Analytical Method Development and Validation by Chemometric Approach for the Marketed Formulations

Abstract

Analysis of multi-component formulations is an important issue in modern analytical chemistry. newlineThe presented work comprised of Design and optimisation of two chemometric techniques, PLS and PCR with UV spectrophotometry in the simultaneous determination of 11 selected multi-component formulations. Development and validation of RP-UHPLC and HPTLC methods with factorial design for the simultaneous determination of selected multidrug combinations. CHEMOMETRICS ASSISTED UV SPECTROPHOTOMETRY: UV spectrophotometry with chemometric techniques, PLS and PCR consisted of designing of 25 and 9 sets of mixed standards of calibration (training) and prediction (validation) sets respectively. The constructed calibration model was validated by means of the prediction set. Then the built model was applied to the pharmaceutical formulations. The accuracy of the proposed method was ensured by performing recovery studies. The prepared mixtures of calibration (training), validation (prediction) sets, commercial formulations and recovery studies were scanned in an electronic UV absorption spectrophotometer and their spectras were recorded in the wavelength range of 200-400 nm at 1 nm interval. The chemometric calculations of the resulting multi-variate data was computed in a Pentium IV computer with CAMO UNSCRAMBLER X version 10.1 and the calculations of the statistical parameters were done on the excel sheet. The selection of optimum no. of factors and wavelength region becomes the important steps in PLS and PCR models. The predictive ability of the models was determined from RMSEC, RMSEP and r values of the drugs. Good agreement was seen in the assay results of the marketed samples. The results of the recovery studies were satisfactory. Reverse Phase - Ultra High Performance Liquid Chromatography with factorial design: The selection of the column, mobile phase, pH, flow rate and detection wavelength were done based on the peak purity and system suitability parameters such as resolution of the peaks, tailing factor, no. of theoretical plates.