Abstract
A multi-element graphite furnace atomic absorption spectrometry (GFAAS) method was elaborated and applied for the simultaneous determination of As, Cd, Cr, Cu, and Pb in various kinds of honey samples (acacia, floral, linden, rape, and milkweed) using the transversally heated graphite atomiser (THGA) with end-capped tubes and integrated graphite platforms (IGPs). For comparative GFAAS analysis, direct (without digestion) and indirect (with digestion in a microwave oven) sample preparation procedures were tested. The effects of several chemical modifiers, such as NH 4H 2PO 4, NH 4H 2PO 4–Mg(NO 3) 2, and Pd(NO 3) 2–Mg(NO 3) 2, were studied to obtain optimal pyrolysis and atomization conditions for the set of analytes studied. The most efficient modifier was proved to be the mixture of 5 μg Pd (applied as nitrate) plus 3 μg Mg(NO 3) 2, allowing the optimal 600 °C pyrolysis and 2300 °C atomization temperatures. To prevent the sputtering and foaming of the matrix during the drying and pyrolysis steps of the furnace heating program, the sample and modifier solutions (20 + 5 μl, respectively) were dispensed together onto the IGP of the THGA pre-heated at 80 °C. The effect of increasing concentration of honey matrix was studied on the integrated absorbance ( A int) signals of analytes. The A int signals of Cr and Pb were not altered up to 10% (m/v) matrix content in the sample solutions. The matrix effect was slightly suppressive on the A int signals of As, Cd, and Cu above 2% (m/v) honey concentration. The recovery was found to be ranged between 85 and 115% for Cd, Cr, Cu, and Pb, whereas it was a lower, compromise value of 70–99% for As. The limit of detection (LOD) data were 1, 0.04, 0.09, 0.3, and 0.6 μg l −1 for As, Cd, Cr, Cu, and Pb, respectively, which values correspond to 20, 0.8, 1.8, 5.3, and 12 ng g −1, respectively, in the solid samples. The characteristic masses were found to be 21 pg As, 1.3 pg Cd, 4 pg Cr, 12 pg Cu, and 33 pg Pb. The As, Cd, Cr, Cu, and Pb contents of the studied 42 honey samples varied significantly, i.e. from below the LOD up to 13, 3.3, 109, 445, and 163 ng g −1, respectively.
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