School of Pharmaceutical Sciences, Lovely Professional University, Phagwara 144411, India.
Department of Pharmacology, Umm Alqura College of Pharmacy, Umm Alqura University, Makkah 21955, Saudi Arabia.
Molecules. 2023 Jan 4;28(2):472. doi: 10.3390/molecules28020472.
The analytical quality by design (AQbD) approach is utilized for developing and validating the simple, sensitive, cost-effective reverse-phase high performance liquid chromatographic method for the estimation of xanthohumol (XH) in bulk and nanoformulations. The Box-Behnken design (BBD) is applied for method optimization. The mobile phase ratio, pH and flow rate were selected as independent variables, whereas retention time, peak area, peak height, tailing factor, and theoretical plates were selected as dependent variables. The chromatogram of XH obtained under optimized conditions has given optimum conditions such as retention time (5.392 min), peak area (1,226,737 mAU), peak height (90,121 AU), tailing factor (0.991) and theoretical plates (4446.667), which are contoured in the predicted values shown by BBD. Validation of the method has been performed according to ICH Q2(R1) recommendations, using optimized conditions for linearity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, robustness and system suitability. All the values of validation parameters lie within the acceptable limits prescribed by ICH. Therefore, the developed and validated method of XH by the AQbD approach can be applied for the estimation of XH in bulk and various nanoformulations.
采用分析设计（AQbD）方法开发和验证了一种简单、灵敏、具有成本效益的反相高效液相色谱法，用于测定大黄素（XH）的含量。采用 Box-Behnken 设计（BBD）对方法进行优化。选择流动相比例、pH 值和流速为自变量，而保留时间、峰面积、峰高、拖尾因子和理论塔板数为因变量。在优化条件下得到的 XH 色谱图给出了最佳条件，如保留时间（5.392 分钟）、峰面积（1,226,737 mAU）、峰高（90,121 AU）、拖尾因子（0.991）和理论塔板数（4446.667），这些条件在 BBD 所示的预测值中得到了很好的体现。根据 ICH Q2(R1)的建议，采用优化条件对该方法进行了线性、检测限（LOD）和定量限（LOQ）、准确度、精密度、稳健性和系统适用性进行了验证。所有验证参数的值均在 ICH 规定的可接受范围内。因此，采用 AQbD 方法开发和验证的 XH 方法可用于测定大黄素的含量。
