2 research outputs found
Stability indicating HPLC method for the simultaneous analysis of Gatifloxacin and Loteprednol in eyedrop formulation using design of experiment approach
Get PDFDesign of experiment (DOE) assisted simple, rapid, precise and accurate stability indicating HPLC method has been developed for simultaneous estimation of Gatifloxacin (GTF) and Loteprednol (LOT) along with their forced degradation products. The developed method has been optimized and developed by using central composite design (CCD) in response surface methodology (RSM). Trails have been undertaken and ratio of phosphate buffer in mobile phase, pH of buffer and flow rate are selected as factors. Resolution, tailing factor (GTF) and tailing factor (LOTE) are selected for determining the system response in the process of method optimization. The responses have been optimized using the Derringer’s desirability function. The effective separation is achieved on Phenomenex EVO-C18 column (250 mm x 4.6 mm i.d, 5 μm particle size) with mobile composed of 10 mM phosphate buffer, pH 3.5 and organic phase composed of mixture of acetonitrile and methanol 60:40 % v/v, the flow rate was 1.0 mL/min, the signals were detected at 267 nm. The developed method was validated for linearity, accuracy, precision, and robustness. The method was applied successfully for stability samples
An gradient HPLC-DAD determination of phenylepherine, paracetamol, ambroxol and levocetrizine in pharmaceutical formulation
Get PDFThe development, validation and application of a simple and reliable gradient high-performance liquid chromatography–diode array detection (HPLC–DAD) procedure for the analysis of a complex mixture containing phenylephrine (PHE), paracetamol (PAR), ambroxol (AMB) and Levocetirizine (LEV) has been carried out . Chromatographic separation of PHE, PAR, AMB and LEV is achieved using a Phenomenex Ultracarb ODS-C18 (4.6×150 mm, 5 µ) column with gradient elution of the mobile phase composed of 10 mM phosphate buffer pH 3.3 and acetonitrile. A three step gradient program has been developed with step-1 elution starting with 2% (by volume) acetonitrile which ramped up linearly to 50% in 10 min, in step-2 reverting back to 20% in 5 min and in step-3 ended to achieve initial concentration of 2% in next 5 min thus contributing a total run time of 20 min. Flow rate maintained throughout the experiment is 1 mL/min. The Diode array detector (DAD) is set at 220 nm for quantification of the analytes based on measuring their peak areas. The retention times for PHE, PAR, AMB and LEV are approximately 4.4, 10.1, 14.00 and 17.90 min respectively. The proposed HPLC procedure is statistically validated with respect to linearity, ranges, precision, accuracy, selectivity and robustness. Calibration curves are found to be linear in 50 to 150% of target analyte in formulation with correlation coefficients > 0.9996. The validated HPLC method is applied successfully with good recoveries of analytes from tablet dosage; no interfering peaks were encountered from the inactive ingredients
