title: Development and validation of a liquid chromatographic method for the simultaneous determination of aniracetam and its related substances in the bulk drug and a tablet formulation.
abstract: Simultaneous determination of aniracetam and its related impurities (2-pyrrolidinone, p-anisic acid, 4-p-anisamidobutyric acid and (p-anisoyl)-4-methyl-2-pyrrolidinone) was accomplished in the bulk drug and in a tablet formulation using a high performance liquid chromatographic method with UV detection. Separation was achieved on a Hypersil BDS-CN column (150 mm × 4.0 mm, 5 μm) using a gradient elution program with solvent A composed of phosphate buffer (pH 4.0; 0.010 M) and solvent B of acetonitrile-phosphate buffer (pH 4.0; 0.010 M) (90:10, v/v). The flow rate of the mobile phase was 1.0 mL min(-1) and the total elution time, including the column re-equilibration, was approximately 20 min. The UV detection wavelength was varied appropriately among 210, 250 and 280 nm. Injection volume was 20 μL and experiments were conducted at ambient temperature. The developed method was validated in terms of system suitability, selectivity, linearity, range, precision, accuracy, limits of detection and quantification for the impurities, short term and long term stability of the analytes in the prepared solutions and robustness, following the ICH guidelines. Therefore, the proposed method was suitable for the simultaneous determination of aniracetam and its studied related impurities.
authors: Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Athens 15771, Greece.
authors: Georgios
authors: G
authors: Papandreou
authors: Kostas
authors: K
authors: Zorpas
authors: Helen
authors: H
authors: Archontaki
mesh_terms: D001549:Benzamides / Q000032:analysis / Q000737:chemistry; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods* / Q000592:standards; D004340:Drug Contamination; D062425:Hydroxybenzoate Ethers; D062385:Hydroxybenzoates / Q000032:analysis / Q000737:chemistry; D004364:Pharmaceutical Preparations / Q000032:analysis / Q000737:chemistry; D011760:Pyrrolidinones / Q000032:analysis* / Q000737:chemistry*; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet / Q000379:methods* / Q000592:standards; D013607:Tablets / Q000032:analysis / Q000737:chemistry
chemical_list: C112588:4-p-anisamidobutyric acid; D001549:Benzamides; D062425:Hydroxybenzoate Ethers; D062385:Hydroxybenzoates; D004364:Pharmaceutical Preparations; D011760:Pyrrolidinones; D013607:Tablets; C004520:4-anisic acid; C036466:aniracetam; C028537:2-pyrrolidone