Kumar Navneet, Sangeetha Dhanaraj, Reddy Pingili Sunil, Prakash Lakkireddy
Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500072, A.P., India.
Sci Pharm. 2012 Jan-Mar;80(1):153-65. doi: 10.3797/scipharm.1111-08. Epub 2011 Dec 12.
A novel, sensitive and selective stability-indicating gradient reverse phase ultra performance liquid chromatographic method was developed and validated for the quantitative determination of desloratadine and sodium benzoate in pharmaceutical oral liquid formulation. The chromatographic separation was achieved on Acquity BEH C8 (100 mm × 2.1 mm) 1.7 μm column by using mobile phase containing a gradient mixture of solvent A (0.05 M KH(2)PO(4) and 0.07 M triethylamine, pH 3.0) and B (50:25:25 v/v/v mixture of acetonitrile, methanol and water) at flow rate of 0.4 mL/min. Column temperature was maintained at 40°C and detection was carried out at a wavelength of 272 nm. The described method shows excellent linearity over a range of 0.254 μg/mL to 76.194 μg/mL for desloratadine and 1.006 μg/mL to 301.67 μg/mL for sodium benzoate. The correlation coefficient for desloratadine and sodium benzoate was more than 0.999. To establish stability-indicating capability of the method, drug product was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from desloratadine and sodium benzoate. The developed method was validated as per international ICH guidelines with respect to specificity, linearity, LOD, LOQ, accuracy, precision and robustness.
开发并验证了一种新颖、灵敏且具选择性的稳定性指示梯度反相超高效液相色谱法，用于定量测定药物口服液体制剂中的地氯雷他定和苯甲酸钠。采用Acquity BEH C8（100 mm×2.1 mm）1.7μm色谱柱进行色谱分离，流动相为溶剂A（0.05 M KH₂PO₄和0.07 M三乙胺，pH 3.0）与B（乙腈、甲醇和水的体积比为50:25:25的混合物）的梯度混合液，流速为0.4 mL/min。柱温保持在40°C，检测波长为272 nm。所描述的方法在0.254μg/mL至76.194μg/mL范围内，地氯雷他定线性良好；在1.006μg/mL至301.67μg/mL范围内，苯甲酸钠线性良好。地氯雷他定和苯甲酸钠的相关系数均大于0.999。为确定该方法的稳定性指示能力，对药品进行了酸、碱、氧化、水解、热和光解降解等加速试验。降解产物与地氯雷他定和苯甲酸钠能很好地分离。按照国际ICH指南，对所开发的方法在专属性、线性、检测限、定量限、准确度、精密度和稳健性等方面进行了验证。
