4° Seminario Sociedad Argentina de Espectrometría de Masa
Ciclo de Seminarios Virtuales
HEADSPACE SOLID PHASE MICROEXTRACTION APPLIED TO ANALYSIS OF COMPOUNDS
WITH LOW VOLATILITY
Fabio Augusto
Institute of Chemistry - University of Campinas (IQ-Unicamp) and National Institute of Science and Technology in Bioanalytics (INCTBio), 13083-970 Campinas, Brazil
*faugusto@unicamp.br
Solid Phase Microextraction (SPME), either using commercially available devices
such as fibers or lab-made systems probably is the most popular extraction and
pre-concentration technique applied to chromatographic analysis. When GC is used, the coupling with SPME is simple, fast and reliable particularly using headspace analysis (HS-SPME). However, there is a practical restriction on HS-SPME: it is limited to compounds with enough volatility to provide a minimum concentration on the vapor phase to allow their transport to the SPME fiber (species with boiling points up to 250 °C or vapor pressures of >10 Pa at ambient conditions). For solid matrixes, GC analysis of non volatile, non-derivatizable substances is usually carried out using lengthy and cumbersome procedures such as Soxhlet extraction – which demands usually aditional extract clean-up. Here, we will assess the combination of HS-SPME to two different approaches to allow its use on GC analysis of compounds with very low vapour pressures (10-7 bar or less): vaccuum-assisted Headspace SPME (Vac-HSSPME, firstly described by Psilakis and co-workers [1]) and Subcritical Water Extraction combined to SPME (SWE-SPME [2]). Both combinations where
tested using apropriate samples (rock samples collected from stratigraphic exploratory oil wells), allowing better sensitivities and quantitative performance when compared to the traditional Soxhlet procedures.
Acknowledgements University of Campinas, Coordination for the Improvement of Higher Education Personnel (CAPES) – Finance Code 001, INCTBio.
References
[1] E. Psillakis, Anal.Chim. Acta 986, 12 (2017).
[2] S.B. Hawthorne and others, Anal. Chem. 68, 3892 (1996)
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