Journal of the Brazilian Chemical Society
versión On-line ISSN 1678-4790
GINE, Maria Fernanda et al. Sequential cloud point extraction of trace elements from biological samples and determination by inductively coupled plasma mass spectrometry. J. Braz. Chem. Soc. [online]. 2008, vol.19, n.3, pp. 471-477. ISSN 1678-4790. http://dx.doi.org/10.1590/S0103-50532008000300014.
A two-step sequential cloud point extraction (CPE) of trace elements from small sample volumes of human serum, animal blood, and food diet is proposed to gain analytical information in the analysis by inductively coupled plasma mass spectrometry. The first CPE was attained by adding O,O-diethyldithiophosphate, the non ionic surfactant Triton® X-114 followed by heating at 40 ºC, centrifugation and cooling at 0 ºC. The resulting surfactant-rich phase was separated to determine Cd, Pb and Cu by isotope dilution. Isotope ratio measurements presented RSD < 0.7%. The residual surfactant-poor phase solution had the pH adjusted in the range 4 to 5 before the chelating reagent, 4-(2-pyridylazo) resorcinol plus surfactant Triton® X-114 were added followed by the sequence to attain the CPE. Co and Ni were quantified in the second extracted surfactant-rich phases by standard additions method with RSD < 2%. Recoveries from 85 to 96% were obtained for all elements. Analyzing reference materials with certified and recommended values assessed accuracy.
Palabras clave : sequential cloud point extraction; CPE; inductively coupled plasma mass spectrometry; isotope dilution; biological samples; trace elements.