ABSTRACT Recent concern about the impact of environmental preservation and the health of living beings has opened new avenues for scientific research. In this context, contemporary analytical chemistry has been marked by the development of green analytical methodologies, which aim to reduce the use of toxic reagents and minimize the environmental impact of analytical processes. Progress in this area involves the optimization of sample preparation techniques and the use of new functional materials, which contribute to a more sustainable and efficient analysis. Among these methodologies, miniaturized sample preparation techniques stand out, as they use smaller volumes of solvents and offer high sensitivity and selectivity. The use of advanced materials, such as molecularly imprinted polymers, MOFs, and conductive polymers, has driven innovation in analytical procedures regarding complex matrices, including environmental, food, and biological samples. These materials offer high selectivity and stability, improving efficiency in the extraction and detection of specific analytes. This review explores the integration of sustainable and green methodologies. It critically highlights applications and evaluates them using the Analytical Greenness Metric for Sample Preparation, based on publications from the past 6 years.