Departamento de Química y Ciencia de los Materiales, Facultad de Ciencias Experimentales, Universidad de Huelva, Campus de El Carmen, 21007 Huelva, Spain.
Analyst. 2010 Oct;135(10):2700-5. doi: 10.1039/c0an00090f. Epub 2010 Aug 20.
The simultaneous speciation of elements is of great concern, especially in the study of the interactions of species in living organisms. Here we report a method based on the coupling of HPLC-ICP-MS that is capable of separating and analyzing different selenium and mercury species (Se-methylselenocysteine, selenite, selenate, L-selenomethionine, D-selenomethionine, methylmercury and inorganic mercury). The proposed method uses two different mobile phases that are suitable for selenium and mercury speciation and leads to a successful determination of all the species in less than 27 min with good efficiency and resolution. The method was efficiently applied for simultaneous speciation of mercury and selenium in urine and in serum, the latter from umbilical cord samples. Selenocystine has been successfully identified in the former sample. Detection limits obtained were between 0.30 and 2.46 ng. Recovery studies of samples spiked with all species were performed to check the reliability of the method, and satisfactory recoveries (93-110%) were obtained in all cases. The relative standard deviations (RSDs) for species with ten replicate determinations of 80 μg L(-1) were between 4.5 and 9.2%. The proposed method offers a deeper insight into selenium and mercury interactions in the human body.
元素的同时形态分析备受关注,特别是在研究生物体内物种相互作用时。在此,我们报告了一种基于 HPLC-ICP-MS 耦联的方法,该方法能够分离和分析不同的硒和汞形态(硒代半胱氨酸甲基、亚硒酸盐、硒酸盐、L-硒代蛋氨酸、D-硒代蛋氨酸、甲基汞和无机汞)。所提出的方法使用两种不同的流动相,适用于硒和汞的形态分析,成功地在不到 27 分钟内实现了所有形态的测定,具有良好的效率和分辨率。该方法成功地应用于尿液和血清(后者来自脐带样本)中汞和硒的同时形态分析。在前一个样本中成功鉴定了硒半胱氨酸。获得的检测限在 0.30 和 2.46 ng 之间。对所有物种进行加标回收研究以检查方法的可靠性,所有情况下的回收率均令人满意(93-110%)。对 80 μg L(-1) 的 10 次重复测定的物种进行相对标准偏差(RSD)为 4.5-9.2%。该方法为深入了解人体内硒和汞的相互作用提供了帮助。