Application of double-spike isotope dilution for the accurate determination of Cr(III), Cr(VI) and total Cr in yeast |
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Authors: | Lu Yang Elena Ciceri Zoltán Mester Ralph E Sturgeon |
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Institution: | (1) Institute for National Measurement Standards, National Research Council Canada, Ottawa, Ontario, K1A 0R6, Canada;(2) Department of Chemical and Environmental Sciences, University of Insubria, Via Valleggio, Como, Italy |
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Abstract: | A method is presented for the simultaneous determination of Cr(III) and Cr(VI) in yeast using species-specific double-spike
isotope dilution (SSDSID) with anion-exchange liquid chromatography (LC) separation and sector field inductively coupled plasma
mass spectrometric (SF-ICP-MS) detection. Total Cr is quantitated using ID SF-ICP-MS. Samples were digested on a hot plate
at 95±2 °C for 6 h in an alkaline solution of 0.5 M NaOH and 0.28 M Na2CO3 for the determination of Cr(III) and Cr(VI), whereas microwave-assisted decomposition with HNO3 and H2O2 was used for the determination of total Cr. Concentrations of 2,014±16, 1,952±103 and 76±48 mg kg−1 (one standard deviation, n=4, 3, 3), respectively were obtained for total Cr, Cr(III) and Cr(VI) in the yeast sample. Significant oxidation of Cr(III)
to Cr(VI) (24.2±7.6% Cr(III) oxidized, n=3) and reduction of Cr(VI) to Cr(III) (37.6±6.5% Cr(VI) reduced, n=3 ) occurred during alkaline extraction and subsequent chromatographic separation at pH 7. Despite this significant bidirectional
redox transformation, quantitative recoveries for both Cr(III) and Cr(VI) were achieved using the SSDSID method. In addition,
mass balance between total Cr and the sum of Cr(III) and Cr(VI) concentrations was achieved. Method detection limits of 0.3,
2 and 30 mg kg−1 were obtained for total Cr, Cr(VI) and Cr(III), respectively, based on a 0.2-g sub-sample. |
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Keywords: | Cr(III) Cr(VI) Double-spike isotope dilution Yeast ICP-MS |
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