ORIGINAL PAPER Determination of lead in wine by hydride generation atomic fluorescence spectrometry in the presence of hexacyanoferrate(III) Irina B. Karadjova & Leonardo Lampugnani & Alessandro D’Ulivo & Massimo Onor & Dimiter L. Tsalev Received: 10 November 2006 / Revised: 8 January 2007 / Accepted: 12 January 2007 / Published online: 14 February 2007 # Springer-Verlag 2007 Abstract A rapid, accurate, and precise method is de- scribed for the determination of Pb in wine using continuous-flow hydride generation atomic fluorescence spectrometry (CF-HGAFS). Sample pretreatment consists of ten-fold dilution of wine followed by direct plumbane generation in the presence of 0.1 mol L -1 HCl and 1% m/v K 3 [Fe(CN) 6 ] with 1% m/v NaBH 4 as reducing agent. An aqueous standard calibration curve is recommended for Pb quantification in wine sample. The method provides a limit of detection and a limit of quantification of 0.3 μgL -1 and 1 μgL -1 , respectively. The relative standard deviation varies between 2–6% (within-run) and 4–11% (between- run) at 3–30 μgL -1 Pb levels in wine. Good agreement has been demonstrated between results obtained by CF-HGAFS and direct electrothermal atomic absorption spectrometry in analyses of red and white wines within the concentration range of 9.2–25.8 μgL -1 Pb. Keywords Lead . Wine . Hydride generation atomic fluorescence spectrometry . Hexacyanoferrate (III) Introduction Wine is one of the most widely consumed beverages and strict control of the levels of toxic elements is required according to national and international regulatory rules [1, 2]. The presence of Pb in wine could be attributed to the so- called primary sources (transfer of metal from the soil/ groundwater to the grapes and finally to the wines, or atmospheric deposition of airborne particulate matter on grapes) and secondary sources including the winemaking process (clarification and fining agents), wine processing equipment (valves, pipes, pumps, bronze tanks), and bottles (cork capsules used for sealed bottles). The Organisation Internationale de la Vigne et du Vin (OIV) has set a maximum limit of 200 μgL -1 for Pb in wine. Various methods have been developed and proposed for Pb determination in wine as reviewed recently [3–5]. Two main directions could be distinguished in sample pretreat- ment procedures for Pb determination in wine: sample digestion by using microwave digestion and UV-photolysis [6–9] or direct instrumental determination after wine dilution. Direct approaches are preferred for routine application. The most widely used method for direct determination of Pb in wine is electrothermal atomic absorption spectrometry (ETAAS) and is proposed as a standard method by OIV, in the presence of different modifiers: NH 4 H 2 PO 4 [10–13], Pd + Mg(NO 3 ) 2 [14–17], or without modifier [18]. Recent procedures based on direct inductively coupled plasma mass spectrometry (ICPMS) determination of Pb in wine [19–22] and precise Pb isotope ratios determination in wine [23–26] have been reported. A few papers dealing with speciation analysis of Pb in wine have been published, based mainly on size exclusion high- performance liquid chromatography (HPLC)-ICPMS [27] and electrochemical methods [28, 29]. Anal Bioanal Chem (2007) 388:801–807 DOI 10.1007/s00216-007-1127-0 I. B. Karadjova : D. L. Tsalev (*) Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., 1164 Sofia, Bulgaria e-mail: tsalev@chem.uni-sofia.bg L. Lampugnani : A. D’Ulivo : M. Onor Istituto per i Processi Chimico-Fisici (IPCF-CNR), Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa, Italy