Solid-phase microextraction (SPME) is an equilibrium-based sample preparation method that permits the integration of sampling, sample clean-up, and preconcentration in a single step. The lack of proper chemical bonding of the stationary phase coating with the substrate surface seems to be responsible for the low thermal and chemical stability of conventionally coated fibers, and these lead to a short lifetime of the coating. Sol–gel technology offers a simple and convenient pathway for the synthesis of advanced material systems to overcome this problem. Strong adhesion of the coating onto the support due to chemical bonding is a very important characteristic which increases the chemical and thermal stability of the coating and subsequently extends the applications of SPME toward less volatile and more polar compounds. This review describes the new developments in the use of sol–gel technology to prepare chemically bonded and stable SPME coatings.

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