Development and validation of analytical method for determination of total urinary antimony by chelation in supercritical carbon dioxide using fluorinated chelating agents

Abstract

Antimony toxicity occurs either due to occupational exposure or during therapy. There is a growing need for biological monitoring of antimony to provide exposure information to help prevent hazardous exposure. This study presents supercritical carbon dioxide (SC-CO₂) extraction as an inherently safe and clean sample treatment method for analyzing trace antimony in spiked human urine. Extraction was performed in the presence of a fluorinated β-diketone chelating agent, thenoyltrifluoroacetone, by unmodified SC-CO₂. Quantitative extractions were conducted at 60 °C and 17.2 MPa with 15 min static plus 10 min dynamic extractions. The extracts were subsequently analyzed by graphite furnace atomic absorption spectroscopy with spiking Pd(NO₃)₂–Mg(NO₃)₂ matrix modifier. The proposed procedure was successfully applied to determine the concentrations of antimony in spiked urine samples with satisfactory recoveries of 95.6%–102.9% (n = 6) and relative standard deviations <5%. The accuracy of the proposed procedure was also validated by the analysis of the certified reference materials.