title: The determination of total Se in urine and serum by graphite furnace atomic absorption spectrometry using Ir as permanent modifier and in situ oxidation for complete trimethylselenonium recovery.
abstract: The present work evaluated the use of iridium (Ir) as permanent modifier for the determination of total selenium in urine and serum by graphite furnace atomic absorption spectrometry. Concerning urine, the presence of trimethylselenonium (TMSe(+)) was especially considered. Pyrolysis and atomization temperatures of 1,000 and 2,100 degrees C, respectively, were used. For nondigested urine and serum samples, 0.2% v/v HNO(3) and Triton X-100 were used as diluents, respectively, and the same initial platform Ir treatment was effective for up to 1,100 atomization cycles. Good precision [less than 5% relative standard deviation (RSD)] can be achieved with the proposed method. Low TMSe(+) recovery was observed for nondigested urine samples. Thus, if this species is to be considered in urine analysis, a previous external mineralization step was found to be necessary. Alternatively, an in situ oxidation treatment was developed. Detection limits of 8, 10, and 7 mug l(-1) were obtained after dilution, microwave-assisted digestion, and in situ oxidation procedures, respectively. The accuracy of the method was validated by the analysis of certified reference or commercial quality control materials and spiked samples.
authors.affiliation: Department of Chemistry, Pontifícia Universidade Católica do Rio de Janeiro, Rua Marquês de São Vicente, 225, Rio de Janeiro, 22453-900, Brazil. rccampos@rdc.puc-rio.br
authors.forename: Patricia
authors.initials: P
authors.lastname: Grinberg
authors.forename: Rodrigo Araújo
authors.initials: RA
authors.lastname: Gonçalves
authors.forename: Reinaldo Calixto
authors.initials: RC
authors.lastname: de Campos
mesh_terms: D006108:Graphite / Q000737:chemistry*; D006801:Humans; D007495:Iridium / Q000737:chemistry*; D010084:Oxidation-Reduction; D015203:Reproducibility of Results; D012643:Selenium / Q000097:blood* / Q000652:urine*; D018036:Selenium Compounds / Q000097:blood / Q000652:urine; D012680:Sensitivity and Specificity; D013054:Spectrophotometry, Atomic / Q000295:instrumentation / Q000379:methods*; D013696:Temperature
chemical_list: D018036:Selenium Compounds; D007495:Iridium; D006108:Graphite; D012643:Selenium; C003717:trimethylselenonium