Kadi Adnan A, Mohamed Mostafa S, Kassem Mohamed G, Darwish Ibrahim A
Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P,O, Box 2457, Riyadh 11451, Saudi Arabia.
Chem Cent J. 2011 Jun 14;5:30. doi: 10.1186/1752-153X-5-30.
A simple, sensitive and accurate stability-indicating HPLC method has been developed and validated for determination of varenicline (VRC) in its bulk form and pharmaceutical tablets. Chromatographic separation was achieved on a Zorbax Eclipse XDB-C8 column (150 mm × 4.6 mm i.d., particle size 5 μm, maintained at ambient temperature) by a mobile phase consisted of acetonitrile and 50 mM potassium dihydrogen phosphate buffer (10:90, v/v) with apparent pH of 3.5 ± 0.1 and a flow rate of 1.0 ml/min. The detection wavelength was set at 235 nm. VRC was subjected to different accelerated stress conditions. The degradation products, when any, were well resolved from the pure drug with significantly different retention time values. The method was linear (r = 0.9998) at a concentration range of 2 - 14 μg/ml. The limit of detection and limit of quantitation were 0.38 and 1.11 μg/ml, respectively. The intra- and inter-assay precisions were satisfactory; the relative standard deviations did not exceed 2%. The accuracy of the method was proved; the mean recovery of VRC was 100.10 ± 1.08%. The proposed method has high throughput as the analysis involved short run-time (~ 6 min). The method met the ICH/FDA regulatory requirements. The proposed method was successfully applied for the determination of VRC in bulk and tablets with acceptable accuracy and precisions; the label claim percentages were 99.65 ± 0.32%. The results demonstrated that the method would have a great value when applied in quality control and stability studies for VRC.
已开发并验证了一种简单、灵敏且准确的稳定性指示高效液相色谱法，用于测定伐尼克兰（VRC）原料药及其药物片剂。采用Zorbax Eclipse XDB-C8色谱柱（150 mm×4.6 mm内径，粒径5μm，室温下操作）进行色谱分离，流动相由乙腈和50 mM磷酸二氢钾缓冲液（10:90，v/v）组成，表观pH值为3.5±0.1，流速为1.0 ml/min。检测波长设定为235 nm。VRC经历了不同的加速应力条件。如有降解产物，其与纯药物能得到很好的分离，保留时间值有显著差异。该方法在2 - 14μg/ml浓度范围内呈线性（r = 0.9998）。检测限和定量限分别为0.38和1.11μg/ml。批内和批间精密度令人满意；相对标准偏差不超过2%。该方法的准确性得到了验证；VRC的平均回收率为100.10±1.08%。由于分析运行时间短（约6分钟），所提出的方法具有高通量。该方法符合ICH/FDA监管要求。所提出的方法已成功应用于测定VRC原料药和片剂，准确度和精密度均可接受；标示量百分比为99.65±0.32%。结果表明，该方法应用于VRC的质量控制和稳定性研究时具有很大价值。
