Coupling continuous ultrasound-assisted extraction, preconcentration and flame atomic absorption spectrometric detection for the determination of cadmium and lead in mussel samples

• Published in: Analytica chimica acta Vol. 533; no. 1; pp. 51 - 56
• Main Authors: Yebra-Biurrun, M.C., Cancela-Pérez, S., Moreno-Cid-Barinaga, A.
• Format: Journal Article
• Language: English
• Published: Elsevier B.V 01.03.2005
• Subjects: Cadmium; Flame atomic absorption spectrometry; Flow injection analysis; Lead; Marine; Minicolumn preconcentration; Mollusca; Mytilidae; Ultrasound-assisted acid extraction; Spain, Galicia; ANE, Spain, Galicia; Ultrasound-assisted acid extraction; Lead; Cadmium; Minicolumn preconcentration; Flow injection analysis; Flame atomic absorption spectrometry
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2004.11.006

Continuous ultrasound-assisted extraction has been coupled with preconcentration and flame atomic absorption spectrometry for the determination of cadmium and lead in mussel samples. Experimental designs were used for the optimisation of the leaching and preconcentration steps. The use of diluted nitric acid as extractant in the continuous mode at a flow rate of 3.5 ml min −1 and room temperature was sufficient for quantitative extraction of these trace metals. A minicolumn containing a chelating resin (Chelite P, with aminomethylphosphoric acid groups) was proved as an excellent material for the quantitative preconcentration of cadmium and lead prior to their flame atomic absorption detection. A flow injection manifold was used as interface for coupling the three analytical steps, which allowed the automation of the whole analytical process. A good precision of the whole procedure (2.0 and 2.3%), high enrichment factors (20.5 and 11.8) and a detection limit of 0.011 and 0.25 μg g −1 for cadmium and lead, respectively, were obtained for 80 mg of sample. The sample throughputs were ca. 16 and 14 samples h −1 for cadmium and lead, respectively. The accuracy of the analytical procedures was verified by using a standard reference material (BCR 278-R, mussel tissue) and the results were in good agreement with the certified values. The method was successfully applied to the determination of trace amounts of cadmium and lead in mussel samples from the coast of Galicia (NW, Spain).