Profiling metabolites gives valuable insight into plant biology, food quality, pharmacokinetics, biochemical pathways involved in various matrices, and their potential therapeutic applications. Hence, profiling phenolic compounds is crucial because of their role in plant physiology, human health, nutrition, and disease prevention. There are two primary strategies for profiling phenolics: targeted and untargeted approaches. Targeted profiling focuses on the quantification and identification of specific and pre-selected phenolics, leveraging techniques such as liquid chromatography coupled with mass spectrometry (LC-MS) and high-performance liquid chromatography (HPLC). The approach is highly sensitive and precise but limited by the scope of predefined targets. In contrast, untargeted profiling aims to comprehensively capture all phenolics within a sample without prior knowledge of their identities. Advanced analytical techniques like ultra-high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (UHPLC-ESI-Q-TOF-MS) and nuclear magnetic resonance (NMR) spectroscopy are often employed. This method offers a broader perspective but comes with significant challenges, including data complexity, the need for sophisticated bioinformatics tools, and difficulty in identifying unknown compounds. Despite numerous studies on phenolic profiling, comprehensive case studies showcasing successful applications of both targeted and untargeted profiling, common challenges such as variability in phenolic composition due to environmental factors, the efficiency of extraction methods, and the stability of phenolic compounds are lacking. This chapter addresses these knowledge gaps while highlighting both the potential and prospects of these profiling techniques in enhancing agricultural practices, improving food quality control, and discovering new bioactive compounds for pharmaceutical development.