Quantitative HPLC-ICP-MC analysis of antimony redox speciation in complex sample matrices: new insights into the Sb-chemistry causing poor chromatographic recoveries

TY - JOUR

T1 - Quantitative HPLC-ICP-MC analysis of antimony redox speciation in complex sample matrices: new insights into the Sb-chemistry causing poor chromatographic recoveries

AU - Hansen, Claus

AU - Schmidt, Bjørn

AU - Larsen, Erik Huusfeldt

AU - Gammelgaard, Bente

AU - Stürup, Stefan

AU - Hansen, Helle Rüsz

PY - 2011/3/7

Y1 - 2011/3/7

N2 - In solution antimony exists either in the pentavalent or trivalent oxidation state. As Sb(iii) is more toxic than Sb(v), it is important to be able to perform a quantitative speciation analysis of Sb's oxidation state. The most commonly applied chromatographic methods used for this redox speciation analysis do, however, often show a low chromatographic Sb recovery when samples of environmental or biological origin are analysed. In this study we explored basal chemistry of antimony and found that formation of macromolecules, presumably oligomeric and polymeric Sb(v) species, is the primary cause of low chromatographic recoveries. A combination of HPLC-ICP-MS, AFFF-ICP-MS and spin-filtration was applied for analysis of model compounds and biological samples. Quantitative chromatographic Sb redox speciation analysis was possible by acidic hydrolysis of the antimony polymers prior to analysis. Sample treatment procedures were studied and the optimum solution was acidic hydrolysis by 1 M HCl in the presence of chelating ligands (EDTA, citrate), which stabilise the trivalent oxidation state of Sb.

AB - In solution antimony exists either in the pentavalent or trivalent oxidation state. As Sb(iii) is more toxic than Sb(v), it is important to be able to perform a quantitative speciation analysis of Sb's oxidation state. The most commonly applied chromatographic methods used for this redox speciation analysis do, however, often show a low chromatographic Sb recovery when samples of environmental or biological origin are analysed. In this study we explored basal chemistry of antimony and found that formation of macromolecules, presumably oligomeric and polymeric Sb(v) species, is the primary cause of low chromatographic recoveries. A combination of HPLC-ICP-MS, AFFF-ICP-MS and spin-filtration was applied for analysis of model compounds and biological samples. Quantitative chromatographic Sb redox speciation analysis was possible by acidic hydrolysis of the antimony polymers prior to analysis. Sample treatment procedures were studied and the optimum solution was acidic hydrolysis by 1 M HCl in the presence of chelating ligands (EDTA, citrate), which stabilise the trivalent oxidation state of Sb.

KW - Former Faculty of Pharmaceutical Sciences

U2 - 10.1039/c0an00796j

DO - 10.1039/c0an00796j

M3 - Journal article

C2 - 21157586

SN - 0003-2654

VL - 136

SP - 996

EP - 1002

JO - Analyst

JF - Analyst

IS - 5

ER -