New pollutants, commonly referred to as emerging contaminants (ECs), are chemicals such as drugs and medicines, cosmetics and detergents, hormones and plastics, pesticides, and industrial products that have potentially disastrous impacts on water bodies and human health because of their ability to exist for long periods and accumulate in living organisms. It originates from irrigation and drain water from agricultural activities, industrial discharge effluents, and domestic sewage, many of which have no legal requirements set or minimal research data. ECs are identified at very low concentrations and are not easily retrievable; this makes analysis calibration and validation processes difficult since there are no reference materials available. This chapter discusses new detection techniques, such as HRMS, LC–MS, SPME, and SFE, for increasing the sensitivity and selectivity of the generated samples. Aptamer-based biosensors also reveal relatively high promise for real-time detection. As elaborated in the chapter, there must be consistent strategies to detect ECs and enhance analytical procedures that support measures to protect people and the environment.