The identification of WADA-prohibited diuretics in sports drinks and energy powder supplements is essential to anti-doping activities. The purpose of this thesis is to create a robust analytical method for extracting and quantifying these illegal chemicals using Liquid Chromatography-Mass Spectrometry (LC-MS) in conjunction with liquid-liquid extraction (LLE). The study assesses the efficacy of LLE approaches for separating target diuretics from complicated dietary supplement matrices, including the use of switchable hydrophilicity solvents (SHS) and salt-assisted liquid-liquid extraction (SALLE). The approach is designed to produce high extraction efficiencies and sensitive detection, allowing for the accurate identification and quantification of even trace quantities of forbidden diuretics that may be present due to contamination or unreported inclusion. This thorough analytical technique provides a vital tool for anti-doping laboratories and regulatory bodies to monitor the quality and safety of sports-related dietary supplements, thereby maintaining the integrity of athletic competition.