Evaluation of on-line coupling size exclusion chromatography electrothermal atomic absorption spectrometry for selenium speciation |
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Authors: | Francisco Laborda María V Vicente José M Mir J R Castillo |
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Institution: | (1) Analytical Spectroscopy and Sensors Group (G.E.A.S.), Department of Analytical Chemistry, University of Zaragoza, E-50009 Zaragoza, Spain, ES |
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Abstract: | Chromatographic effluents were on-line analyzed by Zeeman-ETAAS, using a flow-through cell placed in a graphite furnace autosampler
as interface. To obtain high sampling rates, the use of fast graphite furnace programmes was studied. Conventional programmes
of 96 s were reduced to 18 s by using hot injection (120 °C) and reducing the charring step to 2 s. The increase of the injection
volume from 20 to 60 μl lengthened the programme to 46 s. Nickel had to be added to get a comparable response for both inorganic
and organic selenium species (selenite and selenomethionine) and to reduce the interferent effect produced in presence of
the chromatographic eluent (TRIS 0.01 mol l-1, NH4NO3 0.1 mol l-1, pH 7). The optimized conditions were applied to the speciation of selenium in human erythrocyte lysates by size exclusion
LC-ETAAS. Using a high performance size exclusion column selenium could be assigned to proteins of 100 and 35 kDa. Detection
limits in the range of 1 ng (2 μg l-1 for 500 μl injection volume) were obtained for the combined technique.
Received: 9 October 1996/Revised: 8 July 1996/Accepted: 14 July 1996 |
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