B. Mohammed Ishaq

Analytical method development and validation of prasugrel in bulk and its pharmaceutical formulation using the RP-HPLC method

Purpose: This study was designed to develop and validate a simple, sensitive, precise, and specific reverse phase high-performance liquid chromatographic (HPLC) method for the determination of prasugrel in bulk and its tablet dosage forms. Materials and Methods: The HPLC separation was carried out by reverse phase chromatography on an inertsil ODS-3V column (5 μm; 250 × 4.6mm2) with a mobile phase composed of 0.02 M potassium dihydrogen orthophosphate, 0.02 M dipotassium hydrogen orthophosphate in water:acetonitrile (30:70 v/v) in isocratic mode at a flow rate of 1 ml/min. The detection was monitored at 210 nm. Results: The calibration curve for prasugrel was linear from 100 to 600 μg/ml. The inter-day and intra-day precision was found to be within limits. The proposed method has adequate sensitivity, reproducibility, and specificity for the determination of prasugrel in bulk and its tablet dosage forms. The limit of detection and limit of quantification for prasugrel were found to be 0.25 μg/ml and 0.75 μg /ml, respectively. Accuracy (recoveries: 99.8–101.2%) and reproducibility were found to be satisfactory. Conclusion: The proposed method is simple, fast, accurate, and precise for the simultaneous quantification of prasugrel in the dosage form, bulk drugs as well as for routine analysis in quality control.

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF METAXALONE IN BULK AND ITS PHARMACEUTICAL FORMULATION BY UV SPECTROSCOPIC METHOD

Metaxalone, a muscle relaxant used to relax muscles and relieve p ain caused by strains, sprains and othermusculoskeletal conditions. A simple, accurate, precise, reproducible, highly sensitive, economic UV spectro photometric method has been developed for the estimation of metaxalon in bulk and tablet dosage form. In this method metaxalon showed maximum absorbance at 280 nm in methanol. The developed spectrophotometric method was validat ed in accordance with ICH gui delines. Linearity of the method was found to be 5 - 160µg/ml. The method obeyed Beer’s law in the concentration range of 5 - 160 µ g/ml. The LOD and LOQ were found to be 3.489 μ g/ml and 10.575μ g/ml respectively. A mean recovery of metaxalon in tablet dosage form was found to be 99.69 %.the method was found to be simple, accurate, precise, specific, sensitive, reproducible and can be directly and easily applied to tablet d osage fo rm.

Validated RP-HPLC-PDA method for simultaneous determination of Zidovudine, Lamivudine, and Nevirapine in pharmaceutical formulation

Aim and Objectives: A simple, rapid, and sensitive high performance liquid chromatographic method with ultraviolet detection has been developed and validated according to the International Conference on Harmonization (ICH) guidelines for the quantitation and qualification of zidovudine (ZID), lamivudine (LAM), and nevirapine (NEV) in pharmaceutical dosage forms. Materials and Methods: The proposed method was based on the separation of the drugs in reversed phase mode using Water′s C18 250 cm × 4.6 mm, 5 μ particle size column maintained at an ambient temperature. The optimum mobile phase consisted of Water: Methanol (70:30 v/v), pH adjusted to four with orthophosphoric acid (OPA). The flow rate of mobile phase was set 1.0 mL min -1 and photodiode array detection was performed at 275 nm with a total run time of 8 min which is very short for accurate analysis of simultaneous estimation of three analytes. The method was validated according to ICH guidelines. Results: The method was linear over the concentration range of 25-75 μg mL -1 with limit of quantifications (LOQ) of 13, 0.49, and 0.40 ng mL -1 for ZID, LAM and NEV respectively and limit of detection (LOD) of 4, 0.14, and 0.12 ng mL -1 for ZID, LAM and NEV respectively. Accuracy (% recovery studies) and precision values of both inter and intraday obtained from six different replicates for all the analytes ranged from 99.00% to 100.00% and % relative standard deviation of precision (assay) was between 0.64 and 1.28, respectively. All the three analytes and their combination drug product were exposed to thermal, photolytic, hydrolytic, reductive, oxidative and peroxide stress conditions and the stressed samples were analyzed by the proposed method. There were no interfering peaks from excipients, impurities or degradation products due to variable stress conditions and the proposed method is specific for the simultaneous estimation of ZID, LAM and NEV in the presence of their degradation products. Conclusion: The proposed method can be successfully applied in the quality control and stability samples of pharmaceutical dosage forms.