RESUMO
A method based on flow injection hydride generation atomic absorption spectrometry (FI-HGAAS) with an on-line pre-reduction of Se(VI) to Se(IV) was developed and optimized to determine phosphate-extractable Se (0.1 M phosphate buffer KH2PO4/K2HPO4 at pH 7). The extracted fraction involves water-soluble Se (i.e. the most mobile Se fraction) and exchangeable Se (i.e. sorbed onto soil component surface). Kinetic discrimination mechanisms allowed the complete removal of interferences caused by organic matter due to the formation of humic substances (HS)-Se(IV) complexes observed when batch pre-reduction processes were used. Se(IV) and Se(VI) recoveries ranged 95-105% at a fortification level of 150 µg kg-1. The pre-reduction was efficiently carried out in 20 s in a 6 M HCl medium at 100 °C. Results from phosphate-extractable fractions were comparable to those obtained by ICP-MS. Se bound to organic matter was released digesting the remaining material from the phosphate buffer extraction with 0.1 M K2S2O8. Detection and quantification limits were 15 µg kg-1 Se and 50 µg kg-1 Se, respectively, in each fraction. The methodology was applied to 10 agricultural soils from Argentina with total Se concentration levels between 130 µg kg-1 and 419 µg kg-1.
Assuntos
Selênio , Espectrofotometria Atômica , Solo , FosfatosRESUMO
An optimised FI-HGAAS method was applied to determine the total selenium concentrations in selected high consumption food (fish, beef, chicken, milk, rice, wheat flour, egg) and to estimate their contribution to the Argentinean dietary intake, whose information is scarce nowadays. Through several optimisation steps a suitable method was achieved showing satisfactory figures of merit for all matrices. Average recovery was 96%, RSD<5%, LODs ranged 2.0-7.0 µg kg(-1) and the accuracy was assessed using DOLT-3 NRC certified reference material. Meat and eggs showed the highest values (in µg kg(-1), beef: 42-153; chicken: 62-205; fish: 94-314; canned tuna: 272-282; eggs: 134-217), minor values were found for wheat flour (22-42), rice: (<22), pasta (47-64) and milk (<7-9). An estimated intake of 32 and 24 µg day(-1) for adult men and women, respectively, suggested a deficient Se intake, leading to further comprehensive surveys of Se occurrence in Argentina.