University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Website: @unf

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Classification: Biological tissue -> kidney -> horse

Citations 1

"Thermospray - Micro-atomizer Interface For The Determination Of Trace Cadmium And Cadmium Metallothioneins In Biological Samples With Flow Injection - And High Performance Liquid Chromatography - Atomic Absorption Spectrometry"
Anal. Chem. 1992 Volume 64, Issue 24 Pages 3197-3201
K. A. High, Richard Azani, A. F. Fazekas, Z. A. Chee, and J. S. Blais

Abstract: A description is given of a micro-atomization interface (made from quartz tubes) which is fuelled by hydrogen and can operate with 100% aqueous mobile phases used in HPLC. The system was optimized for the detection of Cd (total and bound soluble) in mussels and animal tissues, using flow injection AAS, or for the determination of metallothionein-bound Cd (isoforms I and II) in horse kidney, using HPLC - AAS. The detection limit obtained for Cd in the flow injection mode was ~2.2 orders of magnitude lower than that obtained with a conventional flame AAS detector, and 27-fold lower than that obtained by a thermospray-enhanced flame AAS system . Similar detection limits were obtained for the determination of metallothionein-bound Cd in the HPLC - AAS mode. A flexible thermospray-microatomization interface providing a high signal/noise ratio for flow injection atomic absorption spectrometry (AAS) and HPLC-AAS was designed and optimized for the determination of soluble Cd and Cd-metallothioneins (MTs). The interface, built from inexpensive quartz tubes, Swagelok fittings and thermoelectric wires, comprised 4 compartments: (1) a thermospray inlet; (2) a premixing tube in which the vaporized mobile phase was homogeneously mixed with preheated H; (3) a combustion chamber in which the fuel/sample mixture was mixed with O and pyrolyzed; and (4) a quartz tube (vapors retainer) mounted in the AAS analysis beam. This approach proved to more efficient than conventional flame AAS detection, due to the fact that the H/O flame (1900-2000°C), which pyrolysis mol. interferents to transparent CO2 and water vapors, is positioned remotely from the AAS optical beam. In this configuration, spectral interferences which are usually observed in flame and graphite furnace atomization were essentially eliminated. In flow injection (FI) mode, the response to Cd was linear from the limit of detection (71 pg) to 6 ng. The interface was optimized for the FI anal. of centrifuged mussel extracts, before and after ultrafiltration of the bound-Cd fraction on a 1000 MW cutoff membrane. During FI analyzes of these crude samples, matrix effect reduced the sensitivity by 13.2%, requiring calibration by standards addition Nonspecific absorption signal was not observed In HPLC-AAS mode, matrix effects in Cd-MTs chromatography bands were negligible. Cd-MTs from horse kidneys and mussels were determined with estimated limits of detection of 10^-40 ng (as protein).
Cadmium HPLC Spectrophotometry Optimization Interface Speciation Interferences