A stability-indicating RP-HPLC method was developed and validated for the estimation of Liraglutide in bulk and pharmaceutical dosage forms. Shiseido C18 (250 mm x 4.6 mm I.D., 5 µm particle size) column was used as stationary phase with mobile phase consisting methanol+acetonitrile (80:20): phosphate buffer (pH 3.0 adjusted with ortho phosphoric acid) in the ratio of 75:25, v/v. The flow rate was maintained at 1.2 ml/min and effluents were monitored at 245 nm. The retention time was found to be 2.837 minutes. The forced degradation studies were performed as per ICH guidelines under acidic, alkali, oxidative, thermal, photostability and neutral conditions. The drug peak was well resolved from the peaks of degraded products. From the degradation studies it is evident that the drug showed instability under acidic, alkali, oxidative, thermal, photostability and neutral conditions. The linearity of the method was observed in the concentration range of 10-60 µg/ml with the number of theoretical plates & tailing factor being 5550 & 1.17 respectively with a correlation coefficient of 0.999. The percentage assay of Liraglutide was found to be 99.66%. The method was validated for its accuracy, precision and system suitability. The results obtained in the study were within the limits of ICH guidelines and hence this method can be used for the estimation of Liraglutide in bulk and pharmaceutical dosage forms.
The main objective of the present work was to develop a simple, precise, accurate and reproducible UV-Spectrophotometric and stability indicating RP-HPLC methods for simultaneous estimation of moxifloxacin HCl (MOX) and ketorolac tromethamine (KET) in bulk and ophthalmic dosage forms. UV Spectrophotometry was carried out by simultaneous equation method using distilled water : acetonitrile (50:50 V/V) as solvent. The wavelengths were found to be 295 nm for MOX and 322 nm for KET. The isobestic point was found to be 308 nm. The linearity range is 2-10 μg/mL for both MOX and KET with correlation co-efficient >0.99. The separation of these two drugs using RP-HPLC was achieved on a SHISHEDO C18, 250×4.6 mm, 5 micron size column with a mobile phase consisting of acetonitrile and acetate buffer (45:55 V/V) at pH 4.0 at a flow rate of 1 mL/min and UV detection at 308 nm. The retention times were observed to be 2.418 and 3.827 minutes for MOX and KET, respectively. Linearity was found to be 10-50 μg/mL for both MOX and KET, respectively. The two developed methods were successfully validated for accuracy, precision, linearity, limit of detection, limit of quantification and robustness. The two developed methods were validated according to ICH guidelines and were found to be with in the limits. The stress testing of the drugs individually was carried out under acidic, alkaline, oxidation, photo-stability and thermal degradation conditions and its degradation products were studied. These two methods could be used for simultaneous estimation of MOX and KET in bulk and ophthalmic dosage forms.
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