Microfabricated Electrochemical Detector for High-Performance Liquid Chromatography

• Published in: Analytical chemistry (Washington) 2011-09, Vol.83 (18), p.6963-6970
• Main Authors: Ogburn, Evan T, Dziewatkoski, Michael, Moles, Don, Johnson, Jay M, Heineman, William R
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography; Electrocatalysis; Electrodes; Exact sciences and technology; General, instrumentation; Other chromatographic methods; Thin films
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/ac200476j

A microfabricated electrochemical cell has been developed as a disposable detector for flow injection analysis (FIA) and high-performance liquid chromatography (HPLC). The simplicity of the fabrication process allows this detector to be used as a low-cost, disposable device that can be replaced easily if its performance degrades rather than disassembling the detector and polishing the electrode surface, which is the usual procedure. The detector consists of thin film-metal electrodesplatinum working electrode, platinum auxiliary electrode, and silver/silver chloride coated on Pt reference electrodedeposited on a polyimide substrate with a locking layer of chromium in between. A microfluidic cover made of polyimide directs the solution flow across the electrodes. The detector was evaluated with FIA of ferrocyanide and HPLC of ascorbic acid and acetaminophen and a mixture of two pharmaceutical compoundsdextrorphan and levallorphanwith acetaminophen internal standard. The HPLC calibration curves showed good linearity (R 2 > 0.99). Limits of detection were 1 nM for acetaminophen, 1 nM for ascorbic acid, 50 nM for dextrorphan, and 80 nM for levallorphan. When detected with a commercial detector dextrorphan and levallorphan had lower limits of detection, 3 and 5 nM, respectively. Chromatograms of the mixture were comparable to those obtained with a commercial detector. The detector could be used continuously for about 48 h with FIA and about 10–20 h with HPLC after which performance gradually degraded as the AgCl on the reference electrode dissolved causing loss of potential control.