SYNTHESIS, CHARECTERIZATION, DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR PROCESS RELATED IMPURITY IN NIMODIPINE BULK AND FORMULATION

LUBNA SHAIKH; VISHAL PANDE; DEEPAK MUSMADE

Authors

LUBNA SHAIKH Research Scholar, Department of Quality Assurance Techniques
VISHAL PANDE Associate Professor and Head, Department of Pharmaceutics and Quality Assurance Techniques
DEEPAK MUSMADE Assistant Professor, Department of Pharmaceutical Chemistry, Sanjivani College of Pharmaceutical Education and Research, Kopargaon, Ahmednagar, Maharashtra, India.

Keywords:

Impurity, IR, NMR, GC-MS, RP-HPLC, Validation

Abstract

The synthesis, characterization and quantitation of process related impurity in Nimodipine i.e.Diethyl 2, 6-dimethyl-4-(2-
nitrophenyl)-1, 4-dihydropyridine-3, 5-dicarboxylate bulk and tablet formulation was performed by using Hantzch pyridine
synthesis. This synthesis includes o-nitrobenzaldehyde, ethylacetoacetate in presence of ammonia and methanol as catalyst.
The percentage yield was found to be 79%. The impurity was recrystallized and preliminary evaluation was done on lab
scale viz. Melting point, TLC and elemental analysis. The melting point of impurity was found to be 156-1580C. The TLC
of impurity was carried out by using benzene and methanol (6:1) and the Rf was found to be 0.78 the conformation of
synthesized Nimodipine impurity was carried out by using sophisticated instrument such as, FT-IR, NMR, GC-MS, and RPHPLC
method was developed to identify and quantify the Nimodipine impurity in bulk and formulation as per ICH Q2B
guidelines. The method was found to be linear, precise, accurate, robust and rugged. Finally 1, 4-Dihydro-2, 6- Dimethyl-4-
(o-nitrophenyl) pyridine-3, 5 dicarboxylate(Nimodipine Impurity) was quantified from bulk Nimodipine and its marketed
tablet formulation. It was concluded that the amount of Nimodipine impurity, present in tablet was found to be 0.0876%and
in bulk 0.0219% respectively.