首页 | 本学科首页   官方微博 | 高级检索  
     检索      


Quality-by-design-based development and validation of a stability-indicating UPLC method for quantification of teriflunomide in the presence of degradation products and its application to in-vitro dissolution
Authors:Nukendra Prasad Nadella  Venkata Nadh Ratnakaram  N Srinivasu
Institution:1. Department of Science and Humanities, VFSTR, Vignan’s University, Guntur, Andhra Pradesh, India;2. Department of Analytical Research and Development, AET Laboratories Pvt Ltd, Hyderabad, Telangana, Indiaprasadnn14@gmail.com;4. Department of Chemistry, GITAM University, Bengaluru, Karnataka, India
Abstract:A systematic design-of-experiments was performed by applying quality-by-design concepts to determine design space for rapid quantification of teriflunomide by the ultraperformance liquid chromatography (UPLC) method in the presence of degradation products. Response surface and central composite quadratic were used for statistical evaluation of experimental data using a Design-Expert software. The response variables such as resolution, retention time, and peak tailing were analyzed statistically for the screening of suitable chromatographic conditions. During this process, various plots such as perturbation, contour, 3D, and design space were studied. The method was developed through UPLC BEH C18 2.1?×?100?mm, 1.7-µ column, mobile phase comprised of buffer (5?mM K2HPO4 containing 0.1% triethylamine, pH 6.8), and acetonitrile (40:60 v/v), the flow rate of 0.5?mL?min?1 and UV detection at 250?nm. The method was developed with a short run time of 1?min. Forced degradation studies revealed that the method was stability-indicating, suitable for both assay and in-vitro dissolution of a drug product. The method was found to be linear in the range of 28–84?µg?mL?1, 2.8–22.7?µg?mL?1 with a correlation coefficient of 0.9999 and 1.000 for assay and dissolution, respectively. The recovery values were found in the range of 100.1–101.7%. The method was validated according to ICH guidelines.
Keywords:Assay and in-vitro dissolution  design of experiments  method validation  stability-indicating  teriflunomide  UPLC
设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号