Abstract
Metamizole (dipyrone) is a non-addictive analgesic with antipyretic and spasmolytic action. A nitrosamine drug substance-related impurity (NDSRI) can be formed with the reaction of metamizole with nitrite. The aim of this study is the development and validation of an analytical method for the determination of N-nitroso metamizole EP impurity C in medicinal products, based on ultraperformance liquid chromatography with a triple quadrupole mass spectrometry (UPLC-MS/MS) system. The specific compound is a potential genotoxic impurity with a limit no more than 1500 ng/g in sample (quantitative) or 0.36 ng/mL in solution. The analyte separation was carried out with a Gemini C6-Phenyl 110 Å, (3.0 x 100 mm, 3 μm) analytical column in gradient elution. The proposed method was fully validated according to the International Council for Harmonization (ICH) Q2(R2) guideline “Validation of analytical procedures”. The method was specific and linear in the working range from 0.036 ng/mL (LOQ) to 0.72 ng/mL with a coefficient of determination (R2) greater than 0.99. The average recovery was 90%, the repeatability and intermediate precision expressed as RSD% ranged from 2-6% and 1-10%, respectively. Furthermore, the analytical methodology has been shown to be robust, environmentally sustainable and feasible.
Published Version
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