Automatic flow system for the sequential determination of copper in serum and urine by flame atomic absorption spectrometry |
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Authors: | Cristina MPV Lopes João LM Santos José LFC Lima |
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Institution: | REQUIMTE, Departamento de Química-Física, Faculdade de Farmácia, Universidade do Porto, Rua Aníbal Cunha 164, 4099-030 Porto, Portugal |
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Abstract: | In this work, a fully automated flow system exploiting the advantages of the association of multi-pumping, multicommutation, binary sampling and merging zones, to accomplish the sequential determination of copper in serum and urine by flame atomic absorption spectrometry, is described. The developed flow system allowed multiple tasks, such as serum samples preparation (samples and standard solutions viscosity adjustment), serum copper (SCu) measurement, urine copper (UCu) pre-concentration and its subsequent elution and measurement, to be carried out sequentially. The implemented flow manifold presented a modular configuration consisting on two quasi-independent modules, each one accountable for a specific sample manipulation and whose combined operation under computer control enabled the determination of copper in a wide concentrations range.Once optimised and with a sample consumption of about 0.250 mL of serum and 7 mL of urine, the developed flow system allowed linear calibration plots up to 5 mg L−1 with a detection limit of 0.035 mg L−1 for SCu and linear calibration plots up to 300 μg L−1 with a detection limit of 0.67 μg L−1 for UCu. The sampling rate varied according to the module employed and was about 360 determinations h−1 (SCu module), 12 determinations h−1 (UCu module) or 24 determinations h−1 (12 urine and 12 serum samples; UCu and SCu modules simultaneously). Repeatability studies (R.S.D.%, n = 10) showed good precision for UCu at concentrations of 25 μg L−1 (2.54%), 50 μg L−1 (0.90%) and 100 μg L−1 (1.62%) as well as for SCu at concentrations of 0.25 mg L−1 (8.11%), 1 mg L−1 (3.11%) and 5 mg L−1 (0.90%). A comparative evaluation showed a good agreement between the results obtained in the analysis of UCu and SCu (n = 18) by both the developed methodology and the reference procedures. Accuracy was further evaluated by means of the analysis of reference samples (Seronorm™ Trace Elements Urine and Seronorm™ Trace Elements Serum) and the obtained results complied with the certified values. |
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Keywords: | Copper Serum Urine Flame atomic absorption spectrometry Multi-pumping flow system |
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