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Abstract

METHOD DEVELOPMENT AND VALIDATION OF BUCLIZINE HYDROCHLORIDE ASSAY AND ITS ORGANIC IMPURITIES IN API AND PHARMACEUTICAL FORMULATION BY USING ORTHOGONAL DETECTOR TECHNIQUES (UHPLC-MS) WITH DESIGN OF EXPERIMENTS

J. Satish*, P. Radhakrishnanand, P. Padmanabha Raju, M. Ajay Babu and K. Eswara Raju

ABSTRACT

To develop and validate a sensitive and stability indicating gradient compatible design of experiment (DOE) based reverse phase ultra-high performance (UHPLC-PDA) liquid chromatography with photodiode array (PDA) and mass spectroscopy (MS) of buclizine hydrochloride (BH) assay and organic impurities (OI) in active pharmaceutical ingredient (API) and pharmaceutical formulation (PF). The chromatographic conditions were optimized using a Zorbax SB-C18 analytical UHPLC column with the dimensions (100 x 2.1) mm and 1.8 μm particle sizes. The mobile phase consisted of 35 mM ammonium formate pH 4.5 (solution A) and 0.02% formic acid in methanol (solution B) with gradient elution as mentioned time (min) % Solution B: 0/70, 0.5/50, 2/80, 6/95, 8/95, 8.2/70 and 10/70.The flow rate was at the rate of 0.4 ml/min and the detection wavelengths were 230nm. The column was maintained at 45°C and the injection volume was 2 μL. Stability of BH sample in different conditions was investigated by exposing the drug to stress study utilizing acid, base, oxidation, thermal, humidity and photolytic. The method was developed in two phases, screening and optimization. During the screening phase, the most suitable stationary phase, organic modifier, and pH were identified. The optimization was done for secondary influential parameters—column temperature, gradient time, and flow rate using fourteen experiments—to examine multifactorial effects of system suitability parameters and generated design space representing the robust region. A verification experiment was performed within the working design space and the model was considered to be accurate. There was no interference from excipients, impurities or degradation products at the retention time of BH for 4.0 min indicating the specificity of the method. The drug showed good stability under base, oxidation, thermal, humidity and photolytic conditions, but significant degradation was observed under acidic conditions. The procedure was validated for specificity, linearity, accuracy, precision and robustness. The degradation products were well resolved from BH and its impurities. The obtained LOD (Limit of detection) values are 0.004% to 0.01% and LOQ (Limit of quantification) values are 0.01% to 0.03% of impurities. A sensitive, rapid, specific and stability indicating gradient reverse phase UHPLC-PDA -PDA with MS (Orthogonal detectors) method for the determination of BH for the assay and OI was successfully developed with DOE. The present method is able to quantify BH and all potential impurities in a shorter (10 min) run time. DOE, statistically based experimental designs proved to be an important approach in optimizing selectivity-controlling parameters for the assay and OI determination in BH API and PF.The developed method was validated to be specific, linear, accurate, precise and robust. The peak purity and LC-MS test results confirmed that the BH peak was homogenous in all stress samples and the mass balance was found to be more than 99%, thus proving the stability indicating power of the method

Keywords: UHPLC-PDA and MS, Orthogonal Detectors, TGA, DOE (Design of Experiments), BH, Stress studies.


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