Abstract
A fully automated sequential injection column preconcentration method for the on-line determination of trace vanadium, cadmium and lead in urine samples was successfully developed, utilizing electrothermal atomic absorption spectrometry (ETAAS). Polyamino-polycarboxylic acid chelating resin (Nobias chelate PA-1) packed into a handmade minicolumn was used as a sorbent material. Effective on-line retention of chelate complexes of analytes was achieved at pH 6.0, while the highest elution effectiveness was observed with 1.0 mol L−1 HNO3 in the reverse phase. Several analytical parameters, like the sample acidity, concentration and volume of the eluent as well as the loading/elution flow rates, have been studied, regarding the efficiency of the method, providing appropriate conditions for the analysis of real samples. For a 4.5 mL sample volume, the sampling frequency was 27 h−1. The detection limits were found to be 3.0, 0.06 and 2.0 ng L−1 for V(V), Cd(II) and Pb(II), respectively, with the relative standard deviations ranging between 1.9–3.7%. The accuracy of the proposed method was evaluated by analyzing a certified reference material (Seronorm™ trace elements urine) and spiked urine samples.
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Acknowledgments
Georgia Giakisikli acknowledges financial support from the State Scholarships Foundation (IKY) in Greece through the project “Scholarships IKY” from resources of the EP (European Program) “Education and Lifelong Learning”, “European Social Fund of ESPA 2007–2013”. This work was partly supported by JSPS KAKENH1 Grant Nos. 26288072 (Grant-in-Aid for Scientific Research (B) for N. T.) and 25860024 (Grant-in-Aid for Young Scientists (B) for H. M.).
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Giakisikli, G., Quezada, A.A., Tanaka, J. et al. Automatic On-line Solid-phase Extraction-Electrothermal Atomic Absorption Spectrometry Exploiting Sequential Injection Analysis for Trace Vanadium, Cadmium and Lead Determination in Human Urine Samples. ANAL. SCI. 31, 383–389 (2015). https://doi.org/10.2116/analsci.31.383
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DOI: https://doi.org/10.2116/analsci.31.383