State Key Laboratory of Coordination Chemistry, Department of Chemistry and Center of Materials Analysis, Nanjing University, 22 Hankou Road, Nanjing 210093, PR China.
Talanta. 2004 Jan 9;62(1):43-50. doi: 10.1016/S0039-9140(03)00405-3.
The determination of trace levels of aluminum by high performance liquid chromatography (HPLC) with spectrophotometric detection using quercetin, a bioactive substance as a pre-column reagent, is developed in this paper. The Al-quercetin chelate was separated on a reversed-phase ODS column with a mobile phase consisting of 70% water (pH 1.0 with perchloric acid) and 30% methanol, and detected at its maximum of 415nm. The response was linear over the 1.0x10(-7) to 8.0x10(-5)M concentration range with a detection limit of 5.0x10(-8)M and a relative standard deviation of 1.0% at the 5x10(-6)M level. The analysis was free from common ions except iron, which could be successfully screened by 1,10-phenanthroline. This method has been employed to the determination of Al in environmental and biological samples. Moreover, direct speciation of labile monomeric Al, the toxic form of Al, in natural water by the present technique was explored. The coordination ratio of Al complex with quercetin was also elucidated by HPLC combined with molar ratio method. Only a 1:1 complex was formed. Because quercetin exists in body, a preliminary thinking of in vivo determination of Al is provided in this study.
本文发展了一种采用高效液相色谱（HPLC）与分光光度检测法，使用槲皮素（一种生物活性物质）作为预柱试剂来测定痕量铝的方法。Al-槲皮素螯合物在反相 ODS 柱上分离，流动相由 70%水（用高氯酸调 pH 值至 1.0）和 30%甲醇组成，在 415nm 处检测。在 1.0x10(-7)至 8.0x10(-5)M 的浓度范围内，响应呈线性，检测限为 5.0x10(-8)M，在 5x10(-6)M 水平时的相对标准偏差为 1.0%。除铁以外，该分析不受常见离子的干扰，铁可以通过 1,10-菲啰啉成功屏蔽。该方法已用于环境和生物样品中铝的测定。此外，还探索了用本技术直接对天然水中不稳定单体铝（铝的毒性形式）进行形态分析。通过 HPLC 与摩尔比法相结合，还阐明了 Al 与槲皮素的配合比。仅形成 1:1 的配合物。由于槲皮素存在于体内，本研究为体内铝的测定提供了初步思路。
