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A New Strategy for the Software-Assisted LC Separations of Ketoconazole and Its Impurities
Journal of Chromatographic Science ( IF 1.5 ) Pub Date : 2022-06-24 , DOI: 10.1093/chromsci/bmac049
Roopali Agrawal 1 , Sateesh Belemkar 1 , Chandrakant Bonde 2
Affiliation  

Analytical quality by design and the use of dissimilar chromatographic systems can be employed to accelerate chromatographic separations. Herein, a software (S-Matrix)-assisted platform was used to proficiently screen, optimize and select the optimal parameters for the chromatographic separation of ketoconazole and its related impurities. This approach evaluated the various chromatographic parameters in a stepwise manner based on the statistical tools and provided an in-depth understanding of the critical parameters influencing the peak selectivities and separations. It was demonstrated that dissimilar conditions, such as different stationary phases, mobile phase pH and organic modifiers (i.e., critical method variables), can improve the peak resolution, while the critical quality attributes can provide conditions appropriate for quantification purposes via a quality target analytical method. Furthermore, an orthogonal method was established to support the primary method. The orthogonality between the two methods was defined by the correlation matrix between the two systems using the Pearson correlation coefficient and was found to be 0.12. Using the optimized method, the primary method was validated as per International Council for Harmonization in the range of 0.05–1.0% for impurities and 80.0–120.0% for ketoconazole, thereby indicating the suitability of the method for use in quality control laboratories.

中文翻译:

软件辅助液相色谱分离酮康唑及其杂质的新策略

分析质量的设计和不同色谱系统的使用可用于加速色谱分离。本文利用软件(S-Matrix)辅助平台对酮康唑及其相关杂质的色谱分离进行了熟练的筛选、优化和选择最佳参数。该方法基于统计工具逐步评估各种色谱参数,并深入了解影响峰选择性和分离的关键参数。结果表明,不同的条件,例如不同的固定相、流动相 pH 值和有机改性剂(即关键方法变量),可以提高峰分辨率,而关键质量属性可以通过质量目标分析方法提供适合量化目的的条件。此外,还建立了一种正交方法来支持主要方法。两种方法之间的正交性由使用 Pearson 相关系数的两个系统之间的相关矩阵定义,发现为 0.12。使用优化方法,主要方法根据国际协调委员会在 0.05–1.0% 的杂质范围和 80.0–120.0% 的酮康唑范围内进行了验证,从而表明该方法适用于质量控制实验室。两种方法之间的正交性由使用 Pearson 相关系数的两个系统之间的相关矩阵定义,发现为 0.12。使用优化方法,主要方法根据国际协调委员会在 0.05–1.0% 的杂质范围和 80.0–120.0% 的酮康唑范围内进行了验证,从而表明该方法适用于质量控制实验室。两种方法之间的正交性由使用 Pearson 相关系数的两个系统之间的相关矩阵定义,发现为 0.12。使用优化方法,主要方法根据国际协调委员会在 0.05–1.0% 的杂质范围和 80.0–120.0% 的酮康唑范围内进行了验证,从而表明该方法适用于质量控制实验室。
更新日期:2022-06-24
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