QBD APPROCH BASED DEVELOPMENT OF VALIDATED ANALYTICAL METHOD FOR ESTIMATION OF CLARITHROMYCIN BY RP-HPLC

Abstract

Based on QbD, a chromatographic technique for estimation of clarithromycin from bulk was developed and validated.
The method for analysis of clarithromycin is obtained by QbD trial optimization. For the QbD approach Mobile phase
and flow rate are chosen as factors. While two responses were taken i.e.retention time and the peak area, the research
was carried out using Design of Expert software. Response 1 RT outcomes are F- Value 145.44, P-Value less than 0.05,
predicted & adjusted R2are 0.9570 & 0.9763 respectively. Response 2 Peak Area outcomes are F- Value72.09, P-Value
less than 0.05, predicted & adjusted R2 are 0.8777 & 0.0.9104 respectively. The optimized batch was carried out by
HPLC gradient system with auto-injector using UV (DAD) detector which had C18 quaternary gradient column at room
temperature. The mobile phase was ACN: Water (09:91) with a flow rate of 0.9 ml/min. The sample was detected at a
wavelength 209 nm and the sample size was 20μl. According to ICH guidelines, the purpose of method validation is to
demonstrate the acceptability of an analytical technique for its intended purpose. The validated parameter includes the
recovery study found (% RCVD -100), Linearity regression (0.999) which obtained a parallel calibration curve,
repeatability (RSD%-0.26) and LOD & LOQ were found at 9.206μg/ml & 27.898μg/ml respectively. Acid, base,
H2O2, and neutral were used in the stress degradation investigation. The degradation with acid (5.08%), base (96%),
H2O2 (32.14%), and neutral (3.42%) were found. The developed approach is used to analyze clarithromycin in
pharmaceutical formulations and is unique and accurate.