Alkaloids, a diverse group of naturally occurring compounds primarily found in plants, possess significant pharmacological properties and are of considerable interest in the fields of medicine, nutraceuticals, and biochemistry. This chapter focuses on the extraction and quantification of these alkaloid classes, emphasizing the methods tailored for their efficient extraction from plant matrices. Various extraction techniques, ranging from traditional methods like maceration, percolation, and Soxhlet extraction to modern approaches such as microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE) were discussed. These methods are compared in terms of efficiency, solvent consumption, extraction time, and their applicability to different alkaloid classes. Different methods of quantification including UV-VIS spectroscopy, HPLC and iodometric back titration analysis was discussed with their principle and detailed procedure.