Citrus peel waste, a major by-product of citrus fruit processing, is an abundant source of pectin, a polysaccharide with significant industrial value due to its gelling, stabilizing, and emulsifying properties. This chapter explores methodologies for extracting, quantifying, and characterizing pectin, focusing on sustainability and maximizing economic efficiency. Various approaches are discussed in detail, including gravimetric, titrimetric, colorimetric, and spectrophotometric methods. Advanced techniques like FTIR and HPLC provide precise insights into pectin’s structural and functional attributes. Protocols such as alcohol precipitation, calcium pectate precipitation, and carbazole assays are evaluated for their accuracy, efficiency, and reproducibility. By comparing the strengths and limitations of different methods, this chapter provides a valuable resource for researchers and industry professionals to estimate pectin in a constructive and precise manner. It emphasizes the potential of citrus peel waste as a sustainable, high-value ingredient, contributing to environmental conservation and economic sustainability.