This review is devoted to analytical methods published in the scientific literature in the last 10 years for the determination of emerging contaminants in aquatic media. The article is mainly focused on sample preparation and on instrumental techniques most used for the detection and quantification of the analytes of interest. The sample preparation techniques include classical liquid-liquid extraction and solid-phase extraction, but also recent microextraction techniques such as solid-phase microextraction, stir-bar sorptive extraction, dispersive liquid-liquid microextraction, ultrasound-assisted emulsification microextraction, or microextraction by packed sorbent. Most studies focus on minimizing the number of analysis steps and on the use of the lowest amount of solvents in the sample treatment step. Liquid chromatography and gas chromatography mainly coupled to tandem mass spectrometry are usually the employed analytical techniques. A large number of multiresidue methods are being developed for the determination of several families of these compounds with only one extraction step to minimize sample handling and treatment.