Abstract
Electrokinetic sample extraction and enrichment is introduced as a newly developed concept for the analysis of substances in sludge-type or paste-like matrices. It is based on electrokinetic transport phenomena as electromigration and electroosmosis occurring when an electrical field is applied to the fresh, wet samples. Problems usually associated to sample drying can be avoided, e.g., losses of volatile analytes or contamination. We have designed and built a suitable apparatus for electrokinetic sample extraction and enrichment. Appropriate operating conditions (field strength, buffer composition, concentration, and volume) were identified in experiments with an artificial sludge model and real-world lake sediments. A proof of principle of the method was provided by the electromigrative extraction and online enrichment on a solid-phase sorbent disk of an azo dye from a diatomaceous earth slurry. Electroosmotic extraction and enrichment of a cyanobacterial hepatotoxin at trace levels was finally investigated as an application example using lake sediments. Rather clean extracts were obtained even with high organic content sediment samples, as shown by high-performance liquid chromatography with diode array detection.
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Acknowledgments
C. S. gratefully acknowledges financial support by a Landesgraduiertenförderung grant from the State of Baden-Württemberg. Lake sediment samples were collected during a joint project (no. 4500004431) with the LUBW Institute for Lake Research (Langenargen, Germany), and their sedimentological parameters were determined at this institute. In this context, we appreciate the support of Viola Burkhardt-Gehbauer, Andreas Jurischitz, Karin Popp, Erwin Rinné, Dr. Martin Wessels, and Dr. Hans Bernd Stich. We wish to express special thanks to Corinna Frey and C. Menno Müller for their skillful technical assistance in SPE and ESEE experiments.
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Schmidtkunz, C., Welsch, T. Electrokinetic sample extraction and enrichment: a new method for the isolation of analytes from sludge-type matrices. Anal Bioanal Chem 395, 1831–1841 (2009). https://doi.org/10.1007/s00216-009-3059-3
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DOI: https://doi.org/10.1007/s00216-009-3059-3