Sirajunisa Talath

The aim of the research study was the development and validation of a simple, rapid, accurate and precise reversed-phase high performance liquid chromatography (RP-HPLC) stability-indicating method for the determination of aceclofenac in bulk and pharmaceutical dosage forms. The RP-HPLC studies was performed on the instrument Jasco HPLC system with Jasco UV 2010 photo diode array detector, ODS C18 RP-column (Intersile 250 mm × 4.6 mm; i.d. 10 μm), Rheodyne injection syringe with 20µL loop volume and windows based chrompass software was used for separation. The isocratic elution was performed using the mobile phase ratio of methanol: water (65:35 v/v) and UV detection wavelength at 263 nm. The overall run time of the analysis was 20 minutes and the flow rate was 1.0 mL/min. The RP-HPLC method developed for analysis of aceclofenac was validated as per the ICH guidelines with respect to specificity, selectivity, linearity, accuracy, precision and robustness. The linearity for developed method was observed in the concentration range of 5-50 μg/mL with the correlation coefficient (r2) of 0.9992. The percentage accuracy of aceclofenac ranged from 99.40 to 100.79%. The relative standard deviation for inter-day precision was lower than 2.0%. The assay of aceclofenac was determined in tablet dosage form was found to be within limits. Aceclofenac was subjected to stress conditions such as neutral, acidic, alkaline, oxidation, and photolysis degradations as per ICH guidelines. The results of degradation studies revealed that the drug degraded a maximum (32.68%) in acidic conditions followed by alkaline conditions (15.05%). The drug was found to be resistant towards neutral, acidic and photolytic degradation conditions.

The objective of this work was to develop a simple, sensitive, accurate, precise and reproducible high performance liquid chromatography (HPLC) method for the determination of salicylic acid in pharmaceutical dosage forms. Shimadzo Prominance model L20 AD HPLC system equipped with SPD 20A UV-Vis detector was used for the analysis. The separation was done on RESTEX allure C18 column (3 μm, 15 cm × 4.6 mm), for an isocratic elution a mixture of water, methanol and glacial acetic acid (65:35:1, v/v) mobile phase at a wavelength of 254 nm. The flow rate was 1.0mL/min. The RP-HPLC method developed for analysis of salicylic acid was validated with respect to specificity, selectivity, linearity, accuracy, precision and robustness as per the ICH guidelines. The retention time of salicylic acid was 7.575 min. The linearity was established over the concentration ranges of 50-350 μg/mL with correlation coefficients ( r2) 0.999.  The percentage accuracy of salicylic acid ranged from 99.76 -101.66%. The relative standard deviation values for intra-day and inter-day precision was lower than 2.0% and the assay result was found to be in the range 99.57-101.32%. Salicylic acid was subjected to stress conditions such as neutral, acidic, alkaline, oxidation and photolysis degradations as per ICH guidelines. The degradation studies revealed that the drug was found to degrade maximum (1.67%) in alkaline degradation conditions and was highly resistant towards neutral, acidic, oxidative and photolytic degradation conditions.

Mannich bases of sparfloxacin were synthesized from the reaction of 5-acetylamino-1-cyclopropyl-7-(3΄,5΄-dimethyl-piperazin-1-yl)-6,8-difluoro-4-oxo1,4-dihydro-quinoline-3-carboxylic acid with formaldehyde and several isatin derivatives. The structures of the synthesized compounds were elucidated from the IR, 1H NMR, 13C NMR and FAB Mass data. The synthesized compounds were evaluated for the antibacterial, antitubercular and anticancer activity. The compounds showed good activity against Gram-positive bacteria and moderate activity against tested Gram-negative bacteria. The MIC for the compounds against M. tuberculosis H37Rv strain was 50 µg/mL. The most potent compound in this series 3c exhibited enhanced antibacterial activity than sparfloxacin against S. aureus, Bacillus Sp while the anticancer activity was in the range of 18.31- 23.61 µg/mL.