R. Shedafa, P. Tibalinda, V. Manyanga, J. Sempombe, E. Kaale, C. Bonsmann, C. Haefelé, M. Chambuso
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引用次数: 2
摘要
本研究描述了一种稳定性高的高效液相色谱分析拉米夫定和富马酸替诺福韦二氧吡酯及其降解物的方法的建立和验证。方法采用resil®-pur碱性C18色谱柱(250 mm × 4.6 mm, 5 μm),在30°C下保持,甲醇和缓冲液(2.3 g/L磷酸二氢铵和1.32 g/L磷酸氢二铵,pH 3.9)的混合物,梯度洗脱,流速1.0 mL/min, 270 nm紫外检测。对拉米夫定和富马酸替诺福韦二氧吡酯及其潜在杂质进行了较好的分离。将两种有效成分分别置于水解和氧化应激条件下,并将降解产物从各自的完整药物中分离出来,验证了所开发方法的稳定性和能力。两种有效成分在80 ~ 120 μg/mL浓度范围内均呈线性,r2> 0.99。拉米夫定的回收率为99.8%,富马酸替诺福韦二氧吡酯的回收率为99.3%,证实了该方法同时测定两种药物固定剂量组合的准确性。关键词:稳定性指示液相色谱,拉米夫定,替诺福韦,验证
Stability Indicating Liquid Chromatographic Method for Determination of Lamivudine and Tenofovir Disoproxil Fumarate in Fixed Dose Combination Formulations
This study describes the development and validation of a stability indicating high performance liquid chromatographic method for the analysis of lamivudine and tenofovir disoproxil fumarate and their degradants. The method uses a Reprosil®-pur basic C18 column (250 mm × 4.6 mm, 5 μm) maintained at 30°C, methanol and a mixture of buffers (2.3 g/L ammonium dihydrogen phosphate and 1.32 g/L of diammonium hydrogen phosphate, pH 3.9) for gradient elution at a flow rate of 1.0 mL/min, and UV detection at 270 nm. Good separation of lamivudine and tenofovir disoproxil fumarate and their potential impurities was achieved. The stability indicating ability of the developed method was validated by subjecting both active ingredients to hydrolytic and oxidative stress conditions and separating the degradation products from their respective intact drugs. The calibration curve was linear over the 80-120 μg/mL concentration range for both active ingredients with r2> 0.99. A recovery rate of 99.8 % for lamivudine and 99.3 % for tenofovir disoproxil fumarate confirmed the accuracy of the method for the simultaneous determination of both drugs in the fixed-dose combination.Keywords: Stability indicating liquid chromatography, lamivudine, tenofovir, validation