ASSAY METHOD DEVELOPMENT AND VALIDATION OF CILNIDIPINE AND RAMIPRIL, CHARACTERIZATION OF ITS DEGRADANTS BY USING LC-MS/MS
Keywords:Cilnidipine, Ramipril, Development, Validation, RP-HPLC
Objective: The current study focused on the development, validation of Ramipril and Cilnidipine using HPLC and characterization of forced degradation products using LC-MS/MS.
Methods: Simple, accurate, and precise method has been developed for the simultaneous estimation of Cilnidipine and Ramipril in tablet type of dosage form using X-bridge phenyl column (150x4.6mm, 3.5m) with mobile phase of buffer and Acetonitrile in the 30:70 v/v ratio was pumped through a column with a 1 ml/min flow rate. The buffer used in this process was 0.1 percent tri ethyl amine in 1 lt of water and adjust its pH-2.5 with 0.1 percent ortho phosphoric acid. At ambient temperature, chromatography was isocratically performed and run time was 8 min. 240 nm was the optimized wave length.
Results: Cilnidipine and Ramipril retention times were 2.79 min, 5.11 min. respectively. By injecting the norm six times, device parameters of suitability have been studied and the results were found to be well under the acceptance criteria. This approach offers strong linearity over a range of 2-30 µg/ml Cilnidipine 1-15 µg/ml Ramipril concentrations. The regression coefficient R2 > 0.999 from the calibrated curve implies that the linearity of the system was within the range.
Conclusion: The system was validated by using HPLC in terms of accuracy, linearity, method precision, accuracy, limit of detection, limit of quantification, robustness, degradation and the degradation products were characterized by using LC-MS/MS.
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