This Reprint aims to cover all aspects of pharmaceutical analysis, including the latest developments and advances in the field. It will highlight the crucial role of analytical methods in assessing the quality of pharmaceutical products, ensuring that safe and effective drugs are released to the market. In the same context, the analytical techniques are necessary in determining pharmaceutical drugs. The design of experiments approach (DOE) is a reference point of systematic innovation. This powerful statistical tool goes beyond traditional experimentation, offering a structured approach to optimizing and validating analytical methodologies and stability testing. Additionally, it ensures the meticulous and accurate quantification of drug constituents, enhances product quality, and empowers data-driven decisions. In this Reprint, leading experts in the field share their insights, research findings and visions for the future, with a particular focus on quantitative and qualitative analyses involving sample preparation, analytical instrumentation and the application of multivariate statistical and chemometric tools in the analysis of pharmaceuticals and data processing. This contributes to increasing the interest in and renown of leaders in the field, as well as stimulating interdisciplinary discussions, as has been the tradition for many years. All new challenges and advances in pharmaceutical analysis must meet the highest quality standards.