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- Title
Quantitative determination of small selenium species in human serum by HPLC/ICPMS following a protein-removal, pre-concentration procedure.
- Authors
Kokarnig, Sabine; Kuehnelt, Doris; Stiboller, Michael; Hartleb, Ulrike; Francesconi, Kevin A.
- Abstract
Protein precipitation was incorporated into a sample preparation method for the quantitative determination of small 'non-protein' selenium species in human serum by high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC/ICPMS). The advantages of cleaner matrix and concomitant concentration of the small compounds result in quantification limits in the native serum at the sub-micrograms Se per litre level. Spiking experiments with methyl 2-acetamido-2-deoxy-1-seleno-β- d-galactopyranoside (selenosugar 1), trimethylselenonium ion, selenomethionine, methylselenocysteine (MeSeCys) and selenate yielded recoveries from 73% to 103%. Selenite had a low recovery (44%), possibly owing to protein binding. The validated method was applied to serum samples from two volunteers before and after ingestion of a selenium food supplement. HPLC/ICPMS analysis showed, besides ingested selenate, the presence of selenosugar 1 and trace amounts of MeSeCys and methyl 2-amino-2-deoxy-1-seleno-β- d-galactopyranoside, which have not been reported in human serum before. [Figure not available: see fulltext.]
- Subjects
SELENIUM; SERUM; HIGH performance liquid chromatography; PROTEINS; NONMETALS
- Publication
Analytical & Bioanalytical Chemistry, 2011, Vol 400, Issue 8, p2323
- ISSN
1618-2642
- Publication type
Article
- DOI
10.1007/s00216-011-4992-5