Advances in the area of sample preparation are significant and have been growing significantly in recent years. This initial step of the analysis is essential and must be carried out properly, consisting of a complicated procedure with multiple stages. Consequently, it corresponds to a potential source of errors and will determine, at the end of the process, either a satisfactory result or a fail. One of the advances in this field includes the miniaturization of extraction techniques based on the conventional sample preparation procedures such as liquid‐liquid extraction and solid‐phase extraction. These modern techniques have gained prominence in the face of traditional methods since they minimize the consumption of organic solvents and the sample volume. As another feature, it is possible to reuse the sorbents, and its coupling to chromatographic systems might be automated. The review will emphasize the main techniques based on liquid‐phase microextraction, as well as those based upon the use of sorbents. The first group includes currently popular techniques such as single drop microextraction, hollow fiber liquid‐phase microextraction, and dispersive liquid‐liquid microextraction. In the second group, solid‐phase microextraction techniques such as in‐tube solid‐phase microextraction, stir bar sorptive extraction, dispersive solid‐phase extraction, dispersive micro solid‐phase microextraction, and microextraction by packed sorbent are highlighted. These approaches, in common, aim the determination of analytes at low concentrations in complex matrices. This article describes some characteristics, recent advances, and trends on miniaturized sample preparation techniques, as well as their current applications in food, environmental, and bioanalysis fields.

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Since its discovery in 2004 by Novoselov et al., graphene has attracted increasing attention in the scientific community due to its excellent physical and chemical properties, such as thermal/mechanical resistance, electronic stability, high Young's modulus, and fast mobility of charged atoms. In addition, other remarkable characteristics support its use in analytical chemistry, especially as sorbent. For these reasons, graphene-based materials (GBMs) have been used as a promising material in sample preparation. Graphene and graphene oxide, owing to their excellent physical and chemical properties as a large surface area, good mechanical strength, thermal stability, and delocalized π-electrons, are ideal sorbents, especially for molecules containing aromatic rings. They have been used in several sample preparation techniques such as solid-phase extraction (SPE), stir bar sorptive extraction (SBSE), magnetic solid-phase extraction (MSPE), as well as in miniaturized modes as solid-phase microextraction (SPME) in their different configurations. However, the reduced size and weight of graphene sheets can limit their use since they commonly aggregate to each other, causing clogging in high-pressure extractive devices. One way to overcome it and other drawbacks consists of covalently attaching the graphene sheets to support materials (e.g., silica, polymers, and magnetically modified supports). Also, graphene-based materials can be further chemically modified to favor some interactions with specific analytes, resulting in more efficient hybrid sorbents with higher selectivity for specific chemical classes. As a result of this wide variety of graphene-based sorbents, several studies have shown the current potential of applying GBMs in different fields such as food, biological, pharmaceutical, and environmental applications. Within such a context, this review will focus on the last five years of achievements in graphene-based materials for sample preparation techniques highlighting their synthesis, chemical structure, and potential application for the extraction of target analytes in different complex matrices.

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