Isocratic elution of the mobile phase 0 02 M potassium dihydrogen

Isocratic elution of the mobile phase 0.02 M potassium dihydrogen orthophosphate, 0.02 M dipotassium hydrogen orthophosphate in water:acetonitrile (30:70 v/v) with the flow rate of 1 ml/min. Separation was performed on an inertsil ODS-3V analytical column http://www.selleckchem.com/products/Tubacin.html (Thermo Hypersil, 5 ��m; 250 �� 4.6mm2 i.d. with C18 insert (100 Ao, waters limited) as pre-column to protect the analytical column from strongly bonded material. Integration of the detector output was performed using the Shimadzu Empower software to determine the peak area. The contents of the mobile phase were filtered through a 0.45-��m membrane filter and degassed by sonication before use. The flow rate of the mobile phase was optimized to 1 ml/min which yields a column back pressure of 110�C112 kg/cm2.

The run time was set at 20 min and a column temperature was maintained at ambient. The volume of injection was 20 ��l, prior to injection of the analyte, the column was equilibrated for 30�C40 min with the mobile phase. The eluent was detected at 210 nm. The developed method was validated in terms of specificity, linearity, accuracy, limit of detection (LOD), limit of quantification (LOQ), intra-day and inter-day precision and robustness for the assay of prasugrel as per ICH guidelines.[11] Diluent Acetonitrile was used as a diluent. Standard preparation Stock solution of prasugrel was prepared by dissolving 500 mg of prasugrel in a 100 ml volumetric flask, and the volume is made up with the diluents. Subsequent dilutions of this solution ranging from 0.05 to 500 ��g/ml were made with the diluent.

Sample preparation Twenty tablets were taken, and their average weight was calculated. The tablets were crushed to a fine powder, dose equivalent to 10 mg was transferred to a 100 ml volumetric flask, dissolved in a diluent, and then the solution was made up to the mark with the same and filtered through 0.45 ��m membrane filter. Five milliliter of this solution was pipetted into a 50 ml volumetric flask and diluted with the diluent to get a concentration of 500 ��g/ml. Assay A mass of not less than 10 tablets was prepared by grinding them to a fine, uniform particle size powder using a mortar and pestle. After calculating the average tablet weight, a composite equivalent to the 10 mg was accurately weighed and quantitatively transferred into a 100-ml volumetric flask.

Approximately, 10-ml milli-Q water was added, the solution was sonicated for 10 min, 70 ml diluents was added to it, and mechanically shaken for 10 more minutes. The flask was equilibrated to room temperature, carefully filled to volume with the diluent, and mixed well. A portion of the solution Carfilzomib was filtered through a 0.45 mm membrane filter, discarding the first 2�C3 ml of the filtrate. A portion of the filtered sample (5.

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