Department of Quality Assurance, Maliba Pharmacy College, Maliba Campus, Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat 394 350, India.
Department of Chemistry and Biochemistry, Ohio University, Athens, OH 45701, USA.
J Chromatogr Sci. 2024 May 31;62(5):454-464. doi: 10.1093/chromsci/bmad057.
A green and robust high-performance thin-layer chromatographic method has been developed for the simultaneous estimation of sildenafil citrate and dapoxetine hydrochloride. A fractional factorial design was applied for analytical quality risk assessment of potential analytical risk factors. The identified critical analytical risk factors were optimized using the design of experiment-based response surface analysis by full factorial design. The analytical design space was navigated for the optimization of the method and the control strategy was framed for low-risk life-cycle management of the chromatographic method. The chromatographic analysis of sildenafil and dapoxetine was carried out on a TLC plate coated with silica gel G60 F254 using n-butanol:ethyl acetate:ethanol (8.0 + 2.0 + 0.5, v/v) as mobile phase. The chromatographic peaks of sildenafil and dapoxetine were found to be at Rf 0.29 and 0.69, respectively. The method was found to be accurate, precise, robust, specific and sensitive. The fixed-dose combinations of sildenafil and dapoxetine were assayed and results were found in compliance with their labeled claim. The present method was developed using safe and eco-friendly organic solvents for the safety of analysts and the protection of the environment. The greenness profiles of developed and reported methods were evaluated using the NEMI scale and AGREE software.
已开发出一种绿色、稳健的高效薄层色谱法，用于同时估算西地那非枸橼酸盐和达泊西汀盐酸盐。部分因子设计用于评估潜在分析风险因素的分析质量风险。通过全因子设计的实验设计响应面分析优化了确定的关键分析风险因素。为优化方法和制定控制策略进行了分析设计空间导航，用于色谱方法的低风险生命周期管理。西地那非和达泊西汀的色谱分析是在涂有硅胶 G60 F254 的 TLC 板上进行的，使用正丁醇：乙酸乙酯：乙醇（8.0+2.0+0.5，v/v）作为流动相。西地那非和达泊西汀的色谱峰分别在 Rf 0.29 和 0.69 处。该方法被发现准确、精密、稳健、特异和灵敏。对西地那非和达泊西汀的固定剂量组合进行了测定，结果符合其标签声称。本方法使用安全、环保的有机溶剂开发，以确保分析人员的安全和环境的保护。使用 NEMI 量表和 AGREE 软件评估了开发和报告方法的绿色度。
