Confirmation and Quantification of Genotoxic Impurity 2- Dimethylaminoethyl chloride hydrochloride (DMC HCl) by GCMS in Chlorpheniramine/Chlorphenamine Maleate

Abstract

The purpose of this research work is to develop a suitable GCMS method for the quantitative determination of Genotoxic impurity 2-Dimethylaminoethyl chloride hydrochloride (DMC HCl). The compound is inorganic and it is not easy to quantify at ppm level present in Chlorpheniramine/ Chlorphenamine Maleate Active Pharmaceutical Ingredients (APIs) with any other methods. Hence the GCMS method was developed on Thermo Scientific, WAXMS, 30 m x 0.32 mm x 0.25μmcolumn using Thermo Scientific Trace 1310 and TSQ at a flow rate of 1.0 mL/min. Under these conditions impurity was quantified by selecting mass range 40 – 700 amu. The limit of detection and the limit of quantitation for the impurity were established. Validation of the developed GCMS method was carried out as per ICH requirements and the data shows that, the proposed method is specific, linear, accurate, precise and robust. This method has been tested in a number of Chlorpheniramine/ Chlorphenamine Maleate samples and used successfully for quantification of the impurity at ppm level. The developed GCMS method was found to be suitable to quantify the Genotoxic impurity 2-Dimethylaminoethyl chloride hydrochloride (DMC HCl) at ppm level present Chlorpheniramine/ Chlorphenamine Maleate.