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Environmental contamination is one of the most significant threats to living beings. The main source of contamination is anthropogenic activity, which generates many wastes with a high impact on ecosystems and human life. The monitoring of these toxic substances in the environment (water, soil, sediments, biota, and air) is of special importance to ensure the safety and adequate management of resources and wastes. The analytical methods require a previous sample preparation step in which target compounds are extracted and interferences are eliminated. Paradoxically, conventional sample preparation procedures are characterized by their low sustainability given the large amounts of toxic solvents and reagents required. In this sense, recent efforts have been shifted to the development of greener sample preparation strategies for the analysis of environmental samples following the Green Analytical Chemistry guidelines. This book chapter gives an overview of the advances in this field, with special attention to the use of microextraction techniques and alternative solvents and sorbents that replace traditional extraction phases, including deep eutectic solvents, supramolecular solvents, and natural sorbents, among others. Moreover, emphasis will be placed on strategies for which the greenness aspects have been evaluated.

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