Elçi Latif, Arslan Zikri, Tyson Julian F
Department of Chemistry, University of Pamukkale, Denizli TR-20020, Turkey.
J Hazard Mater. 2009 Mar 15;162(2-3):880-5. doi: 10.1016/j.jhazmat.2008.05.113. Epub 2008 May 28.
A method for direct determination of lead in wine and rum samples was developed, using a flow injection hydride generation system coupled to an atomic absorption spectrometer with flame-quartz atomizer (FI-HG-AAS). Lead hyride (PbH(4)) was generated using potassium ferricyanide (K(3)Fe(CN)(6)), as oxidant and sodium tetrahydroborate (NaBH(4)) as reductant. Samples were acidified to 0.40% (v/v) HCl for wine and to 0.30% (v/v) HCl for rum, which were then mixed on-line with 3% (m/v) K(3)Fe(CN)(6) solution in 0.03% (v/v) HCl prior to reaction with 0.2% (m/v) alkaline NaBH(4) solution. Lead contents of a rum and two different red wine samples were determined by FI-HG-AAS agreed with those obtained by ICP-MS. The analytical figures of merit of method developed were determined. The calibration curve was linear up to 8.0 microg L(-1) Pb with a regression coefficient of 0.998. The relative error was lower than 4.58%. The relative standard deviation (n=7) was better than 12%. A detection limit of 0.16 microg L(-1) was achieved for a sample volume of 170 microL.
建立了一种直接测定葡萄酒和朗姆酒样品中铅含量的方法,该方法采用流动注射氢化物发生系统与配有火焰石英原子化器的原子吸收光谱仪联用(FI-HG-AAS)。使用铁氰化钾(K₃Fe(CN)₆)作为氧化剂、硼氢化钠(NaBH₄)作为还原剂来生成氢化铅(PbH₄)。葡萄酒样品用盐酸酸化至0.40%(v/v),朗姆酒样品用盐酸酸化至0.30%(v/v),然后在与0.2%(m/v)碱性NaBH₄溶液反应之前,将其与0.03%(v/v)HCl中的3%(m/v)K₃Fe(CN)₆溶液在线混合。通过FI-HG-AAS测定的一种朗姆酒和两种不同红酒样品中的铅含量与通过电感耦合等离子体质谱法(ICP-MS)获得的结果一致。测定了所开发方法的分析性能指标。校准曲线在铅浓度高达8.0 μg L⁻¹时呈线性,回归系数为0.998。相对误差低于4.58%。相对标准偏差(n = 7)优于12%。对于170 μL的样品体积,检测限为0.16 μg L⁻¹。