Development of stability indicating assay method for estimation of Ibuprofen and Famotidine in combined dosage form in tablet

A simple, precise, accurate, simultaneous stability indicating RP-HPLC method for the estimation of IBU (Ibuprofen) and FMT (Famotidine) in combined dosage form was developed using Grace RP-C18 (4.6 x 250mm, 5m) in an gradient mode with mobile phase comprising of Methanol: Water (pH 2.5 using OPA) The flow rate was 0.7 mL/ min and effluent was monitored at 240.0 nm. The retention times were found to be 6.68 min for IBU and 1.76 min for FMT. The assay exhibited a linear dynamic range of 30- 150 g/mL for IBU and 1- 5 g/mL for FMT. The calibration curves were linear (r 2 = 0.994 for IBU and r 2 = 0.997 for FMT) over the entire linear range. Mean % recovery was found to be 99.82 % for IBU and 99.91 % for FMT with % RSD was NMT 2 for both estimations which fully agrees with system suitability which is in good agreement with labeled amount of formulation. The % RSD for Intra- Day and Inter-Day Precision was NMT than 2 for both the drugs. The developed method was validated as per ICH guideline

Quantitative UV-spectrophotometry estimation of risperidone using hydrotropic solubilization phenomenon

The aim of present study was to develop simple and economical UV- pectrophotometric method for estimation of Risperidone using Area Under Curve (AUC) technique with the application of hydrotropic solubilisation phenomenon. Aqueous urea solution (30% v/v ) was used as hydrotropic agent for solubilising risperidone. The method is based upon integration of area under curve for analysis of risperidone in the wavelength range of 265.0 - 287.40 nm. The drug followed linearity in the concentration range of 4 - 24 g/mL with correlation coefficient value r 2 > 0.99. Proposed method was validated for accuracy, precision, repeatability and ruggedness as per ICH guidelines. The proposed method was applied for qualitative and quantitative estimation of risperidone in pharmaceutical formulation and results were found in good agreement with the label claimed. This developed method can be used for routine analysis of Risperidone in bulk and tablets

Stability indicating HPLC method development and validation for the simultaneous determination of Azithromycin & Ofloxacin in bulk and its dosage forms

A simple, precise, sensitive and reproducible stability indicating Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method for determination of Azithromycin and Ofloxacin in tablet dosage form was developed. Chromatographic separation was achieved on Hypersil-Keystone RP C 18 (250 4.6 mm, 5m) column maintained at 30 C eluted with mobile phase at flow rate of 1.2 ml/min. The mobile phase consists of Buffer (0.02 M potassium dihydrogenphosphate): methanol: acetonitrile in the ratio 65:25:10 v/v at pH maintained at 3.2 with OPA was used and the determination was carried out at 285 nm. The retention time for Azithromycin and Ofloxacin were 9.7 min and 5.01 respectively. The linearity was found in the range of 5?50 ?g/ml for Azithromycin and 4?40 ?g/ml for Ofloxacin. In stability studies the drugs were well separated from degradation products. The degradation was studied in the individual standard drugs, their mixture and formulation which gave the idea about the orgin of the degradant products. The analytical method was validated as per ICH guideline for linearity, accuracy, precision, and specificity, limit of detection, limit of quantification, stability in analytical solution etc. and method can be extended to the analysis of Azithromycin and Ofloxacin in tablet formulations

Determination of Rivaroxaban in pure, pharmaceutical formulations and human plasma samples by RP-HPLC

A simple, sensitive and rugged reverse-phase high performance liquid chromatographic method has been developed and validated for the determination of rivaroxaban in pure, pharmaceutical formulations and in spiked human plasma sample. The separation of rivaroxaban and internal standard was achieved on XDB C18 (150 x 4.6) mm column. Mobile phase employed for the study is the mixture of water and acetonitrile in gradient programme. A flow rate of 1 ml/min was found optimum for the study. Linearity of the proposed method was found to be in the range of 0.05 g/ml to 20 g/ml with r 2 =0.9999. The limit of detection and limit of quantification of the proposed method are found to be 0.015 g/ml and 0.046 g/ml, respectively. Intra-day and inter-day assay relative standard deviations were determined and found to be less than 2.0 %. The method has been applied successfully for the determination of rivaroxaban in its pharmaceutical formulations and in spiked human plasma samples

New validated rp-hplc method for simultaneous estimation of lamivudine and tenofovir disproxil fumarate in tablets

A simple, specific and precise reverse phase high performance liquid chromatographic method was developed and validated for simultaneous estimation of Lamivudine and Tenofovir disproxil fumarate in tablets. Quantification was achieved by using a reverse-phase C18 column (Inertsil ODS 3V, 250 mm x 4.6 mm; 5) at 31 o C. The mobile phase consisted of a mixture of phosphate buffer and acetonitrile in the ratio of 55:45 v/v at a flow rate of 1.2 mL/min. The retention times of Lamivudine and Tenofovir disproxil fumarate were found to be 2.430 min and 4.550 min respectively. The developed method was validated as per ICH Guidelines for linearity, accuracy, precision, detection limit, quantification limit, ruggedness, robustness, specificity and system suitability. The percentage recoveries for both of the drugs from their tablets were found to be 98.48 % and 98.64 % respectively. The method may successfully be employed for the simultaneous determination of Lamivudine and Tenofovir disproxil fumarate in pharmaceutical tablet dosage forms

Development and validation of RP-HPLC method for loxapine in capsule dosage form

A reversed phase-high performance liquid chromatography (RP-HPLC) method was developed for the determination of loxapine drug in tablet dosage form. The developed method was validated by measuring linearity, precision, limit of detection (LOD), robustness and ruggedness, drug recovery and for system suitability. Water and acetonitrile in the ratio 55:45 v/v was the mobile phase with C 18 column (250 mm x 4.5 mm x 5 m) as a stationary phase and 265 nm was the detection wavelength. The HPLC system was operated in isocratic mode. The measured retention time of loxapine drug was 6.88 minutes and the limit of detection was 0.035 g/ml, respectively. The linearity measured in the range 10-100 g/ml had a correlation coefficient of 0.999. The results of the parameters precision, robustness, recovery and formulation assay indicate that the developed method is a very good tool for the analysis of loxapine drug in tablet dosage form in bulk

Development and Validation of Glimepiride and Metformin in Human Plasma by HPLC: An application study

A simple and cost effective RP-HPLC method is developed for simultaneous estimation of glimepiride (GLIM) and metformin (MET) at tablet dosage form using C-18 column (4.6 x 250mm, 5?, 100 A?) with a mobile phase composed ofmethanol: water (90:10% v/v) buffered with ortho phosphoric acid at a flow rate of1.0 mL/min (UV detection at 231 nm). The retention time of both drugs (GLIM and MET) are observed as 4.286 and 2.262 respectively. Human plasma spiking studies of both the API and the formulation at the concentration of (0.2g/mL - 1g/mL) for glimepiride and metformin (1g/mL - 5g/mL) expresses the standard correlation coefficients of 0.9998 and 0.9999 respectively for API and 0.9917 and 0.99 respectively for the tablet dosage form. The mean (%) recoveries of glimepiride and metformin are 99.98 and 99.9% respectively. The % RSD below 0.5 shows the high precision of the proposed method. Assay studies revealed that 98.05% of purity is observed for glimepiride and 99.69 for metformin in a tablet dosage form. Human plasma spiking studies revealed that a minimal quantum of glimepiride had been bound with the plasma proteins compare to metformin in the tablet dosage form. The method was validated as per the ICH guidelines

IR quantification of fenofibric acid in bulk and oral dosage form

Simple and sensitive infrared spectrophotometric method has been developed for the estimation of fenofibric acid in tablet dosage form.Beer?s concentration range was found to lie between 5 to 15 mg. The correlation coefficient for the method was found to be 0.9946 and the developed method was analyzed for specificity, linearity of response, precision and accuracy; thus the proposed method could be adopted for routine analysis of bulk drug and its formulation

Development and validation of a stability indicating RP-HPLC method for determination of flucytosine and its process related impurities in injectable pharmaceuticals

A simple, sensitive reproducible and cost effective reversed-phase liquid chromatography (RPHPLC) method coupled with a photodiode array detector was developed and validated for determination of Flucytosine and its related substances in pharmaceutical dosage forms, especially for injectable solution. The separation was achieved from octadecylsilyl silica gel, C18 (4.6 mm x 250 mm, 5) column with a mobile phase consisting of HPLC grade Water and Methanol (95:5) at a flow rate of 1ml/min with UV detection at 260 nm at 30 C column temperature. Total run time was 10 min within which main compound and other known (Fluorouracil) and unknown impurities were separated. Stability indicating capability was established by force degradation experiments and separation of known degradation products. This chromatographic method was optimized using the samples generated from forced degradation studies and the impurity spiked solution. Good resolution between the peaks corresponds to process-related impurities and degradation products from the analyte were achieved. The method was validated for Accuracy, Repeatability, Reproducibility and Robustness, Linearity, LOQ and LOD were established for Flucytosine and its impurities in a single RPHPLC method. Therefore, this method can be used as a more convenient and efficient option for the analysis of Flucytosine assay and its related substances in injectable pharmaceutical dosage form to establish the quality of the drug product during routine analysis with consistent and reproducible results

Simultaneous determination of Cefixime trihydrate and Ofloxacin in pharmaceutical dosage form by second order derivative UV spectrophotometry

Derivative spectrophotometry offers a useful approach for the analysis of drugs in multi-component formulation. In this study a second order derivative spectrophotometric method is applied for the simultaneous determination of Cefixime Trihydrate and Ofloxacin in Tablet dosage form. The measurements were carried out at wavelengths of 307 and 298 nm for Cefixime Trihydrate and Ofloxacin respectively. The method was found to be linear (r=0.999) in the range of 4-20 ?g/ml for Cefixime Trihydrate in the presence of 20 ?g/ml of Ofloxacin at 307 nm. The linear correlation (r=0.999) was obtained in the range of 4-20 ?g/ml for Ofloxacin in the presence of 20 ?g/ml of Cefixime Trihydrate at 298 nm. The method was successfully used for simultaneous determination of Cefixime Trihydrate and Ofloxacin in tablet dosage form without any interference from excipients and prior separation