Department of Pharmaceutical Quality Assurance, B.K. Mody Government Pharmacy College, Polytechnic campus, Near Aji dam, Rajkot, 360003, Gujarat, India.
Department of Pharmaceutical Quality Assurance, B.K. Mody Government Pharmacy College, Polytechnic campus, Near Aji dam, Rajkot, 360003, Gujarat, India.
Ann Pharm Fr. 2024 May;82(3):464-472. doi: 10.1016/j.pharma.2023.10.006. Epub 2023 Oct 20.
High Performance liquid chromatography is an integral analytical tool in assessing drug product stability. A simple, selective, precise, accurate and stability indicating RP-HPLC method was developed and validated for analysis of Tadalafil and Macitentan in synthetic mixture.
Chromatographic separation was performed using Phenomex Gemini C18 (25cm×4.6nm, 5μm) Column. The mobile phase consists of (10mM Ammonium Acetate in water and [Methanol: ACN 20: 80% v/v]) (40: 60% v/v). The flow rate was set to be 1.0mL/min. The injection volume was 10.00μL. The detection was carried out at 260nm at column temperature 35°C.
The method was validating according to ICH QR guideline for accuracy, precision, reproducibility, specificity, robustness and detection and quantification limits. Stability testing was performed on Tadalafil and Macitentan and it was found that these degraded sufficiently in all applied chemical and physical conditions. Linearity for Tadalafil and Macitentan was observed 0.4-100μg/mL and 0.1-25μg/mL with correlation coefficient at 0.9999. LOD and LOQ 0.008μg/mL and 0.024μg/mL and 0.001μg/mL and 0.0029μg/mL for Tadalafil and Macitentan respectively.
The developed RP-HPLC method was found to be suitable for the determination of both the drugs.
高效液相色谱法是评估药物产品稳定性的不可或缺的分析工具。本研究开发并验证了一种简单、选择性强、精密、准确且能显示稳定性的反相高效液相色谱法，用于分析合成混合物中的他达拉非和马昔腾坦。
采用 Phenomex Gemini C18（25cm×4.6nm，5μm）柱进行色谱分离。流动相由（水中 10mM 乙酸铵和[甲醇：乙腈 20：80% v/v]）（40：60% v/v）组成。流速设定为 1.0mL/min。进样量为 10.00μL。检测波长为 260nm，柱温为 35°C。
该方法符合 ICH QR 指导原则的准确性、精密度、重现性、专属性、稳健性以及检测限和定量限的要求。对他达拉非和马昔腾坦进行了稳定性测试，结果发现它们在所有应用的化学和物理条件下都有足够的降解。他达拉非和马昔腾坦的线性范围分别为 0.4-100μg/mL 和 0.1-25μg/mL，相关系数均为 0.9999。他达拉非和马昔腾坦的检测限和定量限分别为 0.008μg/mL 和 0.024μg/mL，以及 0.001μg/mL 和 0.0029μg/mL。
所开发的反相高效液相色谱法被证明适用于两种药物的测定。
