ABSTRACT

Solid-phase microextraction (SPME) has been an important sample preparation technique in gas chromatography for almost 20 years. First developed for the analysis of volatile organic contaminants from water, its application has grown to numerous compound classes, including both volatile and non-volatile analytes. SPME may be combined with classical derivatization reactions to assist in transferring analytes from the sample to the ber coating, from the ber coating into and through the GC, or to aid in detection. This chapter summarizes techniques and efforts in the development and application of SPME methods for GC that include derivatization. Pre and post-extraction derivatization and simultaneous extraction and derivatization are possible and have been used for a variety of analytical problems. Using SPME for sample transfer makes derivatization readily automated and much simpler than

9.1 Introduction .................................................................................................. 373 9.2 Overview ....................................................................................................... 374

9.2.1 Brief History and Timeline of SPME ............................................... 374 9.2.2 Derivatization and Gas Chromatography ......................................... 374 9.2.3 Modes of Derivatization with SPME ................................................ 376

9.3 Pre-Extraction Derivatization ....................................................................... 376 9.4 Simultaneous Extraction and Derivatization ................................................380 9.5 Post-Extraction Derivatization on the Fiber ................................................. 381 9.6 Post-Extraction Derivatization in the Inlet ................................................... 382 9.7 Summary and Conclusions ........................................................................... 386 Acknowledgments .................................................................................................. 386 References .............................................................................................................. 386

in classical solution-based methods. The development of derivatization techniques involving SPME necessitates a further examination of classical derivatization reactions applied to GC.