Raml Reingard, Goessler Walter, Francesconi Kevin A
Karl-Franzens-University Graz, Institute of Chemistry-Analytical Chemistry, Universitaetsplatz 1, 8010 Graz, Austria.
J Chromatogr A. 2006 Sep 22;1128(1-2):164-70. doi: 10.1016/j.chroma.2006.06.061. Epub 2006 Jul 18.
A new group of arsenic species, thio-arsenicals, have recently been reported in several natural samples such as molluscs, algae, and urine. These compounds are the sulfur analogues of oxo-arsenicals, a large group of naturally-occurring compounds, whereby the arsinoyl (As=O) group is substituted by an arsinothioyl group (As=S). The most common separation technique for oxo-arsenicals is anion-exchange HPLC with polymer-based columns, but under these conditions the thio-arsenicals show strong retention, resulting in unacceptably long analysis times and broad peaks. We report the development of a reversed-phase HPLC method, with ICPMS detection, which allows separation of the known thio-arsenicals within 15 min with significantly improved peak shapes. The detection limit is about 0.6 microg As/L based on 10 microL injection volume. Further, we have applied the method to the identification and quantification of thio-arsenic species in two standard reference materials, BCR 710 oyster tissue and NIES 18 human urine.
最近在一些天然样品（如软体动物、藻类和尿液）中报道了一类新的砷物种——硫代砷化合物。这些化合物是含氧砷化合物的硫类似物，含氧砷化合物是一大类天然存在的化合物，其中胂酰基（As=O）被胂硫酰基（As=S）取代。对于含氧砷化合物，最常用的分离技术是使用聚合物基柱的阴离子交换高效液相色谱法，但在这些条件下，硫代砷化合物显示出很强的保留性，导致分析时间长得令人无法接受且峰形很宽。我们报告了一种采用电感耦合等离子体质谱检测的反相高效液相色谱方法的开发，该方法能够在15分钟内分离出已知的硫代砷化合物，且峰形有显著改善。基于10微升进样体积，检测限约为0.6微克砷/升。此外，我们已将该方法应用于两种标准参考物质（BCR 710牡蛎组织和NIES 18人尿）中硫代砷物种的鉴定和定量。
