Despite the widespread use of more and more effective detection technologies such as tandem-mass spectrometry, it is becoming increasingly clear that proper sample preparation is still the key to a successful analysis. The most important demands are thereby complete automation, sensitivity, reliability, economic efficiency and also implementation of ¿green¿ technologies that conserve our environment, e.g., by avoiding the use of larger volumes of organic solvents. Modern microextraction techniques can fulfill these demands and are already capable of replacing many traditional, manual sample preparation approaches. This thesis presents advances in the field of microextraction technologies. The primary scope is thereby the development and evaluation of a novel solid-phase microextraction device (SPME). PAL (prep and load) SPME Arrow retains all advantages of the classical SPME fiber and augments this proven concept with improved mechanical reliability and sorption phase volume. Initial evaluation of the method shows significantly increased extraction yields and a potential to further advance the field of SPME.