Perchlorate contamination in water due to industrial and space activities remains a serious problem as it seriously affects the function of thyroid glands. Various methods are being explored for the removal of perchlorate from the contaminated water. Among them, adsorption is a simple and cost-effective technique. The development of efficient adsorbent materials is the key to the success of the adsorption method of perchlorate removal. This thesis explores the synthesis of magnetically functionalized novel adsorbent materials from bio-waste such as eggshell and watermelon rind. Synthesis of N-doped activated carbon and Metal-Organic- Framework (MOF) based adsorbents are also explored. The perchlorate adsorption efficiency, adsorption mechanism, adsorption isotherm models, and adsorption kinetics are studied with the developed adsorbents. The regeneration of the spent adsorbents using suitable regents is also demonstrated for their reuse. The high perchlorate adsorption capacity of some of the adsorbents demonstrates their potential for practical applications.