No abstract

Objective: Statistically designed and Box-Behnken design (BBD) assisted reversed-phase high-performance liquid chromatography-ultraviolet (HPLC-UV) method was developed and validated for the identification of an antipsychotic medication Olanzapine and its organic impurities in pure drug along with forced degradation studies. Methods: The present developed method employed BBD optimized chromatographic conditions comprising of an Inertsil ODS 3V analytical column with dimension 250 mm x 4.6 mm and particle size 5µ. The isocratic mobile phase was used as a mixture of monobasic sodium phosphate buffer (0.01 M, pH 6), methanol and acetonitrile in the proportion of 40/30/30, v/v. The mobile phase flow rate and UV λmax was 1 ml/min and 260 nm, respectively. The method was optimized by Box-Behnken design using design expert software, comprising of three factors for Olanzapine for instance flow rate (A), mobile phase composition (B) and pH (C) while resolution between Olanzapine related compound A and Olanzapine related compound B (Y1) and tailing of Olanzapine (Y2) were taken as a response. Results: Application of BBD yielded statistically designed method with excellent quality parameters achieved in terms of linearity with the coefficient of correlation (R2>0.9999), limit of detection (LOD, 0.0023-0.16 µg/ml), the limit of quantification (LOQ, 0.007-0.39 µg/ml), accuracy (99-100%) and precision ((2%, relative standard deviation (%RSD) were evaluated as per latest available procedures. Conclusion: Forced degradation conditions were carried out, demonstrated that the optimized method was stable and no any interfering peaks eluting at the similar retention time of the studied compounds. The method was found to be stable, easy, rugged and robust, could be applied for the similar types of the pure drug.

The purpose of the present work was to formulate colon-targeted mesalamine pellets containing gums of Moringa oleifera Lam. (MOG) and Cyamopsis tetragonolobus Taub. (CTG). Formulation of single stimuli mediated release is also difficult to target colon due to variation in the physiological condition, so in present work, pHdependent and enzyme degradation mechanisms are being used to release of drug at the colonic site. Extrusion and spheronization techniques were used for the preparation of pellets. For formulation optimization, factorial design study 32 was used for the selection of the optimized batch. It was found that high ratio of solvent 80:20 and 10% and 7.5% concentration of MOG and CTG respectively produce optimized pellets showed good physical properties and release for F8M and F8C and after coating it showed in vitro release at the colonic condition and in vivo roentgenographic images for targeting. As to say as advantages, spheronization and extrusion method was proved to have economized, whereas natural gums used to control release which added advantage as being as inert and biocompatible. This further formulation scope at industrial scales to reduce side effects of synthetic polymer and make it more biocompatible with the body.

An innovative, specific, economical and precise method was developed and validated by employing reverse phase high performance liquid chromatography (HPLC) for contemporaneous estimation of dextromethorphan hydrobromide (DHB) along with its impurities in liquid formulation with forced degradation studies and confirmation of content of DHB in composition label in three market formulations along with their impurities were detected by this method. The optimized chromatographic conditions comprised of column (25 cm × 0.46 cm) × 5 μm Kromasil C8 bearing flow rate of 1.5 mL/min and wavelength 220 nm for UV-estimation. Design of experiments were implemented by following Box Behnken design with most optimum parameters selected as follows, column temperature (A), flow rate (B) and pH (C) with corresponding responses comprised of resolution between related compound A (RCA) and DHB (Y1), tailing of DHB (Y2) and resolution between related compound B (RCB) and DHB (Y3). Stress testing was performed and proved that method was stable as no interfering peaks were observed. All validation parameters including suitability, linearity, accuracy, specificity, limit of detection, limit of quantitation, ruggedness, robustness and stress study were evaluated as per updated ICH guidelines and found to be within limit for pure DHB and detected impurities.