Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Athens 15771, Greece.
J Pharm Biomed Anal. 2011 Nov 1;56(3):615-22. doi: 10.1016/j.jpba.2011.06.005. Epub 2011 Jun 16.
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.
采用高效液相色谱法（HPLC），结合紫外检测，建立了同时测定原料药及片剂中茴拉西坦及其相关杂质（2-吡咯烷酮、对茴香酸、4-对茴香酰胺基丁酸和（对茴香酰基）-4-甲基-2-吡咯烷酮）的方法。采用 Hypersil BDS-CN 柱（150mm×4.0mm，5μm），以磷酸盐缓冲液（pH4.0；0.010M）-乙腈-磷酸盐缓冲液（pH4.0；0.010M）（90:10，v/v）为流动相进行梯度洗脱，流速为 1.0mL/min，包括柱平衡在内的总洗脱时间约为 20min。紫外检测波长在 210nm、250nm 和 280nm 之间适当切换。进样量为 20μL，实验在室温下进行。根据 ICH 指南，对方法进行了系统适用性、选择性、线性、范围、精密度、准确度、杂质检测限和定量限、制剂溶液中分析物的短期和长期稳定性以及稳健性验证。因此，该方法适用于同时测定茴拉西坦及其研究相关杂质。
