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On-line electrochemically controlled solid-phase extraction interfaced to electrospray and inductively coupled plasma
Gustav Liljegren1, Niklas Forsgard, Camilla Zettersten
1Department of Analytical Chemistry, Uppsala University, Box 599, SE-751 24 Uppsala, Sweden.
The Analyst
|September 21, 2005
Summary
Electrochemically controlled solid-phase extraction (EC-SPE) offers a versatile method for anion analysis. This technique, interfaced with mass spectrometry, effectively extracts bromide ions, even in the presence of interfering ions, and is suitable for lab-on-a-chip systems.
Area of Science:
- Analytical Chemistry
- Electrochemistry
- Materials Science
Background:
- Solid-phase extraction (SPE) is a crucial sample preparation technique.
- Interference from co-existing ions often complicates anion analysis.
- Developing electrochemically controlled methods can enhance SPE versatility.
Purpose of the Study:
- To investigate electrochemically controlled solid-phase extraction (EC-SPE) for anion analysis.
- To evaluate polypyrrole coatings for EC-SPE applications.
- To optimize EC-SPE for bromide ion extraction and detection.
Main Methods:
- On-line interfacing of EC-SPE with electrospray mass spectrometry (ESI-MS) and inductively coupled plasma mass spectrometry (ICP-MS).
- Utilizing polypyrrole-coated electrodes in a thin-layer electrochemical flow cell.
- Employing scanning electron microscopy (SEM) and atomic force microscopy (AFM) to characterize polypyrrole coatings.
- Investigating stopped-flow desorption for enhanced preconcentration.
Main Results:
- EC-SPE demonstrated versatility for extracting various anions.
- Polypyrrole coating properties were tunable by electrodeposition conditions.
- Interference from sulfate ions on bromide extraction was reduced using bromide-doped polypyrrole.
- Stopped-flow desorption significantly increased preconcentration factors for bromide.
- Detection of 3 µM bromide in spiked tap water samples was achieved.
Conclusions:
- EC-SPE is a promising potential-controlled sample preparation technique for anions.
- Modified polypyrrole coatings enhance selectivity and extraction efficiency.
- The developed EC-SPE method is suitable for analyzing low ion concentrations in complex matrices.
- EC-SPE's electrochemical control makes it ideal for miniaturized lab-on-a-chip systems.
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