA determination methods reported in the literature generally require steps such as distillation extraction, extraction purification, evaporation concentration, etc. The operation is cumbersome and the sensitivity is low, which cannot meet the requirements of NDMA limit inspection in drugs.

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