Catarino Sofia, Curvelo-Garcia A S, Sousa R Bruno de
INIAP, Estação Vitivinícola Nacional, 2565-191 Dois Portos, Portugal; Instituto Superior de Agronomia, Departamento de Química Agrícola e Ambiental, Tapada da Ajuda, 1349-017 Lisboa, Portugal.
Talanta. 2006 Dec 15;70(5):1073-80. doi: 10.1016/j.talanta.2006.02.022. Epub 2006 Mar 15.
The aim of the present work was to develop and validate an accurate method by ICP-MS focalized to the measurement of contaminant elements in wines, in special those with legal importance. In addition, we intended to evaluate the suitability of ICP-MS semi-quantitative methodology in order to reduce the time and cost of analysis. Twenty-six contaminant elements of wine (Li, Be, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Ag, Cd, In, Cs, Ba, Hg, Tl, Pb, Bi and U) were measured using quantitative and semi-quantitative calibration approaches, in diluted white and red wines. In an early step potential interferences caused by Cl and Ca species were evaluated, in order to establish suitable mathematical corrections. For validation of ICP-MS procedures a few elements were determined by flame and electrothermal AAS. Reference wines from 1992 year, with provisional values, were analyzed and the results showed satisfactory agreement. The semi-quantitative calibration provided slightly higher limits of detection than those obtained by the quantitative calibration, and always lower than 0.1mugl(-1), except for Fe and Zn. For most elements the recovery percentages (between 90 and 100%) and precision of the results (R.S.D. (%)<4) were similar for both modes. Differences lower than 20% of concentration was obtained for most elements. Both methodologies offer valuable alternatives to wine characterization and comparison purposes. For legal requirements control purposes, with reference to the importance of accurate results, quantitative approach is the most suitable alternative.
本研究的目的是开发并验证一种通过电感耦合等离子体质谱法（ICP-MS）测定葡萄酒中污染元素的准确方法，特别是那些具有法律意义的元素。此外，我们旨在评估ICP-MS半定量方法的适用性，以减少分析时间和成本。使用定量和半定量校准方法，对稀释后的白葡萄酒和红葡萄酒中的26种葡萄酒污染元素（锂、铍、铝、钒、铬、锰、铁、钴、镍、铜、锌、镓、砷、硒、铷、锶、银、镉、铟、铯、钡、汞、铊、铅、铋和铀）进行了测定。在早期步骤中，评估了由氯和钙物种引起的潜在干扰，以建立合适的数学校正方法。为了验证ICP-MS程序，通过火焰原子吸收光谱法和电热原子吸收光谱法测定了一些元素。对1992年具有暂定值的参考葡萄酒进行了分析，结果显示出令人满意的一致性。半定量校准提供的检测限略高于定量校准获得的检测限，除铁和锌外，始终低于0.1μg l⁻¹。对于大多数元素，两种模式下的回收率（90%至100%）和结果的精密度（相对标准偏差（%）<4）相似。大多数元素的浓度差异低于20%。两种方法都为葡萄酒表征和比较提供了有价值的选择。对于法律要求控制目的，考虑到准确结果的重要性，定量方法是最合适的选择。
