Development and Validation of HPLC Method for Quantification of Parecoxib in Parecoxib Injection

The purpose of the present study was to evaluate and optimize lyophilization cycle time for the manufacturing of Parecoxib Injection than reported longer lyophilization cycle times. Optimization of lyophilization cycle time reduces the manufacturing costs since lyophilization process involves longer times which incurs cost to the finished product. Optimization of lyophilization cycle was done by using inputs from the results of Differential Scanning Calorimetry (DSC), Differential Thermal Analysis (DTA) and Impedance analysis. HPLC method was developed for quantification of Parecoxib Active Pharmaceutical Ingredient and Related Substances. Various stages involved in lyophilization cycle viz., freezing, extra-freezing, primary drying and secondary drying were evaluated and optimized. Results of drug excipient compatibility studies indicated no significant interaction between the drug and excipients. Optimization of developed lyophilization cycle resulted in reduced total lyophilization cycle time (29 hrs, 15 mins). Finished drug products were investigated by Powder X-ray Diffraction (PXRD) for evaluating complete conversion of crystalline API into amorphous solid and by Raman Spectroscopy to evaluate absence of hydrolytic conversion of Parecoxib to Valdecoxib. Reconstituted solutions are stable for 24 hrs. Residual moisture content was below 3.5%m/m. Results of chemical analysis are satisfactory. Optimized lyophilization cycle with reduced total lyophilization cycle time reduces the operational costs as well as improves productivity, and so can help manufacturers to sell the drug product at lower price which can be affordable to the common needy people.