The present study described the development of a reversed-phase liquid chromatographic method for the estimation of abiraterone acetate by Quality by Design (QbD) approach. Using an isocratic solvent system for the mobile phase, the chromatographic estimation of analyte was performed on a Hypersil BDS C18 column using mobile phase mixture containing acetonitrile and water with pH adjusted with 0.1% v/v orthophosphoric acid (15:85%v/v ratio), flow rate 1.0 mL.min−1 and detection at 250 nm using photodiode array detector. Systematic development of the chromatographic method was carried out by factor screening using a half-factorial design which suggested organic modifier (%), flow rate (mL.min−1) and autosampler temperature (°C) as influential variables. Further, the method was optimized by Box–Behnken design and trials performed were evaluated for the area under peak, retention time, theoretical plate count and tailing factor as the responses. Validation of the developed method showed good linearity, accuracy, precision and sensitivity. Evaluation of the stability-indicating profile of the method using forced degradation studies revealed the formation of a possible degradation product under acidic and alkaline conditions, while no such degradation product peaks were observed under the oxidative environment. Overall, the study construed the successful development of HPLC assay method for pharmaceutical applications.

Background: Quality by design based software’s in analytical research and development normally encompasses multiple objectives. For decades, this task has been attempted through trial and error, supplemented with the previous experience, knowledge, and wisdom of the analytical researchers. Objective: The study analyzes the current QbD-assisted software’s such as design-experts, minitab, fusion product development etc. and its broad implementations in an analytical research and developments. Methods: Traditional approach may fails to meet the intended purpose by trial and error procedure during the analytical research and development. However, in modern scientific technology equipped with highly advanced features associated software’s of the QbD paradigm. The impact and interactions between the critical process variables and critical method attributes such as resolution, tailing, etc. can be well understood by the screening, optimization and robustness studies based on the principles of experimental design. Result: Design of experiment assimilates statistical multi¬variate analysis instead of one factor at a time approach. This also provides a prominent, most reliable quality output, which is also essential for getting highly robust method as well as to obtain homogenous product development. Conclusion: The present review, critically discussed about the various QbD based multivariate software’s and their applications in drug development and analytical research.

Cleaning validation is a prominent and ideal practice which is employed in industrial aspects to provide utmost shielding to develop drug products, so that a cleaning practice removes the particulate matters, chemicals, as well as the contaminant pathogens reside in active ingredients of drug product in a piece of apparatus, which are produced or being manufactured. The cleaning validation is established as the pre-eminent process that ensures the efficiency, safety, consistency of pharmaceutical equipment and manufactured product of assured quality. The utmost cleaning practice during manufacturing of drug substances affords the appropriate operator safety measures, organized calibration, description and routine monitoring of equipments, Sampling procedures, acceptance criteria's and detection limits of analytical methods. This also lead to systematic data analysis for estimating of probable contagions in product batches builds up. Abortive cleaning may lead to adulterated product that may be originated from preceding batches, clean-up agents or other superfluous materials produced during methodology. Hence to avoid the harmful contamination, sources, safety measures clean-in-practice is highly recommended as per regulatory and stability point of view. The present review intensifies the current challenges, basic mechanisms and future implication of cleaning validation in various analytical development firms and research organizations.

Abstract:Fluoxetine is an antidepressant of the selective serotonin reuptake inhibitor class. Two simple, rapid and sensitive first and second derivative spectrophotometric methods are developed for the determination of fluoxetine (FLX) in pharmaceutical dosage forms (capsules). The absorption minima was chosen (at 235 nm) in first order (Method A) and amplitude (229-238.5 nm) was selected in second order derivative spectral calculations. Fluoxetine follows Beer's law in the concentration range of 1-60 µg mL -1 (r 2 = 0.999) in first order as well as in second order (r 2 = 0.9994) derivative spectroscopy respectively. The proposed methods can be successfully applied for the determination of Fluoxetine in commercial brands of pharmaceutical formulations. No interferences were observed from the common excipients in the formulations. The methods were validated according to ICH guidelines.

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