Rp Pdc Case Study

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DEVELOPMENT AND VALIDATION OF RP-HPLC-PDA METHOD FOR THE ESTIMATION OF MACITENTAN IN BULK AND TABLET DOSAGE FORMS. AZIZ UNNISA1, 2*, SYED. SADATH ALI3, SANTOSH KUMAR.S1 1KVSR Siddhartha College of Pharmaceutical Sciences, Vijayawada-520010, AP, INDIA. 2 Sunrise University, Alwar, Rajasthan, India. 3Azad institute of Pharmacy and research, Lucknow, India. E-mail: khushiazeez@yahoo.co.in Phone no: 09885056721 Corresponding author Aziz Unnisa, Department of Pharmaceutical Analysis, KVSR Siddhartha College of Pharmaceutical Sciences, Vijayawada - 520010, AP, India. Phone no: +919885056721. email address: khushiazeez@yahoo.co.in ABSTRACT The aim of the present study was to develop RP-HPLC-PDA method for the estimation of Macitentan…show more content…
Ammonium Acetate, water and Acetonitrile were perchased from Merck India, Mumbai. All the solvents used were of HPLC grade. The other chemicals and reagents were of AR grade. Instrumentation A Shimadzu Prominence HPLC system provided with DGU-20A3 degasser, LC-20AD binary pumps, SIL-20AHT auto sampler and SPD-M20A PDA detector was used. Data acquisition was carried out using LC solutions software. The chromatographic analysis was performed on Inertsil C18 reverse phase column (150 × 4.6mm, 5µ). Chromatographic Conditions Mobile phase consisting of Acetonitrile:10mM Ammonium acetate (40:60v/v) was used in isocratic mode, the mobile phase was filtered through nylon disc filter of 0.45µm (Millipore) and sonicated for 3 min before use. The flow rate was set at 1.2 mL/min and the injection volume was 10µL. PDA detection was performed at 255 nm and the separation was achieved at ambient temperature. Preparation of stock solutions Accurately weighed quantitiy of MCT was dissolved in sufficient quantity of methanol in a 10mL volumetric flask. The volume was adjusted up to the mark with methanol to obtain a stock solution of 10mg/mL of MCT. Method…show more content…
A series of standard dilutions were prepared over a concentration range of 2-10μg/mL for MCT and injected on to the column in triplicate. Linearity is evaluated by a plot of peak areas as a function of analyte concentration and the test results were evaluated by appropriate statistical methods where by slope, intercept, regression (R2) and correlation coefficient (R) were calculated. Precision Precision is the measure of closeness of the data values to each other for a number of measurements under the same analytical conditions. Repeatability was assessed by using a minimum of six determinations at 100 % of the test concentration (4μg/mL of MCT). The standard deviation and the relative standard deviation (RSD) were computed for precision. Accuracy Accuracy was established across the specified range of the analytical procedure. To ascertain the accuracy of the proposed method recovery studies were performed by the standard addition method by spiking 80%, 100%, 120% of the known quantities of standards within the range of linearity to the synthetic solution of drug product (4μg/mL of MCT), these solutions were analyzed by developed method in triplicate. The % recovery and the %RSD were calculated at each level of

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