eng Oriental Scientific Publishing Company Biosciences Biotechnology Research Asia 0973-1245 2026-03-30 23 1 367 374 10.13005/bbra/3504 58338 article Kavita Bhushan Vikhe 1 Sandeep Suresh Sonawane 1 Department of Pharmaceutical Chemistry, MET’s Institute of Pharmacy, Savitribai Phule Pune University, Maharashtra, India By permitting the simultaneous separation, identification, and quantification of complex mixtures, hyphenated analytical techniques—combinations of chromatographic separation with spectroscopic or spectrometric detection—have revolutionized contemporary pharmaceutical analysis. Drug discovery, impurity profiling, bioanalysis, and quality control have all seen a rise in the use of techniques including LC-MS, GC-MS, LC-NMR, CE-MS, and SFC-MS within the past 20 years. This review critically assesses their analytical performance, limitations, and recent advances, such as miniaturized systems, green chemistry techniques, and AI-driven data processing, whereas the literature currently in publication emphasizes their instrumental configurations and routine applications. In addition to improving existing pharmaceutical workflows, these developments are opening the door for future integration with biologics, nanomedicine, and precision medicine. Views on cost-effective instrumentation, regulatory harmonization, and the changing role of hyphenated technologies in shaping. The article concludes with perspectives on regulatory harmonization, cost-effective instrumentation, and the evolving role of hyphenated technologies in shaping sustainable and personalized healthcare solutions. https://www.biotech-asia.org/vol23no1/hyphenated-techniques-in-drug-discovery-and-quality-control-from-fundamentals-to-future-perspectives/ Drug Discovery; Hyphenated Techniques; Impurity Profiling; LC–MS; Pharmaceutical Analysis; Quality Control