Today’s solid phase microextraction (SPME) is a well known technique that combines knowledge from different fields in an attractive, efficient, and economic way. The development of SPME has seen huge growth since its introduction as a new approach to sample preparation in the early 1990s. The applications of SPME are continuously expanding, and one of the most interesting current aspects consists of applying SPME for fast analysis of biological fluids, both in vitro and in vivo.In spite of this great potential, development of new bio-applications is considerably hindered by the lack of suitable SPME products. The goal of this study is to find SPME coatings that can be utilized for in vivo and in vitro extractions, in direct contact with a biological matrix such as blood or tissue. This thesis presents several effective ways of preparing SPME coatings based on biocompatible polymers and silica-based extractive phases, focusing on their biocompatibility as a must. After fabrication, the proposed coatings are tested for biocompatibility and analytical utility.Finally, some practical applications of the new coatings are presented, such as fast drug analysis and determination of drug plasma protein binding. Six test drugs with different physico-chemical properties are chosen for the investigation: diazepam, verapamil, lorazepam, warfarin, nordiazepam, and loperamide. It is shown that the application of these new SPME fibers for biological sample analysis greatly reduces the time required for sample preparation and limits the exposure of the analytical personnel to potentially infectious biofluids.
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