Pharmaceuticals are subject to analysis in various settings: as raw material, pharmaceutical formulation, as a drug in the biological fluids with its metabolites, and as a drug released to the environment. Emerging separation techniques have played a crucial role in the development and progress of pharmaceuticals. These techniques play an important role in the different stages of drug development: synthesis, purification, formulation, quality control, toxicological, and pharmacokinetic studies.

The need for separation techniques that are reproducible, high throughput, readily available, and easily implemented is important to ascertain the quality and the quantity of drug molecules. These separation techniques allow analysis of drugs either alone or with other drugs, impurities, related substances, and metabolites or any other interferences in different simple or complex matrices: pharmaceuticals, biological, and environmental samples. The most widely used separation technique is high-performance liquid chromatography (HPLC). Although it is an old separation technique, it has many new advanced applications. Similarly, capillary electrophoresis (CE) with its different modes showed great enhancement in drug analysis especially the emerged technique “capillary electro-chromatography”. Liquid chromatography (LC) and CE hyphenated techniques with mass spectrometry (MS) and tandem mass spectrometry (MS/MS) are widely applied for drug analysis especially in complex matrices with many unknown interferences and small samples volume. They have shown great advantages in results interpretation especially with their ability to identify foreign peaks and explain mechanisms of drug degradation. The enentioseparation of chiral drugs is recommended by many organizations such as the FDA and ICH. The guidelines recommend considering the inactive enantiomer as an impurity, so it is important for chiral drugs to apply enantioseparation techniques for the separation and the analysis of enantiomers and their racemic mixture. Thin layer chromatography, especially high-performance thin-layer chromatography (HPTLC) technique, is still used in drug analysis due to its simplicity and cost effectiveness.

The aim of this Special Issue is to collate original research and review articles in this field.

Potential topics include but are not limited to the following:

• Capillary electrophoresis
• Chiral separation and application of nanomaterials
• Hydrophilic interaction liquid chromatography (HILIC) methods in pharmaceutical analysis
• Advances in preparation of monolithic columns
• Green methodology of choosing mobile phase
• Development of solid-phase extraction technique for biological samples pre-treatment
• Separation technique for monitoring of pharmaceuticals