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Characterization of a Microfabricated Electrochemical Detector and Coupling with High Performance Liquid Chromatography

Ogburn, Evan T.
http://rave.ohiolink.edu/etdc/view?acc_num=ucin1258475031

Abstract Details

2009, MS, University of Cincinnati, Arts and Sciences : Chemistry.
A disposable micro-fabricated electrochemical cell has been developed, characterized with multiple electrochemical systems, and coupled with high performance liquid chromatography to form a high performance liquid chromatography electrochemical detection (HPLC-ED) system. The detection system consisted of the micro-fabricated electrochemical detector, a flow-cell and a fixture mounted with electrical connections leading from the detector to the potentiostat. The detector is easy to fabricate, inexpensive, and maintains a high performance level which makes it a practical choice for electrochemical detection. The simplicity of the fabrication process for this detector allows it to be used as a disposable device that can be replaced easily if its performance degrades. Parameters for the optimization of the performance were studied in a three-electrode system with a special focus on HPLC-ED, using ascorbic acid, acetaminophen, and potassium ferricyanide as model compounds. A separation of three pharmaceutical compounds, dextrorphan, levallorphan, and acetaminophen was also performed in order to demonstrate the performance of the novel detector in comparison to commercially available macro electrochemical detectors. It was determined that the micro-fabricated detector’s performance was comparable to traditional non-disposable electrodes in these systems, especially HPLC-ED, which was the system of focus. The calibration curves constructed for each model compound showed linearity (R² > 0.99), the limit of detection reached picomolar (< 100) levels, and the peaks generated were more resolved and free from interference when the micro-fabricated detector was used. When this novel detector was used, the limit of detection reached 1.00 nM for acetaminophen, 1.00 nM for ascorbic acid, 50.0 nM for dextrorphan and 80.0 nM for levallorphan. When the nondisposable commercially available detector was used, the limit of detection reached 0.0500 nM for acetaminophen and 1.00 nM for ascorbic acid. Dextrorphan and levallorphan were detected as low as 2.5 nM and 5.00 nM, respectively, with the commercial system when samples were diluted in mobile phase, but the signal reproducibility was not good when tested in human plasma. The results within this thesis demonstrate that a micro-fabricated electrochemical detector can operate at a high level of performance when used in HPLC-ED, while maintaining cost effectiveness.
William Heineman, PhD (Committee Chair)
Carl Seliskar, PhD (Committee Member)
78 p.
Analytical Chemistry
Microfabricated Electrochemical Detector

Recommended Citations

Citations

  • Ogburn, E. T. (2009). Characterization of a Microfabricated Electrochemical Detector and Coupling with High Performance Liquid Chromatography [Master's thesis, University of Cincinnati]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1258475031

    APA Style (7th edition)

  • Ogburn, Evan. Characterization of a Microfabricated Electrochemical Detector and Coupling with High Performance Liquid Chromatography. 2009. University of Cincinnati, Master's thesis. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=ucin1258475031.

    MLA Style (8th edition)

  • Ogburn, Evan. "Characterization of a Microfabricated Electrochemical Detector and Coupling with High Performance Liquid Chromatography." Master's thesis, University of Cincinnati, 2009. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1258475031

    Chicago Manual of Style (17th edition)

ucin1258475031
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© 2009, all rights reserved.
This open access ETD is published by University of Cincinnati and OhioLINK.