K. Vanitha Prakash

The aim of present work was to develop an accurate, precise, reproducible and economical UV spectrophotometric method for estimation of 1H, 1’-H-2, 2’-Bibenzimidazole Impurity In Telmisartan Bulk and Formulation. This method was based on area under curve of UV spectrum between 235 to 254 nm and validated as per ICH guideline Q2 (R1). The method has followed linearity in the range of 5-30μg/ml. The value of correlation coefficient was 0.998. Satisfactory values of Percent relative standard deviation for the intra-day and inter-day precision indicated that method is precise. Results of the recovery studies (97.63% to 98.66 %) showed accuracy of the method. LOD and LOQ were calculated as 0.3221μg/ml and 0.9761 μg/ml, respectively. The developed method can be used for routine estimation of 1H, 1’-H-2, 2’-Bibenzimidazole Impurity In Telmisartan Bulk and Formulation.

A new simple, precise, accurate and reproducible RP-HPLC method for simultaneous estimation of gentamicin and clobetasol in bulk and pharmaceutical formulations. Separation of gentamicin and clobetasol was successfully achieved on a Zorbax C18 (150 mm x 4.6mm x 5µ ) in an isocratic mode utilizing disodium hydrogen phosphate buffer and methanol (60:40 v/v) at a flow rate of 1.0 mL/min. The method was validated according to ICH guidelines for linearity, sensitivity, accuracy, precision, specificity and robustness. The response was found to be linear in the drug concentration range of 0.1-0.30 mg/mL for gentamicin and 0.05–0.15 mg/mL for clobetasol. The correlation coefficient was found to be 0.9997 for both the drugs. The LOD and LOQ for gentamicin were found to be 0.3525 µg/mL and 1.1751 µg/mL respectively. The LOD and LOQ for clobetasol were found to be 0.1938 µg/mL and 0.6460 µg/mL respectively.  The proposed method was found to be good percentage recovery for gentamicin and clobetasol, which indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard solution with the sample solution. Therefore, the proposed method specifically determines the analyte in the sample without interference from excipients of pharmaceutical dosage forms.

A simple, accurate, precise and rapid reversed-phase high performance liquid chromatographic (RP-HPLC) method has been developed and subsequently validated for the estimation of Liraglutide in bulk and Parenteral Dosage form. The proposed method is based on the separation of drugs in reversed-phase mode using Waters HPLC 22695 model, Inertsil ODS column (250 x 4.6 mm, 5µm particle size).The optimum mobile phase consisted of methanol: phosphate buffer in the ratio of 85:15 v/v(Phosphate buffer pH 5.5) was selected as a mobile phase, flow rate of 1.0 ml/min and UV detection was set at 246 nm. The retention time was 3.25.The method was validated according to ICH guidelines. It was found to be accurate and reproducible. Linearity was obtained in the concentration range of 20-80 μg/ml . The percentage RSD for precision and accuracy of the method was found to be less than 2%. The proposed method can be successfully applied in the quality control of bulk and pharmaceutical dosage forms.

A Simple, selective, accurate, precise and linear RP-HPLC method was developed and subsequently validated for estimation of cinacalcet in bulk & tablet dosage form. Gradient elution at a flow rate of 0.8ml/min was used for separation of drugs in reversed-phase mode using Waters HPLC 22695 model on a INERTSIL ODS C18 column (150 x 4.6 mm; 5µ) at a ambient temperature. Mobile phase consisted of water: methanol: acetonitrile (20:60:20). The UV detection wavelength was 235nm 20 µl was injected. The retention time for cinacalcet was 3.7min. The percentage RSD for precision and accuracy of the method was found to be less than 2%. The % recovery was within the range between 99.73% and 99.85%. The method was validated as per the ICH guidelines. Key words: cinacalcet, RP-HPLC, validation