Abstract
A new, specific, rapid and stability indicating reversed phase liquid chro-matographic (RP-LC) method for the determination of process related and degradation related impurities of Apremilast has been developed and validated. The degradation study performed in acid, base, oxidative, photolytic, and thermal stressed conditions. Eight process related impurities (Imp-1 to Imp-8) in test sample of Apremilast have been detected by developed RP-LC method. The good chromatographic resolution between the peaks of process related impurities, degradation impurities and Apremilast has been achieved on a Synergi Max-RP 80 A (150 × 4.6 mm ID), 4 μ column. The process and degradation related impurities were characterized by mass spectrometry, 1H NMR and FT-IR spectral data. The method was validated as per ICH guideline and found to be specific, rapid, and stability indicating. The proposed RP-PLC method was successfully applied to the analysis of drug substance samples of Apremilast.
Highlights
IntroductionApremilast is a novel, oral small-molecule inhibitor of phosphodiesterase 4 (PDE4) that works intracellularly to modulate a network of pro- and anti-in-
This paper presents a rapid, specific, precise, accurate and stability indicating gradient reversed phase liquid chromatographic (RP-LC) method that separates the related substances and degradation products of Apremilast with good resolution
The process and degradation related impurities present in Apremilast sample were identified by LC-Mass Spectrometry (MS) and characterized by using MS, Fourier Transform Infrared Spectroscopy (FT-IR) and 1HNMR spectral data
Summary
Apremilast is a novel, oral small-molecule inhibitor of phosphodiesterase 4 (PDE4) that works intracellularly to modulate a network of pro- and anti-in-. The proinflammatory mediators that are up regulated in PsA include the cytokines TNF-α, IL-1, IL-6, and IL-8, and the chemokines monocyte chemotactic protein-1 (MCP-1) and macrophage inflammatory protein-1 beta (MIP-1β) (CC-10004-PSA-002-PD) Based on these effects, Apremilast is being developed for use in the treatment of various immune-mediated inflammatory conditions such as psoriasis, PsA, rheumatoid arthritis (RA), Behçet disease (BD), and ankylosing spondylitis (AS). As per our knowledge there is no method reported for the determination of process related and degradation related impurities of Apremilast in drug substance and drug product by using HPLC for regular analysis and stability study analysis in QC laboratory. The core-objective of this research work was to develop a specific and robust stability-indicating RP-LC method for the determination of process and degradation related impurities of Apremilast and its analytical validation. The developed method was successfully validated according to the USP Validation of Compendial Procedures and ICH Q2 (R1) guidelines [15] [16]
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