title: Force degradation behavior of glucocorticoid deflazacort by UPLC: isolation, identification and characterization of degradant by FTIR, NMR and mass analysis.
abstract: In this investigation, sensitive and reproducible methods are described for quantitative determination of deflazacort in the presence of its degradation product. The method was based on high performance liquid chromatography of the drug from its degradation product on reverse phase using Acquity UPLC BEH C18 columns (1.7 µm, 2.1 mm × 150 mm) using acetonitrile and water (40:60 V/V) at a flow rate of 0.2 mL/minute in UPLC. UV detection was performed at 240.1 nm. Deflazacort was subjected to oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The drug was found to be stable in water and thermal stress, as well as under neutral stress conditions. However, forced-degradation study performed on deflazacort showed that the drug degraded under alkaline, acid and photolytic stress. The degradation products were well resolved from the main peak, which proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to accuracy, linearity, limit of detection, limit of quantification, accuracy, precision and robustness, selectivity and specificity. Apart from the aforementioned, the results of the present study also emphasize the importance of isolation characterization and identification of degradant. Hence, an attempt was made to identify the degradants in deflazacort. One of the degradation products of deflazacort was isolated and identified by the FTIR, NMR and LC-MS study.
authors.affiliation: Macleods Pharmaceuticals Ltd., Kachigam, Daman, 396320, India.
authors.forename: Rajesh
authors.initials: R
authors.lastname: Deshmukh
authors.affiliation: School of Pharmaceutical Science, Rajiv Gandhi Prodyogiki Vishwavidyalaya, Gandhi Nagar, Bhopal 462036, India.
authors.forename: Lata
authors.initials: L
authors.lastname: Sharma
authors.affiliation: TIT College of Pharmacy, Technocrats Institute of Technology, Anand Nagar, Bhopal 462021, India.
authors.forename: Muktika
authors.initials: M
authors.lastname: Tekade
authors.affiliation: Department of Pharmaceutical Sciences, Eugene Applebaum College of Pharmacy and Health Sciences, Wayne State University, Detroit, MI 48201, USA.
authors.forename: Prashant
authors.initials: P
authors.lastname: Kesharwani
authors.affiliation: School of Pharmaceutical Science, Rajiv Gandhi Prodyogiki Vishwavidyalaya, Gandhi Nagar, Bhopal 462036, India.
authors.forename: Piyush
authors.initials: P
authors.lastname: Trivedi
authors.affiliation: The University of Texas Southwestern Medical Center, Advanced Imaging Research Center, Dallas, TX 75390, USA.|The International Medical University, School of Pharmacy, Department of Pharmaceutical Technology, Kuala Lumpur, 57000, Malaysia; rakeshtekade@gmail.com and rakeshtekade@yahoo.com.
authors.forename: Rakesh K
authors.initials: RK
authors.lastname: Tekade
keywords: Deflazacort; characterization; degradant; forced degradation