ISSN : 2663-2187

A Novel Derivatised Method For The Determination Of Residual Ethylenediamine Content By Using Gc-Fid

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K. Srivalli, N. Annapurna, CH. Ramdas
» doi: 10.48047/AFJBS.6.10.2024.5896-5906

Abstract

The aim of the research work is to develop and validate a sensitive GC-FID (Gas Chromatography-Flame ionization Detector) method for the quantification of residual Ethylenediamine (Quantified as N,N’-Ditrifluoroacetyl-1,2-Ethandimine) in SOT-II (4-(4-aminophenoxy)-N-methyl-pyridine-2-carboxamide), which is the one of the intermediate of Sorafenib tosylate drug substance to fulfill the current regulatory requirements. A novel derivatised method was developed and validated according to ICH guidelines. Using a fused silica capillary column Rtx-35, 30m length, 0.53mm internal diameter, coated with 35% diphenyl and 65% dimethyl polysiloxane stationary phase of 1.0μm film thickness and Helium gas used as carrier gas. Chromatographic parameters i.e. Column flow rate: 5.0 ml/min, Injection volume: 2.0μL, Split ratio: 5:1 and Run time: 40 min. The method was calibrated with a linearity range from LOQ to 150% concentration with respect to the specification level and achieved a limit of detection (LOD) and limit of quantification (LOQ) were 11.5 ppm and 3.8 ppm, respectively, for Ethylenediamine with a correlation coefficient of 0.9992. The average recovery was found to be 100.0%. The method validation parameters strongly support and it was discovered to be specific, accurate, linear, sensitive, robust, and stable. This method is suitable for the detetermination of Ethylenediamine in the regular analysis of SOT-II intermediate

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