Bantan T, Milacic R, Pihlar B
Department of Environmental Sciences, Jozef Stefan Institute, Jamova 39, 1000 Ljubljana, Slovenia.
Talanta. 1998 May;46(1):227-35. doi: 10.1016/s0039-9140(97)00282-8.
An anion-exchange fast protein liquid chromatographic-inductively coupled plasma atomic emission spectrometric procedure (FPLC-ICP-AES) was developed for speciation of Al-citrate and other negatively charged Al complexes. FPLC separations were carried out on a Mono Q HR 5/5 strong anion-exchange FPLC column over a pH range from 3.5 to 11.0. An aqueous-NaNO(3) (4 mol dm(-3)) linear gradient elution was applied over 10 min for separation of a particular Al species. The separated Al species were determined in 0.5 cm(3) eluate fractions ;off line' by ICP-AES. Under optimal analytical procedures Al-citrate was separated from Al-oxalate and Al-EDTA in a neutral pH range. Good reproducibility of the FPLC-ICP-AES procedure was obtained for determination of a particular Al species at optimal measurement conditions (RSD +/-2%). Al(3+) and neutral Al-citrate species were strongly adsorbed on the column resin and did not interfere with the separation of negatively charged Al complexes. Al(OH)(4)(-) species were separated from Al-citrate in an alkaline pH region, but quantitatively determined only at a pH of 11.0. The distribution of Al species over a pH range from 3.5 to 11.0 agreed with the reported calculated data. The limit of detection (3sigma basis) for separated Al species was 0.1 mug cm(-3).
开发了一种阴离子交换快速蛋白质液相色谱-电感耦合等离子体原子发射光谱法（FPLC-ICP-AES），用于柠檬酸铝和其他带负电荷的铝配合物的形态分析。FPLC分离在Mono Q HR 5/5强阴离子交换FPLC柱上进行，pH范围为3.5至11.0。采用水-NaNO₃（4 mol dm⁻³）线性梯度洗脱，在10分钟内分离特定的铝物种。分离出的铝物种在0.5 cm³洗脱液馏分中离线通过ICP-AES测定。在最佳分析程序下，柠檬酸铝在中性pH范围内与草酸铝和铝-EDTA分离。在最佳测量条件下，FPLC-ICP-AES法测定特定铝物种具有良好的重现性（RSD±2%）。Al³⁺和中性柠檬酸铝物种强烈吸附在柱树脂上，不干扰带负电荷的铝配合物的分离。Al(OH)₄⁻物种在碱性pH区域与柠檬酸铝分离，但仅在pH为11.0时可定量测定。在3.5至11.0的pH范围内铝物种的分布与报道的计算数据一致。分离出的铝物种的检测限（基于3σ）为0.1 μg cm⁻³。
