The disinfection of drinking water is an integral component of water treatment in large volume, provides hygienically safe drinking water, and very essential worldwide. The interaction between the disinfectant agents and different dissolved components in water resultant in the formation of chemical substances categorized as disinfection by-products. The exposure to disinfection by-products and their potential toxic effects causes the occurrence of hazardous effects on human health. The levels of disinfection by-products in the drinking water strictly regulated due to their toxicity effects. This chapter is devoted to review, in brief, the recent reports on the various disinfection by-products and their associated toxicity effects. Furthermore, the approach of identification followed with controlling the disinfection by-products through different methods covering the broad aspects of conventional and recent ones will be covered.