Precision

The aim of the present work was to develop and validate a simple and efficient method for the analysis of Ambrisentan in pharmaceutical dosage forms by reverse phase high pressure liquid chromatography. A stainless steel column 150 mm long, 4.6 mm internal diameter filled with octasilyl silica chemically bonded with silica gel particles of 5 mm diameter was used for elution. The retention time of Ambrisentan was 4.451 min. The method showed a good linearity in the concentration range of 12.5-250 µg/mL with a correlation coefficient of 1.000. The validation characteristics included specificity, linearity, limit of detection, limit of quantification, precision, robustness and stability. Validation acceptance criteria were met in all cases. The method could be successfully used for the analysis of Ambrisentan in pharmaceutical dosage forms.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Fosfomycin in Fosfomycin for Injection. The drug is freely soluble in analytical grade water 1. The drug was identified in terms of solubility studies and on the basis of melting point done on melting point apparatus of Equiptronics 2. It showed absorption maxima were determined in analytical grade water. The drug obeyed the Beer’s law and showed good correlation of concentration with absorption which reflect in linearity 4, 5, 6. The UV spectroscopic method was developed for estimation of Fosfomycin in injection dosage form and also validated as per ICH guidelines. The drug is freely soluble in analytical grade water, slightly soluble in 95% Methanol and Ethanol. Almost insoluble in anhydrous acetone, ether and chlorinated solvent. So, the analytical grade water is used as a diluent in method. The melting point of Fosfomycin was found to be 94 - 95?C (uncorrected). It showed absorption maxima 254 nm in analytical grade water. On the basis of absorption spectrum the working concentration was set on 50µg/ml (PPM). The linearity was observed between 30-70 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 101.00 and 99.17% for three levels respectively. The % RSD for precision was found to be 0.41%. A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Fosfomycin in Fosfomycin for Injection dosage form. The method could be considered for the determination of Fosfomycin in quality control laboratories.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Fluconazole in tablet dosage form. The drug is freely soluble in organic solvents such as ethanol, DMSO, and dimethyl formamide. The drug was identified in terms of solubility studies and on the basis of melting point done on Melting Point Apparatus of Equiptronics. It showed absorption maxima were determined in Ethanol. The drug obeyed the Beer’s law and showed good correlation of concentration with absorption which reflect in linearity. The UV spectroscopic method was developed for estimation of Fluconazole in tablet dosage form and also validated as per ICH guidelines. The drug is freely soluble in organic solvents such as Ethanol, DMSO, and Dimethyl Formamide. So, the Analytical Grade Ethanol is used as a diluent in method. The melting point of Fluconazole was found to be 139-140?C (uncorrected). It showed absorption maxima 252 nm in Ethanol. On the basis of absorption spectrum the working concentration was set on 60µg/ml (PPM). The linearity was observed between 20-100 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 101.00 and 100.83% for three levels respectively. The % RSD for precision was found to be 0.78%. A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Fluconazole in tablet dosage form. The method could be considered for the determination of Fluconazole in quality control laboratories.

A simple Reverse phase liquid chromatographic method has been developed and subsequently validated for estimation of lansoprazole in tablet dosage form. The separation was carried out using a mobile phase consisting of Methanol and 0.1% OPA (Ortho Phosphoric Acid) in the ratio of 70:30. The column used was C18 and 250 mm length with flow rate of 1.2 ml / min using UV detection at 285nm. The described method was linear over a concentration range of 10-50 μg/ml for the assay of Lansoprazole. The retention time of Lansoprazole was found to be 6.6 min, and all the results of analysis were validated statistically. The results of the study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of Lansoprazole in tablet dosage form and in its pharmaceutical dosage forms.

A new, simple, accurate, precise and robust isocratic RP-HPLC method has been developed and subsequently validated for the determination of Regorafenib in pure form and pharmaceutical dosage forms as per ICH guidelines. The separation achieved on a Symmetry C18 Column, 250 mm x 4.6 mm i.d. and 5µm particle size column as a stationary phase and Methanol: Phosphate buffer (pH adjusted to 4.80 with phosphoric acid) in the ratio of 70:30v/v used as mobile phase at a flow rate of 1.0 ml/min. The UV detection was performed at 268nm. The retention time for Regorafenib was found to be 3.544minutes. The detector response was linear in the concentration range of 0-16µg/ml. The respective linear regression equation being Y= 58945.x + 9634 with R2 = 0.999. The percentage of Regorafenib in pharmaceutical dosage form was found to be within the limits. The limit of detection and the limit of quantification were found to be 0.90µg/ml and 2.90µg/ml respectively. The results of the study showed that, the proposed RP-HPLC method was simple, rapid, precise, accurate and stability indicating, which can be used for the routine determination of Regorafenib in pure form and pharmaceutical dosage forms.

Zafirlukast, Cyclopentyl (3-(2-methoxy-4-((o-tolylsulfonyl) carbamoyl) benzyl)-1-methyl-1H-indol-5-yl) carbamate (I). A high-performance liquid chromatographic (HPLC) reversed-phase rapid resolution method has been developed and validated for estimation of zafirlukast in a pharmaceutical active pharmaceutical ingredient, which was chromatographed on reversed-phase Hypersil Gold C18 , 2.1 x 100 mm , 1.9 µ column using mixtures of acetonitrile/water and the eluents were monitored at different wavelengths. The method was validated statistically for its linearity, accuracy, robustness and precision. The method employed same chromatographic condition as above and validated in terms of linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and solution stability. Present work also describes the development and validation of RP- RRLC method for the determination of impurities of zafirlukast.