New Techniques for Sample Preparation in Analytical Chemistry Microextraction in Packed Syringe (MEPS) and Methacrylate Based Monolithic Pipette Tips

Sample preparation is often a bottleneck in systems for chemical analysis. The aim of this work was to investigate and develop new techniques to address some of the shortcomings of current sample preparation methods. The goal has been to provide full automation, on-line coupling to detection systems, short sample preparation times and high-throughput. In this work a new technique for sample preparation that can be connected on-line to liquid chromatography (LC) and gas chromatography (GC) has been developed. Microextraction in packed syringe (MEPS) is a new solid-phase extraction (SPE) technique that is miniaturized and can be fully automated. In MEPS approximately 1 mg of sorbent material is inserted into a gas tight syringe (100-250 µL) as a plug. Sample preparation takes place on the packed bed. Evaluation of the technique was done by the determination of local anaesthetics in human plasma samples using MEPS on-line with LC and tandem mass spectrometry (MS-MS). MEPS connected to an autosampler was fully automated and clean-up of the samples took about one minute. In addition, in the case of plasma samples the same plug of sorbent could be used for about 100 extractions before it was discarded. A further aim of this work was to increase sample preparation throughput. To do that disposable pipette tips were packed with a plug of porous polymer monoliths as sample adsorbent and were then used in connection with 96-well plates and LC-MS-MS. The evaluation of the methods was done by the analysis of local anaesthetics lidocaine and ropivacaine, and anti-cancer drug roscovitine in plasma samples. When roscovitine and lidocaine in human plasma and water samples were used as model substances, a 96-plate was handled in about two minutes. Further, disposable pipette tips may be produced at low cost and because they are used only once, carry-over is eliminated. 5 To my Parents; " scholarship and books are the building blocks of a better world ". 6 Abbreviations γ-MAPS tri((methoxysilyl)propyl)methacrylate ACN Acetonitrile AIBN 2,2'-Azobis(2-methylpropionitrile) ATP Adenosine Triphosphate BMA Butyl Methacrylate BP Benzophenone BPO Benzoyl Peroxide C2