High performance liquid chromatography was applied to the simultaneous determination of naloxone and oxycodone. The method depends on separation and analysis of naloxone and oxycodone using C18 analytical column (250 × 4.6 mm, 5 µm). The mobile phase consists of a mixture of potassium dihydrogen phosphate (pH 5.5; 0.1 M) and acetonitrile (70:30, v/v). The photodiode array detector was set at 210 nm. The retention times of naloxone and oxycodone were 2.893 and 4.946 min, respectively. The total run time was 6 min. The developed method was validated as per the guidelines of International Conference on Harmonization and successfully applied to the simultaneous determination of naloxone and oxycodone in their tablets. All the results of validation parameters were acceptable and confirmed that the method is appropriate for the estimation of naloxone and oxycodone simultaneously.
Background and Aim: Process impurities may adversely affect the efficacy, excellent quality, and safety of pharmaceutical drugs. Ultimately, the purpose of this research work was to develop and validate a LC-MS/MS-based method for determining the Vinamidinium hexafluorophosphate impurity (VHP) in Etoricoxib in a simple, specific, accurate, and precise manner. Materials and Methods: To elute the Vinamidinium hexafluorophosphate impurity in Etoricoxib at a flow rate of 0.5mL/min within 20.0 min of runtime, a Symmetry Shield RP18, 5µm column with a 150 x 3.9 mm internal diameter was utilized in binary gradient mode. The buffer solution, which contained formic acid (0.1%) and acetonitrile (100%), as well as a diluent solution of acetonitrile (50%) and water (50%), was used to achieve the chromatographic separation. A triple quadrupole mass spectrometer (Shimadzu LC/MS/MS 8040) in Multiple Reaction Monitoring (MRM) mode was needed to monitor the results. Results and Discussion: The method's linearity was evaluated at levels from 25% to 150%, and the R 2 value was discovered to be 0.99. Sensitivity values of 0.04µg/g (LOD) and 0.13µg/g (LOQ) were established. The recovery of impurity levels of Vinamidinium hexafluorophosphate ranges from 70.0% to 130%. Linearity, specificity, accuracy, LOD, LOQ, and precision of the method were all validated. Within the assay variability limitations, it was found that the intra-and inter-day precision values were 0.67%, and 0.58%, respectively. Conclusion: According to ICH and FDA specifications, the optimized method was validated. The developed method was found to be appropriate for quantifying Vinamidinium hexafluorophosphate in Etoricoxib by employing LC-MS.
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