Sivagami B

Ensitrelvir, is an oral SARS-CoV-2 3CL protease inhibitor that was approved in Japan to treat SARS-CoV-2 infections. This paper describes the AQbD approach and Box Behnken Design assisted development of a HPLC method and its validation for Ensitrelvir in bulk and dosage form. The three independent variables of the RP-HPLC method were flow rate, organic ratio in mobile phase and runtime and the responses retention time and tailing factor were taken as dependent variables. The study utilized a PLATSIL C18-EP column (4.6 x 250mm, 5µm) the chromatographic conditions were optimized using Acetonitrile: Triethylamine pH: 4 (60:40 mL) as the mobile phase, 1 mL/min as flow rate with a Rt of 9.609 min, at a λ max of 228 nm. The devised technique was found to be linear with a serial dilution of 10–50 μg/ml with (r2) of 0.991. The tailing factor (TF) and theoretical plates (N) were 1.28 and 4883 results indicated the system suitability test, respectively. The precision for Intraday and Interday were determined and % RSD was observed to be 1.6 and 0.9 %. The robustness values were below 2%. No other coeluting peaks were found with the Ensitrelvir peak, according to the chromatographic peak purity data. According to ICH specifications, the parameters for method validation were within the permissible range.

Background: A simple new novel, accurate, robust and precise RP-HPLC method was developed and validated for the simultaneous quantification of Rilpivirine and Dolutegravir in bulk and marketed tablet formulations. Methods: The method development was carried out by using INERTSIL ODS column (250×4.6mm, 5µm), by isocratic approach using a mixture of Phosphate Buffer (pH 6.8): Acetonitrile in the ratio of (35: 65) as mobile phase. The flow rate was 1.0 ml/min, 259 nm as detection wavelength. Results: The retention time of 3.285 min was observed for Dolutegravir and 4.635 min for Rilpivirine. Dolutegravir percentage purity was 99.97% and 100.63% for Rilpivirine. The system suitability parameters such as theoretical plate and tailing factor for Dolutegravir and Rilpivirine was observed in the range of 3209, 1.13 and 5210, 1.11and was found to be within the limit. The linear was observed in the concentration ranges of 50µg – 250µg for Dolutegravir and 30µg - 150µg for Rilpivirine and correlation coefficient (r2) value for Dolutegravir was 0.999 and 0.999 for Rilpivirine. The percentage RSD for repeatability was observed to be within the acceptance limit 0.1 and 0.7. The percentage RSD for intermediate precision was 0.4 and 0.8. The precision study was precise, robust, and repeatable. The LOD values were 3 and 3.02 and LOQ values were 9.98 and 10.01. Conclusion: Hence the optimized RP-HPLC method can be used for simultaneous quantification and concurrent analysis of Dolutegravir and Rilpivirine in API and combined dosage formulations.

Background: Residual solvents and organic volatile impurities are monitored using Head Space Gas Chromatography present in pharmaceutical samples. Mesalamine is a 5-aminosalicylic acid 5-ASA based agent which is used to treat adults with ulcerative colitis. Objective: In this study, an attempt was made to analyze the residual organic solvents such as isopropyl alcohol and dichloromethane present in Mesalamine Delayed-Release Tablets by headspace gas chromatography (HS-GC). Method: The carrier gas streamed was nitrogen, the method was developed and optimized by using a DB-624(60 m × 0.53 mm × 3.0 µm) column coupled with a flame ionization detector. A capillary column consisting of 6 % cyanopropylphenyl - 94 % dimethyl polysiloxane was employed as the stationary phase. An injector temperature of 200°C was programmed to prevent degradation. Results: A temperature of 40°C was set as the initial oven temperature for a period of 10 min and set at a rate of 20°C min−1 and monitored at a final temperature of 220°C for 5 min. Chloroform and N, N-dimethylacetamide was selected as the sample solvent. The validation studies were performed with regard to International Council for Harmonization (ICH) Q2 guidelines for the validation of analytical experiments. Conclusion: All the validation parameters complied with the acceptance criteria. Hence, the optimized method developed and validated can be utilized for the concurrent estimation of residual solvents in tablet formulations.

A simple, Accurate, precise and rapid method was developed for the simultaneous estimation of the Metformin and Linagliptin in Tablet dosage form. Chromatogram was run through Inertsil ODS C18 (250 x 4.6 mm, 5). Mobile phase containing Methanol, Acetonitrile and Water in the ratio of 40: 40: 20 was pumped through column at a flow rate of 1ml/min. Optimized wavelength for Metformin and Linagliptin was 258 nm. Retention time of Metformin and Linagliptin were found to be 2.764 min and 3.162 min %RSD of Metformin and Linagliptin were found to be 0.507 and 0.51 respectively. % Assay was obtained as 99.24% and 99.82% for Metformin and Linagliptin respectively. LOD, LOQ values of Metformin and Linagliptin were 0.08ppm, 0.25ppm and 0.03ppm, 0.08ppm respectively. Regression equation of Metformin was found to be y = 10831x-34273, and for Linagliptin value was found y = 21030x + 31232. Hence the developed method can be successfully employed for the routine analysis of Metformin and Linagliptin in bulk and pharmaceutical dosage forms.