Synthesis and Quantitation of Process-Related Impurity in Felodipine Bulk and Formulation

This research is directed towards Synthesis and quantitation of process-related impurity in Felodipine bulk and formulation. The synthesis of 1,4-Dihydro-2,6-Dimethyl-4-(m- chloro phenyl) pyridine-3,5 Dicarboxylate was identified, characterized, developed and validate by using various analytical techniques such as UV, IR, NMR  for the assessment of impurities in the bulk and formulation in Felodipine. The synthesis of of 1,4-Dihydro-2,6-Dimethyl-4-(m- chloro phenyl) pyridine-3,5 Dicarboxylate was performed by Hantzch pyridine synthesis, by using m-chlorobenzaldehyde, ethylacetoacetate, in presence of ammonia and methanol as a catalyst. The percentage yield was observed to be 80.29%. The preliminary evaluation was performed via melting point, elemental analysis and thin layer chromatography (TLC). Melting point of obtained synthesised compound was noticed to be 134-1370C, whereas Rate of flow ( Rf) value was estimated and found to be 0.70. The TLC of impurity was performed by using Benzene and Methanol (6:1). The structure confirmation of obtained synthesized impurity by using sophisticated analytical instrument viz, Fourier transform infra red( FT-IR), nuclear magnetic resonance (NMR) and ultra violet (UV) spectroscopy. The method was validated as per ICH guidelines and was found to be linear, precise, robust, accurate, rugged.