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The analysis of emerging contaminants (ECs) remains a dynamic and challenging field because this involves analyzing chemicals with widely varying properties in a large variety of environmental matrices. Usually, concentration levels of ECs are particularly low, such that sensitive and selective analytical methods are required for their analysis. This chapter focuses on five classes of ECs (pharmaceuticals and personal care products, disinfection by-products, perfluorinated compounds, polybrominated diphenyl ethers, and benzotriazoles and dioxane [B and D]) in terms of their occurrence and level of detection. It also highlights the rule of regulatory agencies on the EC detection limit. Sampling techniques used to detect ECs in different environmental matrices are discussed, such as (1) water grab samples from inland and offshore; (2) large-volume solid-phase extraction for water samples; (3) passive samplers (Polar Organic Chemical Integrative Sampler, Chemcatcher, Altesil SR sheet, and semipermeable membrane devices); (4) sediment grab samples (Van Veen and gravity-free fall corer); (5) biota grab samples with different trophic levels (sediment microorganisms, mussels, fish, and mammals; and (6) air passive samplers (inland and/or offshore). In addition, the latest progress is reviewed in sample preparation, extraction, and cleanup.