Novel drug delivery systems (NDDS) are revolutionizing treatment by leveraging progressive technologies to deliver drugs precisely to their targets within the body. This targeted approach enhances therapeutic efficacy while minimizing unwanted side effects. This review delves into the various techniques employed for developing and characterizing NDDS. We focus on the critical role of characterization, encompassing both pre- and post-formulation stages. Pre-formulation techniques explored include physicochemical properties (melting point, solubility, etc.) spectroscopic analysis (UV, FTIR), thermal analysis (DSC, TGA), and powder characterization (XRD, polarized microscopy). In addition, post-formulation methods such as NMR spectrometry, atomic force microscopy, and in vitro drug release investigations are covered. By comprehensively characterizing these systems, researchers can optimize their design and formulation, ultimately leading to improved patient outcomes and encouraging improvements in the study and development of pharmaceuticals.