This paper includes the development of a novel, systematic, quality by design (QbD)-based high-performance thin-layer chromatography (HPTLC) method for the simultaneous estimation of torsemide and eplerenone. Chromatographic separation was carried out on aluminum-backed silica gel 60 F254 plates using toluene–ethyl acetate–glacial acetic acid (7:3:0.1, V/V) as the mobile phase. UV detection was carried out at 297 nm for torsemide and 247 nm for eplerenone. A 3-factor 17-run regular 3-level factorial design was applied to factor screening studies, and Box-Behnken design was utilized for optimization of the experimental parameters of HPTLC for obtaining anticipated chromatographic conditions. Risk assessment was executed to understand the basic method parameters. From the risk assessment, 3 independent parameters, such as band length, saturation time, and wavelength, were selected and studied for the impact of these 3 parameters on the responses. The method yields compact and well-resolved band at RF = 0.24 ± 0.02 for torsemide and RF = 0.50 ± 0.02 for eplerenone. In the linear regression analysis carried out for torsemide and eplerenone, the regression coefficient was found to be r2 = 0.999 for torsemide and r2 =0.995 for eplerenone. The method was validated for validation parameters like accuracy, precision, robustness, limit of detection, and limit of quantification as per the International Conference on Harmonization (ICH) guidelines.

中文翻译：

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设计方法同时测定托塞米德和依普利农的高效薄层色谱方法的开发和验证

本文包括开发一种基于设计（QbD）的新颖，系统，高质量的高性能薄层色谱（HPTLC）方法，用于同时估算托塞米德和依普利农。色谱分离是在铝制硅胶60 F254板上，使用甲苯-乙酸​​乙酯-冰醋酸（7：3：0.1，V / V）作为流动相。托拉塞米在297 nm处进行紫外检测，对于依普利农在247 nm处进行UV检测。将3因子17次运行的常规3阶因子设计应用于因子筛选研究，Box-Behnken设计用于优化HPTLC的实验参数以获得预期的色谱条件。执行风险评估以了解基本方法参数。从风险评估中，选择了3个独立的参数，例如带宽，饱和时间和波长，并研究了这3个参数对响应的影响。对于托拉塞米和R，该方法在R F = 0.24±0.02时产生紧凑且分辨良好的谱带依匹乐酮F = 0.50±0.02。在对托拉塞米和依普利农进行的线性回归分析中，托拉塞米的回归系数为r 2 = 0.999 ，依普利农的回归系数为r 2 = 0.995。根据国际协调会议（ICH）指南，对方法的准确性，准确性，鲁棒性，检测极限和定量极限等验证参数进行了验证。