Laboratoire de Chimie Analytique Bio-Inorganique et Environnement (LCABIE), Université de Pau et des Pays de l'Adour/CNRS, UMR 5254, IPREM, Hélioparc, 2 Avenue du Président Angot, 64053 Pau Cedex 9, France.
Anal Chim Acta. 2011 Jan 17;684(1-2):126-33. doi: 10.1016/j.aca.2010.10.044. Epub 2010 Nov 9.
This paper describes the development of an analytical methodology to determine speciation of selenium present in soils at trace level (μg kg(-1)). The methodology was based on parallel single extractions and high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC-ICPMS). Two complementary chromatographic separations were used to confirm Se species identity. Different extractants, selected on the basis of sequential extraction schemes, were compared. Ultrapure water, 0.1 molL(-1) phosphate buffer (KH(2)PO(4)/K(2)HPO(4)) at pH 7 and 0.1 molL(-1) sodium hydroxide extractants were finally chosen owing to their efficiency in extracting Se and compatibility with Se species stability. These extractants allow also assessing respectively water-soluble Se (i.e. the most mobile Se fraction), exchangeable Se (i.e. sorbed onto soil component surface) and Se bound to soil organic matter. This methodology gives thus information on Se mobility related to its distribution in soil with preservation of original Se speciation. Detection limits range from 3 to 29ng(Se)L(-1) and from 0.1 to 10 μg(Se)kg(-1), allowing determination of Se species concentrations in extracts from soils containing native Se at trace level. The methodology was applied to three soils with total Se concentrations between 210 and 1560 μg(Se)kg(-1).
本文描述了一种分析方法的发展,用于测定痕量水平(μg kg(-1))土壤中硒的形态。该方法基于平行单提取和高效液相色谱与电感耦合等离子体质谱联用(HPLC-ICPMS)。使用两种互补的色谱分离方法来确认硒形态的身份。选择了基于顺序提取方案的不同提取剂进行比较。最终选择了超纯水、0.1 molL(-1) 磷酸缓冲液(KH(2)PO(4)/K(2)HPO(4))在 pH 7 和 0.1 molL(-1) 氢氧化钠提取剂,因为它们能够有效地提取硒,并且与硒形态的稳定性兼容。这些提取剂还允许分别评估水溶性硒(即最具移动性的硒部分)、可交换硒(即吸附在土壤成分表面上的硒)和与土壤有机质结合的硒。因此,该方法提供了有关硒与其在土壤中分布相关的移动性的信息,同时保留了原始硒形态。检测限范围为 3 至 29ng(Se)L(-1)和 0.1 至 10μg(Se)kg(-1),允许测定含有痕量天然硒的土壤提取物中的硒形态浓度。该方法应用于总硒浓度在 210 至 1560μg(Se)kg(-1)之间的三种土壤。