Wrasse-Sangoi M, Sangoi M S, Oliveira P R, Secretti L T, Rolim C M B
Department of Industrial Pharmacy, Federal University of Santa Maria, 97105-900 Santa Maria-RS, Brazil.
J Chromatogr Sci. 2011 Feb;49(2):170-5. doi: 10.1093/chrsci/49.2.170.
A reversed-phase liquid chromatography (RP-LC) method is validated for the determination of aliskiren in tablet dosage form. The LC method is carried out on a Waters XBridge C(18) column (150 × 4.6 mm i.d.), maintained at 25°C. The mobile phase consisted of acetonitrile:water (95:5, v/v)/phosphoric acid (25 mM, pH 3.0) (40:60, v/v), run at a flow rate of 1.0 mL/min, with photodiode array detector set at 229 nm. The chromatographic separation is obtained with aliskiren retention time of 3.68 min, and it is linear in the range of 10-300 μg/mL (r = 0.9999). The limits of detection and quantitation are 2.38 and 7.93 μg/mL, respectively. The specificity and stability-indicating capability of the method are proven through degradation studies, which also showed that there is no interference of the formulation excipients, showing that peak is free from any coeluting peak. The method showed adequate precision, with a relative standard deviation (RSD) values lower than 0.92%. Good values of accuracy were also obtained, with a mean value of 99.55%. Experimental design is used during validation to calculate method robustness. The proposed method is applied for the analysis of the tablet dosage forms, contributing to improve the quality control and to assure the therapeutic efficacy.
已验证一种反相液相色谱（RP-LC）方法用于测定片剂剂型中的阿利吉仑。该液相色谱法在Waters XBridge C(18) 柱（内径150×4.6 mm）上进行，柱温保持在25°C。流动相由乙腈:水（95:5，v/v）/磷酸（25 mM，pH 3.0）（40:60，v/v）组成，流速为1.0 mL/min，光电二极管阵列检测器设置在229 nm。阿利吉仑的保留时间为3.68 min，实现了色谱分离，在10 - 300 μg/mL范围内呈线性（r = 0.9999）。检测限和定量限分别为2.38和7.93 μg/mL。通过降解研究证明了该方法的特异性和稳定性指示能力，研究还表明制剂辅料无干扰，即该峰无任何共洗脱峰。该方法显示出足够的精密度，相对标准偏差（RSD）值低于0.92%。准确度值也良好，平均值为99.55%。在验证过程中使用实验设计来计算方法的稳健性。所提出的方法用于片剂剂型的分析，有助于提高质量控制并确保治疗效果。
