SYNTHESIS, CHARACTERIZATION AND QUANTITATION OF REGIOISOMERIC IMPURITY IN NIMODIPINE BULK AND FORMULATION

Objective: The present research work was directed towards the synthesis characterization and quantitation of regioisomeric impurity of Nimodipine i.e. diethyl 1, 4-dihydro-2,6-dimethyl pyridine dicarboxylate in bulk and tablet formulation, by UV,IR,NMR and GC-MS techniques and a RP-HPLC method was developed as per ICH Q2B guidelines for quantitation of 1, 4-Dihydro-2, 6-Dimethyl-4-(p-nitro phenyl) pyridine-3,5 dicarboxylate (NI) from bulk and formulation. Methods: The synthesis of NI was carried out by Hantzch pyridine synthesis, by using p-nitrobenzaldehyde, ethylacetoacetate, in presence of ammonia and methanol as a catalyst. The percentage yield was found to be 89.29%. Recrystallization and purification of NI was done. The preliminary evaluation was done on laboratory scale via melting point, elemental analysis and TLC. Results: The melting point of impurity was found to be 156-1580C. The TLC of impurity was carried by using Chloroform: Methanol (9:1) and the Rf was found to be 0.79. The confirmation of structure of NI was carried out by using sophisticated techniques i.e., FT-IR, NMR (13C and 1H), GC-MS etc. The RP-HPLC method was developed to quantify the NI in Nimodipine bulk and formulation as per ICH Q2B guidelines. The method validation was done as per ICH guidelines. Conclusion: The validated optimized method was found to be linear, précised, robust, rugged and accurate. Finally NI was quantified from bulk Nimodipine and its marketed tablet formulation. It was concluded that the amount of NI, present in tablet was found to be 0.1% and in the bulk 0.067% respectively. Thus it was revealed that the NI was found to be within the limit laid down ICH guidelines (Not more than 0.1 %)

Review On Method Development And Validation

High performance liquid chromatography is most accurate methods widely used for the qualitative and quantitative analysis of drug product. Analytical method development and validation play important roles in the Drug discovery, Drug development and Manufacture of pharmaceuticals. It involves detection of the purity and toxicity of a drug substance. A number of chromatographic parameters have been evaluated in order to optimize the methods in the analysis of method development in HPLC. An appropr- iate mobile phase, column, column tempe- rature, wavelength and gradient are develop- ped. Force degradation studies are helpful in development and validation of stability-indicating studies, determination of degrad- ation pathways of drug substances and drug products. Validation of an analytical procedure is to demonstrate that it is suitable for its intended purpose. The parameters described here are according to ICH guidelines and include accuracy, precision, specificity, limit of detection, limit of quantitation, linearity, range, ruggedness and robustness. The objective of this paper is to review the method development, optimize method parameters and validation of method for drug product from developm- ental stage of formulation to commercial batch of product

Advances of MXene heterostructure composites in the area of sensing and biomedical applications: an overview

Among various two-dimensional materials, MXenes have emerged as versatile materials that incorporate transition metal carbide, nitride, and carbonitrides. MXenes are gaining paramount attraction among the scientific community in areas of catalyst, energy, electromagnetic shielding, and sensors due to their outstanding mechanical, electrical, sensing, optical, and tunable characteristics. The unique properties such as surface chemistry, graphene-like morphology, metal-like conductivity, and high hydrophilicity ameliorate MXene as an ideal 2D material for surface-related applications. This review focuses on the most recent reports on the surface modifications/surface chemistry and electrochemical sensing of different analytes using MXenes for biomedical applications, biomolecule detection, and environmental monitoring. The present review concisely summarizes different characterization techniques, such as X-ray diffraction methods and electron microscopy, for evaluating MXene characteristics. Apart from titanium carbide MXene, other MXene needs a careful investigation to accentuate the future perspectives of MXenes in sensor devices. This comprehensive review paper aims to inspire the scientific community that is intrigued by the potential properties, benefits, prospects, and difficulties of utilizing 2D materials in various biosensing and biomedical applications