Dr Reddy's Laboratories Ltd, Active Pharmaceutical Ingredients, IPDO, Bachupally, Hyderabad 500072, AP, India.
J Pharm Biomed Anal. 2010 Nov 2;53(3):483-9. doi: 10.1016/j.jpba.2010.05.022.
A simple, precise, accurate stability-indicating gradient reverse phase ultra-performance liquid chromatographic (RP-UPLC) method was developed for the quantitative determination of purity of Valsartan drug substance and drug products in bulk samples and pharmaceutical dosage forms in the presence of its impurities and degradation products. The method was developed using Waters Aquity BEH C18 (100 mm x 2.1 mm, 1.7 microm) column with mobile phase containing a gradient mixture of solvents A and B. The eluted compounds were monitored at 225 nm, the run time was within 9.5 min, which Valsartan and its seven impurities were well separated. Valsartan was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Valsartan was found to degrade significantly in acid and oxidative stress conditions and stable in base, hydrolytic and photolytic degradation conditions. The degradation products were well resolved from main peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per international conference on harmonization (ICH) guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of Valsartan in pharmaceutical dosage forms.
建立了一种简单、准确、精确的稳定性指示梯度反相超高效液相色谱（RP-UPLC）方法，用于定量测定缬沙坦原料药和制剂在杂质和降解产物存在下的纯度。该方法采用 Waters Aquity BEH C18（100mm×2.1mm，1.7μm）柱，以溶剂 A 和 B 的梯度混合物作为流动相。在 225nm 处监测洗脱化合物，运行时间在 9.5min 内，缬沙坦及其七种杂质得到了很好的分离。缬沙坦经受了氧化、酸、碱、水解、热和光降解的应力条件。发现缬沙坦在酸和氧化应激条件下显著降解，在碱、水解和光降解条件下稳定。降解产物与主峰及其杂质得到很好的分离，证明了该方法的稳定性指示能力。该方法按照国际协调会议（ICH）指南进行了专属性、线性、检测限、定量限、准确度、精密度和稳定性验证。该方法也适用于药物制剂中缬沙坦的含量测定。
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